data_pl16010_sq
_audit_creation_date              2016-04-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
loop_
  _publ_author_name
  _publ_author_email
  _publ_author_address
 'Nichol, G.S.' g.s.nichol@ed.ac.uk
;
Joseph Black Building David Brewster Road
Edinburgh
EH9 3FJ
;

_publ_contact_author_address
;
Joseph Black Building David Brewster Road
Edinburgh
EH9 3FJ
;
_publ_contact_author_email        g.s.nichol@ed.ac.uk
_publ_contact_author_name         'Nichol, G.S.'
_publ_contact_author_phone        '+44 131 658 4806'
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common             ?
_chemical_name_systematic         ?
_chemical_formula_moiety
'C120 H84 Co4 N24, 12(Cl0.33 O1.33), 12(F6 P), 4(H4 N1), 4 C2 H3 N2'
_chemical_formula_sum             'C216 H244 Cl4 Co4 F72 N76 O16 P12'
_chemical_formula_weight          6278.02
_chemical_absolute_configuration  ad
_chemical_melting_point           ?
_chemical_oxdiff_formula          'C120 H84 Co4 F72 N24 P12'
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Co' 'Co' -2.3653 3.6143
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system       'cubic'
_space_group_IT_number            218
_space_group_name_H-M_alt         'P -4 3 n'
_space_group_name_Hall            'P -4n 2 3'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 '-x, y, -z'
 'x, -y, -z'
 'z, x, y'
 'z, -x, -y'
 '-z, -x, y'
 '-z, x, -y'
 'y, z, x'
 '-y, z, -x'
 'y, -z, -x'
 '-y, -z, x'
 'y+1/2, x+1/2, z+1/2'
 '-y+1/2, -x+1/2, z+1/2'
 'y+1/2, -x+1/2, -z+1/2'
 '-y+1/2, x+1/2, -z+1/2'
 'x+1/2, z+1/2, y+1/2'
 '-x+1/2, z+1/2, -y+1/2'
 '-x+1/2, -z+1/2, y+1/2'
 'x+1/2, -z+1/2, -y+1/2'
 'z+1/2, y+1/2, x+1/2'
 'z+1/2, -y+1/2, -x+1/2'
 '-z+1/2, y+1/2, -x+1/2'
 '-z+1/2, -y+1/2, x+1/2'

_cell_length_a                    21.728
_cell_length_b                    21.728
_cell_length_c                    21.728
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      10257.6
_cell_formula_units_Z             2
_cell_measurement_reflns_used     67367
_cell_measurement_temperature     120.0
_cell_measurement_theta_max       75.9040
_cell_measurement_theta_min       3.5210
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     5.275
_exptl_absorpt_correction_T_max   0.4717
_exptl_absorpt_correction_T_min   0.3174
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1055 before and 0.0880 after correction.
The Ratio of minimum to maximum transmission is 0.6729.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details    ?
_exptl_crystal_colour             yellow
_exptl_crystal_colour_primary     yellow
_exptl_crystal_density_diffrn     2.033
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_description        block
_exptl_crystal_F_000              6408
_exptl_crystal_preparation        ?
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of acetonitrile and diisopropyl ether by vapour diffusion'
_exptl_crystal_size_max           0.2923
_exptl_crystal_size_mid           0.1923
_exptl_crystal_size_min           0.1339
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0792
_diffrn_reflns_av_unetI/netI      0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max        27
_diffrn_reflns_limit_h_min        -26
_diffrn_reflns_limit_k_max        25
_diffrn_reflns_limit_k_min        -27
_diffrn_reflns_limit_l_max        27
_diffrn_reflns_limit_l_min        -27
_diffrn_reflns_number             179104
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full         67.679
_diffrn_reflns_theta_max          76.323
_diffrn_reflns_theta_min          4.550
_diffrn_ambient_environment       N~2~
_diffrn_ambient_temperature       120.0
_diffrn_detector                  'CCD plate'
_diffrn_detector_area_resol_mean  5.1574
_diffrn_detector_type             Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -113.00  -21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -38.0000 -120.0000 92

#__ type_ start__ end____ width___ exp.time_
  2 omega  -65.00   26.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   57.0000  150.0000 91

#__ type_ start__ end____ width___ exp.time_
  3 omega  -93.00  -67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686 -146.0000  128.0000 26

#__ type_ start__ end____ width___ exp.time_
  4 omega -113.00  -18.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000    0.0000 95

#__ type_ start__ end____ width___ exp.time_
  5 omega  -73.00  -14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  125.0000  120.0000 59

#__ type_ start__ end____ width___ exp.time_
  6 omega   46.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -125.0000  -30.0000 47

#__ type_ start__ end____ width___ exp.time_
  7 omega   56.00   82.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
  8 omega   89.00  137.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000 -180.0000 48

#__ type_ start__ end____ width___ exp.time_
  9 omega  109.00  135.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 10 omega   44.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 11 omega   86.00  122.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   48.0000  -37.8939 36

#__ type_ start__ end____ width___ exp.time_
 12 omega   92.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   90.0000 82

#__ type_ start__ end____ width___ exp.time_
 13 omega   44.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 14 omega   80.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 15 omega   38.00   73.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  120.0000 35

#__ type_ start__ end____ width___ exp.time_
 16 omega   79.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  150.0000 37

#__ type_ start__ end____ width___ exp.time_
 17 omega   89.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -60.0000 32

#__ type_ start__ end____ width___ exp.time_
 18 omega   40.00   72.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -60.0000 32

#__ type_ start__ end____ width___ exp.time_
 19 omega   83.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -30.0000 30

#__ type_ start__ end____ width___ exp.time_
 20 omega   88.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
 21 omega   39.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 30

#__ type_ start__ end____ width___ exp.time_
 22 omega   85.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 36

#__ type_ start__ end____ width___ exp.time_
 23 omega  131.00  168.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   48.0000  -37.8939 37

#__ type_ start__ end____ width___ exp.time_
 24 omega   92.00  141.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 49

#__ type_ start__ end____ width___ exp.time_
 25 omega   40.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -90.0000 29

#__ type_ start__ end____ width___ exp.time_
 26 omega   64.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 41

#__ type_ start__ end____ width___ exp.time_
 27 omega   42.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  120.0000 55

#__ type_ start__ end____ width___ exp.time_
 28 omega  107.00  135.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  120.0000 28

#__ type_ start__ end____ width___ exp.time_
 29 omega   51.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   90.0000 30

#__ type_ start__ end____ width___ exp.time_
 30 omega   96.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
 31 omega   91.00  136.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 45

#__ type_ start__ end____ width___ exp.time_
 32 omega   95.00  130.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000   90.0000 35

#__ type_ start__ end____ width___ exp.time_
 33 omega  143.00  169.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   70.0000  -96.0346 26

#__ type_ start__ end____ width___ exp.time_
 34 omega   87.00  159.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 72

#__ type_ start__ end____ width___ exp.time_
 35 omega  140.00  165.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
 36 omega   37.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 51

#__ type_ start__ end____ width___ exp.time_
 37 omega   93.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   49.0000   -4.3165 85

#__ type_ start__ end____ width___ exp.time_
 38 omega   51.00   77.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
 39 omega  104.00  130.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   70.0000  -96.0346 26

#__ type_ start__ end____ width___ exp.time_
 40 omega   48.00   85.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -30.0000 37

#__ type_ start__ end____ width___ exp.time_
 41 omega   96.00  169.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  150.0000 73

#__ type_ start__ end____ width___ exp.time_
 42 omega   72.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
 43 omega  142.00  168.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 44 omega   67.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  -30.0000 72

#__ type_ start__ end____ width___ exp.time_
 45 omega   91.00  134.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -120.0000 43

#__ type_ start__ end____ width___ exp.time_
 46 omega   64.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   30.0000 51

#__ type_ start__ end____ width___ exp.time_
 47 omega   40.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 65

#__ type_ start__ end____ width___ exp.time_
 48 omega  143.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   30.0000 33

#__ type_ start__ end____ width___ exp.time_
 49 omega   36.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 50 omega   77.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 51 omega   95.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 52 omega  141.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000    0.0000 36

#__ type_ start__ end____ width___ exp.time_
 53 omega   41.00   66.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 54 omega   93.00  118.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 55 omega   44.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 56 omega   62.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
 57 omega  113.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 58 omega  137.00  163.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 59 omega  129.00  154.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000   30.0000 25

#__ type_ start__ end____ width___ exp.time_
 60 omega   97.00  149.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  120.0000 52

#__ type_ start__ end____ width___ exp.time_
 61 omega  103.00  129.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 62 omega   54.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   90.0000 37

#__ type_ start__ end____ width___ exp.time_
 63 omega  142.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   60.0000 36

#__ type_ start__ end____ width___ exp.time_
 64 omega   51.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -53.0000    8.8022 52

#__ type_ start__ end____ width___ exp.time_
 65 omega   75.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
 66 omega   40.00   65.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
 67 omega   82.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 39

#__ type_ start__ end____ width___ exp.time_
 68 omega   96.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
 69 omega   96.00  148.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000 -150.0000 52

#__ type_ start__ end____ width___ exp.time_
 70 omega   85.00  146.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -89.0000 -106.1944 61
;
_diffrn_measurement_device        'four-circle diffractometer'
_diffrn_measurement_device_type   'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method        'ω scans'
_diffrn_orient_matrix_UB_11       -0.0232989000
_diffrn_orient_matrix_UB_12       -0.0212352000
_diffrn_orient_matrix_UB_13       0.0635406000
_diffrn_orient_matrix_UB_21       -0.0546590000
_diffrn_orient_matrix_UB_22       -0.0328420000
_diffrn_orient_matrix_UB_23       -0.0310063000
_diffrn_orient_matrix_UB_31       0.0386858000
_diffrn_orient_matrix_UB_32       -0.0591287000
_diffrn_orient_matrix_UB_33       -0.0054915000
_diffrn_radiation_monochromator   mirror
_diffrn_radiation_probe           x-ray
_diffrn_radiation_type            CuK\a
_diffrn_radiation_wavelength      1.54178
_diffrn_source                    'sealed X-ray tube'
_diffrn_source_current            0.8
_diffrn_source_type               'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage            50
_diffrn_special_details           ?
_diffrn_standards_number          0
_reflns_Friedel_coverage          0.845
_reflns_Friedel_fraction_full     1.000
_reflns_Friedel_fraction_max      0.996
_reflns_number_gt                 3584
_reflns_number_total              3595
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression      'I > 2σ(I)'
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'ShelXL (Sheldrick, 2015)'
_computing_structure_solution     'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max          1.995
_refine_diff_density_min          -1.444
_refine_diff_density_rms          0.331
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    0.50(2)
_refine_ls_extinction_coef        0.0074(13)
_refine_ls_extinction_expression  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method      'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref    1.976
_refine_ls_hydrogen_treatment     mixed
_refine_ls_matrix_type            full
_refine_ls_number_parameters      213
_refine_ls_number_reflns          3595
_refine_ls_number_restraints      79
_refine_ls_R_factor_all           0.1452
_refine_ls_R_factor_gt            0.1451
_refine_ls_restrained_S_all       1.986
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.3653
_refine_ls_wR_factor_ref          0.3656
_refine_special_details
;
The crystals desolvated instantly when removed from the mother liquor.  An aliquot of mother liquor was transferred by pipette to a shallow well microscope slide.  A crystal was pushed from solvent into Paratone oil then rapidly mounted on the diffractometer to prevent further decomposition.


Both the tetrahedral cage and the associated hexafluorophosphate anions were located easily from a difference Fourier map and refined without using restraints.

When these had been identified it was clear that two regions of residual electron density remained which corresponded with a further tetrahedral chemical species, one inside the cage, one outside.  On the basis of the chemical synthesis this was identified as perchlorate.  Symmetry considerations require that there be, in the asymmetric unit, one crystallographically unique ammonium site per asymmetric unit.  This balances with two partial perchlorate anions.  Least squares restraints were used to control the geometry of the ammonium and perchlorate sites.  The perchlorate sites were modelled as disordered on the basis of appropriate residual electron density peaks.

The SQUEEZE routine of PLATON was then used to account for 1632 electrons per unit cell, which approximately corresponds with four molecules of acetonitrile per asymmetric unit.

The SHELX weighting scheme could not be optimized.


#===============================================================================
>>> The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
084_ALERT_3_B High wR2 Value (i.e. > 0.25) ...................       0.37 Report

A significant portion of the model is accounted for with SQUEEZE.  The SHELXL weighting
scheme could not be optimized.  wR2 is sensitive to the weighting scheme.

434_ALERT_2_B Short Inter HL..HL Contact F3     ..  F3      ..       2.44 Ang.
434_ALERT_2_B Short Inter HL..HL Contact F3     ..  F3      ..       2.44 Ang.

F atoms located in a difference map

936_ALERT_2_B The Embedded RES File Includes a DAMP Command ..      100.0 Report

Needed to control some U(iso) values

987_ALERT_1_B The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check

Refined as such

#===============================================================================
082_ALERT_2_C High R1 Value ..................................       0.15 Report

Noted

141_ALERT_4_C s.u. on a - Axis Small or Missing ..............    0.00000 Ang.
151_ALERT_1_C No s.u. (esd) Given on Volume ..................     Please Do !
234_ALERT_4_C Large Hirshfeld Difference P1     --  F6      ..       0.16 Ang.
244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors of         Cl1 Check
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0132 Ang.

Noted

420_ALERT_2_C D-H Without Acceptor       N3     --  H3A    ...     Please Check
420_ALERT_2_C D-H Without Acceptor       N3     --  H3B    ...     Please Check

Consequence of SQUEEZE

918_ALERT_3_C Reflection(s) with I(obs) much Smaller I(calc) .          3 Check
#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          6 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         13 Report

Noted

041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ     Please Check
042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
044_ALERT_1_G Calculated and Reported Density Dx  Differ by ..     0.6384 Check
051_ALERT_1_G Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .       6.29 %
068_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...     Please Check

Rounding errors and/or consequence of SQUEEZE

072_ALERT_2_G SHELXL First  Parameter in WGHT  Unusually Large       0.20 Report

Discussed above

172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          1 Report
173_ALERT_4_G The CIF-Embedded .res File Contains DANG Records          1 Report
174_ALERT_4_G The CIF-Embedded .res File Contains FLAT Records          1 Report
176_ALERT_4_G The CIF-Embedded .res File Contains SADI Records          4 Report
178_ALERT_4_G The CIF-Embedded .res File Contains SIMU Records          1 Report
244_ALERT_4_G Low   'Solvent' Ueq as Compared to Neighbors of          P1 Check
302_ALERT_4_G Anion/Solvent Disorder ............ Percentage =         44 Note
432_ALERT_2_G Short Inter X...Y Contact  F5     ..  C8      ..       2.82 Ang.
434_ALERT_2_G Short Inter HL..HL Contact F1     ..  F6      ..       2.70 Ang.
434_ALERT_2_G Short Inter HL..HL Contact F2     ..  F5      ..       2.78 Ang.
434_ALERT_2_G Short Inter HL..HL Contact F3     ..  F5      ..       2.74 Ang.

Noted

605_ALERT_4_G Largest Solvent Accessible VOID in Structure ...        474 A**3

Consequence of SQUEEZE

802_ALERT_4_G CIF Input Record(s) with more than 80 Characters          4 Info
860_ALERT_3_G Number of Least-Squares Restraints .............         79 Note
869_ALERT_4_G ALERTS Related to the use of SQUEEZE Suppressed           ! Info
870_ALERT_4_G ALERTS Related to Twinning Effects Suppressed ..          ! Info
910_ALERT_3_G Missing # of FCF Reflection(s) Below Th(Min) ...          2 Report
961_ALERT_5_G Dataset Contains no Negative Intensities .......     Please Check

Noted

#===============================================================================
;


# SQUEEZE RESULTS (Version =  11015)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.500       489       274 ' '
   2  0.000  0.500  0.000       489       274 ' '
   3  0.000  0.500  0.500       489       275 ' '
   4  0.115  0.115  0.885        10        -2 ' '
   5  0.115  0.885  0.115        10        -2 ' '
   6  0.500  0.000  1.000       489       274 ' '
   7  0.500  0.500  0.000       489       275 ' '
   8  0.500  0.000  0.500       489       274 ' '
   9  0.385  0.385  0.385        10         0 ' '
  10  0.385  0.615  0.615        10        -2 ' '
  11  0.615  0.385  0.615        10        -2 ' '
  12  0.615  0.615  0.385        10        -2 ' '
  13  0.885  0.115  0.115        10        -2 ' '
  14  0.885  0.885  0.885        10         0 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
  _platon_missing_refln_index_h
  _platon_missing_refln_index_k
  _platon_missing_refln_index_l
  _platon_missing_refln_theta
    0    1    1     2.876
    0    0    2     4.069
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details 'Four MeCN per asymmetric unit'



_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(2) 0.50(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
3. Restrained distances
 N3-H3A = N3-H3B
 0.9 with sigma of 0.02
 H3A-H3B
 1.47 with sigma of 0.04
 Cl1-O1A \\sim Cl1-O1
 with sigma of 0.02
 Cl1-O1A \\sim Cl1-O1
 with sigma of 0.02
4. Restrained planarity
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
6. Rigid body (RIGU) restrains
 P1, F1, F2, F3, F4, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, O2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(O1A)=0.33333*(1-FVAR(2))
 Sof(O1)=0.33333*FVAR(2)
 Sof(O2A)=1-FVAR(2)
 Sof(O2)=FVAR(2)
8.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9)
;
_atom_sites_solution_hydrogens    mixed
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Co1 Co 0.34695(6) 0.34695(6) 0.65305(6) 0.0209(6) Uani 1 3 d S T P . .
 N1 N 0.2749(3) 0.3053(3) 0.6206(3) 0.0262(13) Uani 1 1 d . . . . .
 N2 N 0.3843(3) 0.3181(3) 0.5788(3) 0.0232(12) Uani 1 1 d . . . . .
 C1 C 0.4445(3) 0.3222(4) 0.5630(4) 0.0239(15) Uani 1 1 d . . . . .
 H1 H 0.4723 0.3411 0.5910 0.029 Uiso 1 1 calc R . . . .
 C2 C 0.4680(4) 0.2989(4) 0.5057(5) 0.0371(18) Uani 1 1 d . . . . .
 C3 C 0.4266(5) 0.2747(6) 0.4638(4) 0.044(2) Uani 1 1 d . . . . .
 H3 H 0.4394 0.2611 0.4242 0.053 Uiso 1 1 calc R . . . .
 C4 C 0.3634(4) 0.2710(4) 0.4829(4) 0.0368(19) Uani 1 1 d . . . . .
 H4 H 0.3337 0.2551 0.4551 0.044 Uiso 1 1 calc R . . . .
 C5 C 0.3455(4) 0.2892(4) 0.5381(3) 0.0289(15) Uani 1 1 d . . . . .
 C6 C 0.2180(4) 0.3018(4) 0.6468(5) 0.0375(18) Uani 1 1 d . . . . .
 H6 H 0.2120 0.3202 0.6860 0.045 Uiso 1 1 calc R . . . .
 C7 C 0.1702(4) 0.2739(5) 0.6199(4) 0.0360(17) Uani 1 1 d . . . . .
 H7 H 0.1312 0.2733 0.6397 0.043 Uiso 1 1 calc R . . . .
 C8 C 0.1781(4) 0.2452(7) 0.5618(5) 0.053(3) Uani 1 1 d . . . . .
 H8 H 0.1463 0.2213 0.5435 0.064 Uiso 1 1 calc R . . . .
 C9 C 0.2346(5) 0.2536(6) 0.5329(5) 0.042(2) Uani 1 1 d . . . . .
 H9 H 0.2409 0.2389 0.4923 0.050 Uiso 1 1 calc R . . . .
 C10 C 0.2807(4) 0.2831(4) 0.5633(4) 0.032(2) Uani 1 1 d . . . . .
 Cl1 Cl 0.5000 0.5000 0.5000 0.0406(18) Uani 1 12 d DS TU P . .
 O1 O 0.4617(6) 0.4617(6) 0.5383(6) 0.047(8) Uani 0.56(6) 3 d DS TU P A 1
 O1A O 0.4619(8) 0.4619(8) 0.4619(8) 0.13(2) Uani 0.44(6) 3 d DS TU P A 2
 Cl2 Cl 0.0000 0.2500 0.5000 0.0426(10) Uani 1 4 d S TU P . .
 O2 O 0.0485(6) 0.1996(8) 0.4742(5) 0.047(4) Uani 0.56(3) 1 d . U . B 1
 O2A O 0.0652(7) 0.2516(9) 0.4667(7) 0.044(5) Uani 0.44(3) 1 d . U . B 2
 P1 P 0.2503(3) 0.0892(2) 0.6055(2) 0.0854(13) Uani 1 1 d . U . . .
 F1 F 0.2961(7) 0.1365(6) 0.5789(7) 0.095(3) Uani 1 1 d . U . . .
 F2 F 0.3017(10) 0.0626(10) 0.6514(7) 0.121(5) Uani 1 1 d . U . . .
 F3 F 0.2759(11) 0.0458(7) 0.5537(8) 0.119(5) Uani 1 1 d . U . . .
 F4 F 0.2379(8) 0.1298(9) 0.6581(8) 0.117(4) Uani 1 1 d . U . . .
 F5 F 0.2025(9) 0.1177(7) 0.5608(8) 0.110(4) Uani 1 1 d . U . . .
 F6 F 0.2077(9) 0.0453(7) 0.6318(6) 0.107(4) Uani 1 1 d . U . . .
 N3 N 0.3091(5) 0.3091(5) 0.3091(5) 0.095(9) Uani 1 3 d DS T P . .
 H3A H 0.2849(9) 0.2849(9) 0.2849(9) 0.114 Uiso 1 3 d DRS T P . .
 H3B H 0.287(4) 0.312(8) 0.345(3) 0.114 Uiso 1 1 d DR . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Co1 N1 1.941(7) 8_656 ?
 Co1 N1 1.941(7) . ?
 Co1 N1 1.941(7) 11_566 ?
 Co1 N2 1.911(6) 11_566 ?
 Co1 N2 1.911(7) 8_656 ?
 Co1 N2 1.911(6) . ?
 N1 C6 1.362(10) . ?
 N1 C10 1.341(12) . ?
 N2 C1 1.355(9) . ?
 N2 C5 1.373(9) . ?
 C1 H1 0.9500 . ?
 C1 C2 1.438(13) . ?
 C2 C2 1.414(16) 3_656 ?
 C2 C3 1.383(13) . ?
 C3 H3 0.9500 . ?
 C3 C4 1.436(12) . ?
 C4 H4 0.9500 . ?
 C4 C5 1.322(10) . ?
 C5 C10 1.516(11) . ?
 C6 H6 0.9500 . ?
 C6 C7 1.337(14) . ?
 C7 H7 0.9500 . ?
 C7 C8 1.420(11) . ?
 C8 H8 0.9500 . ?
 C8 C9 1.391(16) . ?
 C9 H9 0.9500 . ?
 C9 C10 1.360(15) . ?
 Cl1 O1 1.44(2) . ?
 Cl1 O1 1.44(2) 3_656 ?
 Cl1 O1 1.44(2) 4_566 ?
 Cl1 O1 1.44(2) 2_665 ?
 Cl1 O1A 1.43(3) 3_656 ?
 Cl1 O1A 1.43(3) 2_665 ?
 Cl1 O1A 1.43(3) 4_566 ?
 Cl1 O1A 1.43(3) . ?
 Cl2 O2 1.620(14) 3_556 ?
 Cl2 O2 1.620(14) 24 ?
 Cl2 O2 1.620(14) . ?
 Cl2 O2 1.620(14) 22_455 ?
 Cl2 O2A 1.591(16) 22_455 ?
 Cl2 O2A 1.591(16) 24 ?
 Cl2 O2A 1.591(16) 3_556 ?
 Cl2 O2A 1.591(16) . ?
 P1 F1 1.544(16) . ?
 P1 F2 1.61(2) . ?
 P1 F3 1.570(18) . ?
 P1 F4 1.469(17) . ?
 P1 F5 1.550(19) . ?
 P1 F6 1.445(17) . ?
 N3 H3A 0.91(3) . ?
 N3 H3B 0.91(3) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 N1 Co1 N1 94.9(3) 8_656 . ?
 N1 Co1 N1 94.9(3) 11_566 8_656 ?
 N1 Co1 N1 94.9(3) 11_566 . ?
 N2 Co1 N1 83.3(3) 11_566 11_566 ?
 N2 Co1 N1 176.2(3) 11_566 8_656 ?
 N2 Co1 N1 83.3(3) 8_656 8_656 ?
 N2 Co1 N1 88.6(3) . 8_656 ?
 N2 Co1 N1 88.6(3) 11_566 . ?
 N2 Co1 N1 176.2(3) 8_656 . ?
 N2 Co1 N1 83.3(3) . . ?
 N2 Co1 N1 176.2(3) . 11_566 ?
 N2 Co1 N1 88.6(3) 8_656 11_566 ?
 N2 Co1 N2 93.3(2) 8_656 11_566 ?
 N2 Co1 N2 93.3(2) . 11_566 ?
 N2 Co1 N2 93.3(2) . 8_656 ?
 C6 N1 Co1 127.3(6) . . ?
 C10 N1 Co1 115.4(6) . . ?
 C10 N1 C6 116.9(8) . . ?
 C1 N2 Co1 127.0(5) . . ?
 C1 N2 C5 117.4(7) . . ?
 C5 N2 Co1 115.6(5) . . ?
 N2 C1 H1 118.7 . . ?
 N2 C1 C2 122.6(7) . . ?
 C2 C1 H1 118.7 . . ?
 C2 C2 C1 120.0(10) 3_656 . ?
 C3 C2 C1 118.3(8) . . ?
 C3 C2 C2 121.7(12) . 3_656 ?
 C2 C3 H3 121.6 . . ?
 C2 C3 C4 116.9(8) . . ?
 C4 C3 H3 121.6 . . ?
 C3 C4 H4 119.1 . . ?
 C5 C4 C3 121.8(8) . . ?
 C5 C4 H4 119.1 . . ?
 N2 C5 C10 112.2(7) . . ?
 C4 C5 N2 122.7(7) . . ?
 C4 C5 C10 125.1(8) . . ?
 N1 C6 H6 118.4 . . ?
 C7 C6 N1 123.3(8) . . ?
 C7 C6 H6 118.4 . . ?
 C6 C7 H7 120.2 . . ?
 C6 C7 C8 119.6(8) . . ?
 C8 C7 H7 120.2 . . ?
 C7 C8 H8 121.6 . . ?
 C9 C8 C7 116.7(9) . . ?
 C9 C8 H8 121.6 . . ?
 C8 C9 H9 120.2 . . ?
 C10 C9 C8 119.6(9) . . ?
 C10 C9 H9 120.2 . . ?
 N1 C10 C5 113.0(8) . . ?
 N1 C10 C9 123.4(8) . . ?
 C9 C10 C5 123.4(9) . . ?
 O1 Cl1 O1 109.471(1) 3_656 4_566 ?
 O1 Cl1 O1 109.471(1) 2_665 . ?
 O1 Cl1 O1 109.471(9) 2_665 3_656 ?
 O1 Cl1 O1 109.471(4) 2_665 4_566 ?
 O1 Cl1 O1 109.5 4_566 . ?
 O1 Cl1 O1 109.471(2) 3_656 . ?
 O1A Cl1 O1A 109.471(10) 2_665 3_656 ?
 O1A Cl1 O1A 109.5 4_566 . ?
 O1A Cl1 O1A 109.471(4) 2_665 4_566 ?
 O1A Cl1 O1A 109.471(1) 2_665 . ?
 O1A Cl1 O1A 109.471(2) 4_566 3_656 ?
 O1A Cl1 O1A 109.471(2) 3_656 . ?
 O2 Cl2 O2 117.2(6) 22_455 . ?
 O2 Cl2 O2 117.2(6) 3_556 22_455 ?
 O2 Cl2 O2 117.2(6) 24 . ?
 O2 Cl2 O2 95.0(11) 24 22_455 ?
 O2 Cl2 O2 117.2(6) 24 3_556 ?
 O2 Cl2 O2 95.0(11) 3_556 . ?
 O2A Cl2 O2A 90.03(3) . 22_455 ?
 O2A Cl2 O2A 177.6(14) . 3_556 ?
 O2A Cl2 O2A 90.03(3) . 24 ?
 O2A Cl2 O2A 90.03(3) 22_455 3_556 ?
 O2A Cl2 O2A 90.03(3) 24 3_556 ?
 O2A Cl2 O2A 177.6(14) 24 22_455 ?
 F1 P1 F2 91.3(10) . . ?
 F1 P1 F3 84.4(9) . . ?
 F1 P1 F5 86.1(9) . . ?
 F3 P1 F2 89.1(10) . . ?
 F4 P1 F1 90.5(9) . . ?
 F4 P1 F2 81.9(11) . . ?
 F4 P1 F3 169.5(12) . . ?
 F4 P1 F5 97.2(11) . . ?
 F5 P1 F2 177.2(11) . . ?
 F5 P1 F3 91.6(10) . . ?
 F6 P1 F1 178.7(9) . . ?
 F6 P1 F2 87.8(10) . . ?
 F6 P1 F3 96.6(9) . . ?
 F6 P1 F4 88.4(9) . . ?
 F6 P1 F5 94.8(11) . . ?
 H3A N3 H3B 104(6) . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Co1 N1 C6 C7 177.4(7) . . . . ?
 Co1 N1 C10 C5 6.5(9) . . . . ?
 Co1 N1 C10 C9 -178.8(8) . . . . ?
 Co1 N2 C1 C2 -179.9(6) . . . . ?
 Co1 N2 C5 C4 174.6(8) . . . . ?
 Co1 N2 C5 C10 -3.3(8) . . . . ?
 N1 C6 C7 C8 1.1(15) . . . . ?
 N2 C1 C2 C2 -173.7(6) . . . 3_656 ?
 N2 C1 C2 C3 3.6(13) . . . . ?
 N2 C5 C10 N1 -2.1(10) . . . . ?
 N2 C5 C10 C9 -176.9(9) . . . . ?
 C1 N2 C5 C4 -6.7(12) . . . . ?
 C1 N2 C5 C10 175.4(7) . . . . ?
 C1 C2 C3 C4 -4.0(15) . . . . ?
 C2 C2 C3 C4 173.4(9) 3_656 . . . ?
 C2 C3 C4 C5 -0.8(16) . . . . ?
 C3 C4 C5 N2 6.4(15) . . . . ?
 C3 C4 C5 C10 -175.9(10) . . . . ?
 C4 C5 C10 N1 -180.0(9) . . . . ?
 C4 C5 C10 C9 5.3(15) . . . . ?
 C5 N2 C1 C2 1.6(11) . . . . ?
 C6 N1 C10 C5 179.8(7) . . . . ?
 C6 N1 C10 C9 -5.4(13) . . . . ?
 C6 C7 C8 C9 -6.7(17) . . . . ?
 C7 C8 C9 C10 6.3(18) . . . . ?
 C8 C9 C10 N1 -0.2(17) . . . . ?
 C8 C9 C10 C5 173.9(11) . . . . ?
 C10 N1 C6 C7 5.0(12) . . . . ?

_shelx_SHELXL_version_number      '2014/7'
loop_
  _exptl_crystal_face_index_h
  _exptl_crystal_face_index_k
  _exptl_crystal_face_index_l
  _exptl_crystal_face_perp_dist
  _exptl_oxdiff_crystal_face_indexfrac_h
  _exptl_oxdiff_crystal_face_indexfrac_k
  _exptl_oxdiff_crystal_face_indexfrac_l
  _exptl_oxdiff_crystal_face_x
  _exptl_oxdiff_crystal_face_y
  _exptl_oxdiff_crystal_face_z
 -2 -7 12 0.1038 -2.0000 -6.9981 12.0004 0.9577 -0.0329 0.2705
 -6 9 -9 0.0916 -6.0002 8.9985 -8.9991 -0.6231 0.3115 -0.7148
 1 -10 10 0.0950 1.0002 -9.9982 9.9999 0.8244 -0.0364 0.5750
 12 2 7 0.0928 11.9997 2.0003 6.9982 0.1226 -0.9386 0.3075
 4 5 -13 0.0804 4.0002 4.9982 -13.0008 -1.0254 0.0203 -0.0694
 -2 11 -9 0.0928 -2.0004 10.9982 -8.9997 -0.7588 0.0272 -0.6783
 -9 8 7 0.1431 -9.0008 8.0002 7.0017 0.4847 0.0121 -0.8597
 -7 -10 -7 0.0670 -6.9991 -9.9997 -6.9991 -0.0693 0.9280 0.3589
 -12 -2 -7 0.0928 -11.9997 -2.0003 -6.9982 -0.1226 0.9386 -0.3075
 9 -11 0 0.1101 9.0007 -10.9993 -0.0016 0.0238 -0.1307 0.9986
 5 -13 -3 0.1010 5.0009 -12.9993 -3.0010 -0.0312 0.2466 0.9786
 6 -2 13 0.0898 5.9996 -1.9986 12.9992 0.7286 -0.6654 0.2789
 7 -3 12 0.0913 6.9998 -2.9987 11.9990 0.6630 -0.6562 0.3822
 7 10 7 0.0670 6.9991 9.9997 6.9991 0.0693 -0.9280 -0.3589
 1 -1 -14 0.0736 1.0006 -1.0014 -14.0004 -0.8916 0.4123 0.1748
 -1 -7 -12 0.0726 -0.9991 -7.0006 -12.0001 -0.5906 0.6566 0.4412
 -6 -11 7 0.0947 -5.9996 -10.9982 7.0009 0.8182 0.4721 0.3798
 9 -9 -7 0.1026 9.0009 -9.0002 -7.0017 -0.4635 0.0207 0.9188
 7 9 -8 0.0708 6.9998 8.9983 -8.0012 -0.8626 -0.4300 -0.2173
 -8 11 1 0.1197 -8.0008 10.9994 1.0014 0.0165 0.0450 -0.9654

_olex2_date_sample_data_collection 2016-03-24
_olex2_date_sample_submission     2016-03-18
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id MB4085
_olex2_submission_special_instructions 'No special instructions were received'
loop_
  _twin_individual_id
  _twin_individual_mass_fraction_refined
 1 0.50(2)
 2 0.50(2)

_vrf_CHEMW03_pl16010_sq
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Please see the _refine_special_details section of the CIF
;
