data_cx1846
_audit_creation_date               2020-03-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_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. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C56 H48 N4, 4(Cl), 2(C3 H6 O), 6(H2 O)'
_chemical_formula_sum              'C62 H72 Cl4 N4 O8'
_chemical_formula_weight           1143.03
_chemical_melting_point            ?
_chemical_oxdiff_formula           C104H96Cl4N36O16
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'
 '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'

_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        'monoclinic'
_space_group_IT_number             14
_space_group_name_H-M_alt          'P 1 21/c 1'
_space_group_name_Hall             '-P 2ybc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'

_cell_length_a                     15.6756(7)
_cell_length_b                     11.7857(4)
_cell_length_c                     16.4783(8)
_cell_angle_alpha                  90
_cell_angle_beta                   91.124(4)
_cell_angle_gamma                  90
_cell_volume                       3043.7(2)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      3054
_cell_measurement_temperature      100.01(10)
_cell_measurement_theta_max        51.5280
_cell_measurement_theta_min        2.8110
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.215
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.76560
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              yellow
_exptl_crystal_colour_primary      yellow
_exptl_crystal_density_diffrn      1.247
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         plate
_exptl_crystal_F_000               1208
loop_
  _exptl_crystal_face_index_h
  _exptl_crystal_face_index_k
  _exptl_crystal_face_index_l
  _exptl_crystal_face_perp_dist
 1 -1 -1 0.0675
 -1 1 1 0.0430
 -1 0 0 0.0150
 1 0 0 0.0056
 0 -1 1 0.0357
 0 1 -1 0.0288

_exptl_crystal_recrystallization_method 
 'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max            0.171
_exptl_crystal_size_mid            0.065
_exptl_crystal_size_min            0.021
loop_
  _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
 0.9988 -0.9998 -1.0000 -0.1346 -0.1281 -0.0239
 -0.9988 0.9998 1.0000 0.1346 0.1281 0.0239
 -1.0002 0.0006 -0.0003 -0.0222 0.0950 0.0121
 1.0002 -0.0006 0.0003 0.0222 -0.0950 -0.0121
 -0.0022 -0.9993 0.9990 -0.0569 -0.0338 0.1463
 0.0022 0.9993 -0.9990 0.0569 0.0338 -0.1463

_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0668
_diffrn_reflns_av_unetI/netI       0.0775
_diffrn_reflns_Laue_measured_fraction_full  0.982
_diffrn_reflns_Laue_measured_fraction_max  0.982
_diffrn_reflns_limit_h_max         15
_diffrn_reflns_limit_h_min         -15
_diffrn_reflns_limit_k_max         11
_diffrn_reflns_limit_k_min         -11
_diffrn_reflns_limit_l_max         16
_diffrn_reflns_limit_l_min         -16
_diffrn_reflns_number              11277
_diffrn_reflns_point_group_measured_fraction_full  0.982
_diffrn_reflns_point_group_measured_fraction_max  0.982
_diffrn_reflns_theta_full          51.830
_diffrn_reflns_theta_max           51.830
_diffrn_reflns_theta_min           2.819
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        100.01(10)
_diffrn_detector                   'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean   10.0000
_diffrn_detector_type              HyPix
_diffrn_measured_fraction_theta_full  0.982
_diffrn_measured_fraction_theta_max  0.982
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     17.00  52.00   0.50   20.00    --    0.86  80.00  79.00   70
  2  ω     56.00  81.00   0.50   80.00    --   56.43  80.00  79.00   50
  3  ω     71.00  97.00   0.50   80.00    --   56.43  57.00  30.00   52
  4  ω      0.00  25.00   0.50   20.00    --    0.86 -80.00 -44.00   50
  5  ω    -15.00  79.00   0.50   80.00    --   56.43 -80.00 -44.00  188
  6  ω    -14.00  17.00   0.50   80.00    --   56.43 -19.00   0.00   62
  7  ω    -18.00  12.00   0.50   80.00    --   56.43 -19.00 -30.00   60
  8  ω    -18.00  17.00   0.50   80.00    --   56.43 -19.00  30.00   70
  9  ω    -18.00  17.00   0.50   80.00    --   56.43 -19.00 120.00   70
 10  ω    -18.00  17.00   0.50   80.00    --   56.43 -19.00 150.00   70
 11  ω    -40.00 -13.00   0.50   20.00    --    0.86 -80.00 -44.00   54
 12  ω    -17.00   8.00   0.50   20.00    --    0.86 -99.00-180.00   50
 13  ω    -18.00  16.00   0.50   80.00    --   56.43 -19.00-180.00   68
 14  ω    -19.00  21.00   0.50   80.00    --  -54.72  19.00 -90.00   80
 15  ω    -78.00  18.00   0.50   80.00    --  -54.72  80.00  79.00  192
 16  ω   -108.00 -69.00   0.50   80.00    --  -54.72 -80.00 -44.00   78
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type   
 'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        0.0222314000
_diffrn_orient_matrix_UB_12        0.1068330000
_diffrn_orient_matrix_UB_13        0.0499662000
_diffrn_orient_matrix_UB_21        -0.0950059000
_diffrn_orient_matrix_UB_22        0.0336460000
_diffrn_orient_matrix_UB_23        -0.0003883000
_diffrn_orient_matrix_UB_31        -0.0121715000
_diffrn_orient_matrix_UB_32        -0.0673301000
_diffrn_orient_matrix_UB_33        0.0790282000
_diffrn_oxdiff_digest_frames
;
01f7e9f23a64872840e109be5c6fd5630800025e289
;
_diffrn_oxdiff_digest_hkl
;
01757786dbb831b082ddfea8d85a581b6e3bb5
;
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  2196
_reflns_number_total               3312
_reflns_odcompleteness_completeness  100.00
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       50.38
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection         'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction          'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'XL (Sheldrick, 2008)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.417
_refine_diff_density_min           -0.416
_refine_diff_density_rms           0.061
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.003
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       371
_refine_ls_number_reflns           3312
_refine_ls_number_restraints       2
_refine_ls_R_factor_all            0.1010
_refine_ls_R_factor_gt             0.0554
_refine_ls_restrained_S_all        1.005
_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)+(0.0939P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1311
_refine_ls_wR_factor_ref           0.1523
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O3-H3A = O3-H3B
 0.98 with sigma of 0.02
3.a Free rotating group:
 H3A(H3B), O4(H4A,H4B)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C22(H22A,H22B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24),
  C25(H25), C27(H27), C28(H28)
3.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_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
 N1 N -0.2026(3) 0.2737(3) 0.0394(2) 0.0325(10) Uani 1 1 d . . . . .
 N2 N 0.4427(2) 0.3380(3) 0.7914(2) 0.0303(10) Uani 1 1 d . . . . .
 C1 C -0.2792(3) 0.2832(3) -0.0153(3) 0.0310(12) Uani 1 1 d . . . . .
 H1A H -0.307356 0.210130 -0.019848 0.037 Uiso 1 1 calc R . . . .
 H1B H -0.262213 0.306637 -0.069005 0.037 Uiso 1 1 calc R . . . .
 C2 C -0.1365(3) 0.3448(4) 0.0306(3) 0.0386(13) Uani 1 1 d . . . . .
 H2 H -0.135711 0.393819 -0.013607 0.046 Uiso 1 1 calc R . . . .
 C3 C -0.0706(3) 0.3462(3) 0.0855(3) 0.0368(13) Uani 1 1 d . . . . .
 H3 H -0.025032 0.395191 0.077567 0.044 Uiso 1 1 calc R . . . .
 C4 C -0.0699(3) 0.2758(3) 0.1534(3) 0.0307(12) Uani 1 1 d . . . . .
 C5 C -0.1378(3) 0.2000(3) 0.1586(3) 0.0391(13) Uani 1 1 d . . . . .
 H5 H -0.139151 0.148337 0.201206 0.047 Uiso 1 1 calc R . . . .
 C6 C -0.2026(3) 0.2007(3) 0.1017(3) 0.0356(13) Uani 1 1 d . . . . .
 H6 H -0.247385 0.149576 0.106389 0.043 Uiso 1 1 calc R . . . .
 C7 C -0.0020(3) 0.2866(3) 0.2132(3) 0.0353(13) Uani 1 1 d . . . . .
 H7 H 0.041766 0.336962 0.201799 0.042 Uiso 1 1 calc R . . . .
 C8 C 0.0035(3) 0.2306(3) 0.2836(3) 0.0346(12) Uani 1 1 d . . . . .
 H8 H -0.037753 0.175748 0.293197 0.042 Uiso 1 1 calc R . . . .
 C9 C 0.0685(3) 0.2482(3) 0.3467(3) 0.0328(13) Uani 1 1 d . . . . .
 C10 C 0.1296(3) 0.3345(3) 0.3422(3) 0.0387(13) Uani 1 1 d . . . . .
 H10 H 0.130298 0.381685 0.296955 0.046 Uiso 1 1 calc R . . . .
 C11 C 0.1883(3) 0.3498(4) 0.4039(3) 0.0427(14) Uani 1 1 d . . . . .
 H11 H 0.227381 0.408867 0.400101 0.051 Uiso 1 1 calc R . . . .
 C12 C 0.1915(3) 0.2805(4) 0.4717(3) 0.0340(12) Uani 1 1 d . . . . .
 C13 C 0.1320(4) 0.1930(4) 0.4760(3) 0.0446(14) Uani 1 1 d . . . . .
 H13 H 0.132788 0.144295 0.520368 0.054 Uiso 1 1 calc R . . . .
 C14 C 0.0716(3) 0.1784(3) 0.4144(3) 0.0409(14) Uani 1 1 d . . . . .
 H14 H 0.032012 0.119994 0.418630 0.049 Uiso 1 1 calc R . . . .
 C15 C 0.2573(3) 0.3050(4) 0.5351(3) 0.0429(14) Uani 1 1 d . . . . .
 H15 H 0.293792 0.365718 0.525836 0.051 Uiso 1 1 calc R . . . .
 C16 C 0.2686(3) 0.2492(3) 0.6024(3) 0.0405(14) Uani 1 1 d . . . . .
 H16 H 0.233942 0.186589 0.611320 0.049 Uiso 1 1 calc R . . . .
 C17 C 0.3329(3) 0.2789(3) 0.6658(3) 0.0338(13) Uani 1 1 d . . . . .
 C18 C 0.3896(4) 0.3708(4) 0.6601(3) 0.0457(14) Uani 1 1 d . . . . .
 H18 H 0.390851 0.412953 0.612426 0.055 Uiso 1 1 calc R . . . .
 C19 C 0.4428(3) 0.3991(4) 0.7235(3) 0.0426(14) Uani 1 1 d . . . . .
 H19 H 0.479087 0.461114 0.719177 0.051 Uiso 1 1 calc R . . . .
 C20 C 0.3920(3) 0.2475(3) 0.7974(3) 0.0426(14) Uani 1 1 d . . . . .
 H20 H 0.393597 0.204619 0.844768 0.051 Uiso 1 1 calc R . . . .
 C21 C 0.3387(3) 0.2171(4) 0.7361(3) 0.0420(14) Uani 1 1 d . . . . .
 H21 H 0.305018 0.152719 0.741719 0.050 Uiso 1 1 calc R . . . .
 C22 C 0.4933(3) 0.3788(3) 0.8640(3) 0.0349(12) Uani 1 1 d . . . . .
 H22A H 0.547054 0.410826 0.846832 0.042 Uiso 1 1 calc R . . . .
 H22B H 0.505577 0.315818 0.900226 0.042 Uiso 1 1 calc R . . . .
 C23 C 0.4423(3) 0.4676(3) 0.9074(3) 0.0294(11) Uani 1 1 d . . . . .
 C24 C 0.4486(3) 0.5815(3) 0.8866(3) 0.0355(13) Uani 1 1 d . . . . .
 H24 H 0.487670 0.603901 0.847908 0.043 Uiso 1 1 calc R . . . .
 C25 C 0.3977(3) 0.6618(3) 0.9226(3) 0.0368(13) Uani 1 1 d . . . . .
 H25 H 0.402405 0.737709 0.907887 0.044 Uiso 1 1 calc R . . . .
 C26 C 0.3398(3) 0.6301(3) 0.9802(3) 0.0283(11) Uani 1 1 d . . . . .
 C27 C 0.3348(3) 0.5171(3) 1.0039(3) 0.0339(12) Uani 1 1 d . . . . .
 H27 H 0.297775 0.495218 1.044455 0.041 Uiso 1 1 calc R . . . .
 C28 C 0.3860(3) 0.4369(3) 0.9661(3) 0.0353(13) Uani 1 1 d . . . . .
 H28 H 0.381840 0.361052 0.981036 0.042 Uiso 1 1 calc R . . . .
 Cl1 Cl 0.14772(7) 0.51127(7) 0.15508(6) 0.0309(4) Uani 1 1 d . . . . .
 Cl2 Cl 0.38179(8) 0.51729(8) 0.39647(8) 0.0496(4) Uani 1 1 d . . . . .
 O1 O 0.1981(5) 0.5832(4) 0.5939(5) 0.202(4) Uani 1 1 d . . . . .
 C29 C 0.1534(7) 0.5310(5) 0.6366(7) 0.109(3) Uani 1 1 d . . . . .
 C30 C 0.0700(6) 0.4886(6) 0.6063(6) 0.119(3) Uani 1 1 d . . . . .
 H30A H 0.056408 0.523242 0.554888 0.178 Uiso 1 1 calc GR . . . .
 H30B H 0.026663 0.507378 0.644453 0.178 Uiso 1 1 calc GR . . . .
 H30C H 0.072575 0.407766 0.599833 0.178 Uiso 1 1 calc GR . . . .
 C31 C 0.1811(6) 0.5028(6) 0.7209(7) 0.133(4) Uani 1 1 d . . . . .
 H31A H 0.193477 0.423148 0.724631 0.199 Uiso 1 1 calc GR . . . .
 H31B H 0.136418 0.521499 0.757588 0.199 Uiso 1 1 calc GR . . . .
 H31C H 0.231419 0.545475 0.735022 0.199 Uiso 1 1 calc GR . . . .
 O2 O 0.3225(3) 0.6093(3) 0.2251(3) 0.0600(12) Uani 1 1 d . . . . .
 H2A H 0.278(4) 0.581(4) 0.214(4) 0.06(2) Uiso 1 1 d . . . . .
 H2B H 0.331(6) 0.570(7) 0.278(6) 0.17(4) Uiso 1 1 d . . . . .
 O3 O 0.5377(4) 0.3739(4) 0.4487(3) 0.1173(19) Uani 1 1 d D . . . .
 H3A H 0.498183 0.439156 0.435019 0.176 Uiso 1 1 d D . . . .
 H3B H 0.485802 0.345046 0.484031 0.176 Uiso 1 1 d DG . . . .
 O4 O 0.3894(3) 0.6671(3) 0.7051(2) 0.0784(14) Uani 1 1 d . . . . .
 H4A H 0.354091 0.719577 0.715447 0.118 Uiso 1 1 d G . . . .
 H4B H 0.380193 0.651671 0.655276 0.118 Uiso 1 1 d G . . . .


_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
 N1 C1 1.490(6) . ?
 N1 C2 1.343(6) . ?
 N1 C6 1.340(5) . ?
 N2 C19 1.331(6) . ?
 N2 C20 1.335(5) . ?
 N2 C22 1.501(6) . ?
 C1 H1A 0.9700 . ?
 C1 H1B 0.9700 . ?
 C1 C26 1.517(6) 3_566 ?
 C2 H2 0.9300 . ?
 C2 C3 1.359(7) . ?
 C3 H3 0.9300 . ?
 C3 C4 1.393(6) . ?
 C4 C5 1.394(6) . ?
 C4 C7 1.442(7) . ?
 C5 H5 0.9300 . ?
 C5 C6 1.368(7) . ?
 C6 H6 0.9300 . ?
 C7 H7 0.9300 . ?
 C7 C8 1.336(6) . ?
 C8 H8 0.9300 . ?
 C8 C9 1.455(7) . ?
 C9 C10 1.400(6) . ?
 C9 C14 1.387(6) . ?
 C10 H10 0.9300 . ?
 C10 C11 1.371(7) . ?
 C11 H11 0.9300 . ?
 C11 C12 1.384(7) . ?
 C12 C13 1.393(7) . ?
 C12 C15 1.483(7) . ?
 C13 H13 0.9300 . ?
 C13 C14 1.384(7) . ?
 C14 H14 0.9300 . ?
 C15 H15 0.9300 . ?
 C15 C16 1.298(7) . ?
 C16 H16 0.9300 . ?
 C16 C17 1.479(7) . ?
 C17 C18 1.405(6) . ?
 C17 C21 1.371(6) . ?
 C18 H18 0.9300 . ?
 C18 C19 1.365(7) . ?
 C19 H19 0.9300 . ?
 C20 H20 0.9300 . ?
 C20 C21 1.346(7) . ?
 C21 H21 0.9300 . ?
 C22 H22A 0.9700 . ?
 C22 H22B 0.9700 . ?
 C22 C23 1.506(6) . ?
 C23 C24 1.389(6) . ?
 C23 C28 1.372(6) . ?
 C24 H24 0.9300 . ?
 C24 C25 1.380(6) . ?
 C25 H25 0.9300 . ?
 C25 C26 1.378(6) . ?
 C26 C27 1.390(5) . ?
 C27 H27 0.9300 . ?
 C27 C28 1.394(6) . ?
 C28 H28 0.9300 . ?
 O1 C29 1.176(8) . ?
 C29 C30 1.477(13) . ?
 C29 C31 1.486(12) . ?
 C30 H30A 0.9600 . ?
 C30 H30B 0.9600 . ?
 C30 H30C 0.9600 . ?
 C31 H31A 0.9600 . ?
 C31 H31B 0.9600 . ?
 C31 H31C 0.9600 . ?
 O2 H2A 0.78(6) . ?
 O2 H2B 0.99(9) . ?
 O3 H3A 1.01(2) . ?
 O3 H3B 1.0653 . ?
 O4 H4A 0.8498 . ?
 O4 H4B 0.8501 . ?

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
 C2 N1 C1 120.2(4) . . ?
 C6 N1 C1 120.0(4) . . ?
 C6 N1 C2 119.6(5) . . ?
 C19 N2 C20 120.3(4) . . ?
 C19 N2 C22 119.2(4) . . ?
 C20 N2 C22 120.2(4) . . ?
 N1 C1 H1A 109.9 . . ?
 N1 C1 H1B 109.9 . . ?
 N1 C1 C26 108.9(3) . 3_566 ?
 H1A C1 H1B 108.3 . . ?
 C26 C1 H1A 109.9 3_566 . ?
 C26 C1 H1B 109.9 3_566 . ?
 N1 C2 H2 119.5 . . ?
 N1 C2 C3 120.9(4) . . ?
 C3 C2 H2 119.5 . . ?
 C2 C3 H3 119.3 . . ?
 C2 C3 C4 121.4(4) . . ?
 C4 C3 H3 119.3 . . ?
 C3 C4 C5 115.9(5) . . ?
 C3 C4 C7 119.4(4) . . ?
 C5 C4 C7 124.7(4) . . ?
 C4 C5 H5 119.6 . . ?
 C6 C5 C4 120.8(4) . . ?
 C6 C5 H5 119.6 . . ?
 N1 C6 C5 121.2(4) . . ?
 N1 C6 H6 119.4 . . ?
 C5 C6 H6 119.4 . . ?
 C4 C7 H7 117.1 . . ?
 C8 C7 C4 125.8(4) . . ?
 C8 C7 H7 117.1 . . ?
 C7 C8 H8 117.2 . . ?
 C7 C8 C9 125.6(4) . . ?
 C9 C8 H8 117.2 . . ?
 C10 C9 C8 122.4(4) . . ?
 C14 C9 C8 120.2(4) . . ?
 C14 C9 C10 117.4(5) . . ?
 C9 C10 H10 119.8 . . ?
 C11 C10 C9 120.5(4) . . ?
 C11 C10 H10 119.8 . . ?
 C10 C11 H11 118.9 . . ?
 C10 C11 C12 122.3(4) . . ?
 C12 C11 H11 118.9 . . ?
 C11 C12 C13 117.7(5) . . ?
 C11 C12 C15 117.8(4) . . ?
 C13 C12 C15 124.5(5) . . ?
 C12 C13 H13 119.9 . . ?
 C14 C13 C12 120.3(5) . . ?
 C14 C13 H13 119.9 . . ?
 C9 C14 H14 119.0 . . ?
 C13 C14 C9 121.9(4) . . ?
 C13 C14 H14 119.0 . . ?
 C12 C15 H15 117.1 . . ?
 C16 C15 C12 125.7(5) . . ?
 C16 C15 H15 117.1 . . ?
 C15 C16 H16 117.9 . . ?
 C15 C16 C17 124.3(5) . . ?
 C17 C16 H16 117.9 . . ?
 C18 C17 C16 123.9(5) . . ?
 C21 C17 C16 120.3(4) . . ?
 C21 C17 C18 115.7(5) . . ?
 C17 C18 H18 119.5 . . ?
 C19 C18 C17 121.0(5) . . ?
 C19 C18 H18 119.5 . . ?
 N2 C19 C18 120.1(4) . . ?
 N2 C19 H19 120.0 . . ?
 C18 C19 H19 120.0 . . ?
 N2 C20 H20 119.4 . . ?
 N2 C20 C21 121.3(5) . . ?
 C21 C20 H20 119.4 . . ?
 C17 C21 H21 119.2 . . ?
 C20 C21 C17 121.5(4) . . ?
 C20 C21 H21 119.2 . . ?
 N2 C22 H22A 109.9 . . ?
 N2 C22 H22B 109.9 . . ?
 N2 C22 C23 108.9(4) . . ?
 H22A C22 H22B 108.3 . . ?
 C23 C22 H22A 109.9 . . ?
 C23 C22 H22B 109.9 . . ?
 C24 C23 C22 120.9(4) . . ?
 C28 C23 C22 120.4(4) . . ?
 C28 C23 C24 118.6(4) . . ?
 C23 C24 H24 119.6 . . ?
 C25 C24 C23 120.8(4) . . ?
 C25 C24 H24 119.6 . . ?
 C24 C25 H25 119.8 . . ?
 C26 C25 C24 120.3(4) . . ?
 C26 C25 H25 119.8 . . ?
 C25 C26 C1 120.3(4) . 3_566 ?
 C25 C26 C27 119.7(4) . . ?
 C27 C26 C1 120.0(4) . 3_566 ?
 C26 C27 H27 120.4 . . ?
 C26 C27 C28 119.2(4) . . ?
 C28 C27 H27 120.4 . . ?
 C23 C28 C27 121.4(4) . . ?
 C23 C28 H28 119.3 . . ?
 C27 C28 H28 119.3 . . ?
 O1 C29 C30 120.6(12) . . ?
 O1 C29 C31 120.6(11) . . ?
 C30 C29 C31 118.8(8) . . ?
 C29 C30 H30A 109.5 . . ?
 C29 C30 H30B 109.5 . . ?
 C29 C30 H30C 109.5 . . ?
 H30A C30 H30B 109.5 . . ?
 H30A C30 H30C 109.5 . . ?
 H30B C30 H30C 109.5 . . ?
 C29 C31 H31A 109.5 . . ?
 C29 C31 H31B 109.5 . . ?
 C29 C31 H31C 109.5 . . ?
 H31A C31 H31B 109.5 . . ?
 H31A C31 H31C 109.5 . . ?
 H31B C31 H31C 109.5 . . ?
 H2A O2 H2B 96(6) . . ?
 H3A O3 H3B 83.9 . . ?
 H4A O4 H4B 104.5 . . ?

loop_
  _geom_hbond_atom_site_label_D
  _geom_hbond_atom_site_label_H
  _geom_hbond_atom_site_label_A
  _geom_hbond_distance_DH
  _geom_hbond_distance_HA
  _geom_hbond_distance_DA
  _geom_hbond_angle_DHA
  _geom_hbond_site_symmetry_A
  _geom_hbond_publ_flag
 O4 H4A O2 0.85 2.08 2.858(6) 151.3 4_576 yes
 O4 H4B O3 0.85 2.18 2.842(7) 134.1 3_666 yes

_olex2_date_sample_data_collection  2020-03-04
_olex2_date_sample_submission      2020-03-02
_olex2_diffrn_ambient_temperature_device  'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
 'The crystal was mounted on a MITIGEN holder with Paratone oil'
_olex2_submission_original_sample_id  cx1846
_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  2.266
_oxdiff_exptl_absorpt_empirical_full_min  0.219
_vrf_THETM01_cx1846
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Despite long exposure times, the crystal did not exhibit observable
 intensity to a resolution higher than 0.98 angstrom
;
