 
data_mo_kdm_123_0m_pl
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety           'C17 H16 O3' 
_chemical_formula_sum
 'C17 H16 O3' 
_chemical_formula_weight          268.30

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 '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'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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.
;
 
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                    11.8124(4)
_cell_length_b                    10.5930(4)
_cell_length_c                    11.7212(4)
_cell_angle_alpha                 90
_cell_angle_beta                  115.7150(10)
_cell_angle_gamma                 90
_cell_volume                      1321.41(8)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used      9946
_cell_measurement_theta_min        2.71
_cell_measurement_theta_max       32.58
 
_exptl_crystal_description        'PLATE'
_exptl_crystal_colour             'COLOURLESS'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.349          
_exptl_crystal_F_000              568
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.210
_exptl_crystal_size_mid           0.130
_exptl_crystal_size_min           0.090
_exptl_absorpt_coefficient_mu     0.092
_shelx_estimated_absorpt_T_min    0.981
_shelx_estimated_absorpt_T_max    0.992
_exptl_absorpt_correction_type    'MULTI-SCAN'
_exptl_absorpt_correction_T_min   0.981
_exptl_absorpt_correction_T_max   0.992
_exptl_absorpt_process_details    'SADABS (BRUKER, 2016)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'micro-focus sealed tube'
_diffrn_radiation_monochromator   'multilayer mirrors'
_diffrn_source_type               'Incoatech I\mS HB'
_diffrn_measurement_device        'κ-geometry diffractometer'
_diffrn_measurement_device_type   'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector                  'Photon II CPAD Area Detector'
_diffrn_detector_area_resol_mean  7.39
_diffrn_reflns_number             30220
_diffrn_reflns_av_unetI/netI      0.0156
_diffrn_reflns_av_R_equivalents   0.0232
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          2.713
_diffrn_reflns_theta_max          32.592
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.969
_diffrn_measured_fraction_theta_full  0.938
_diffrn_reflns_Laue_measured_fraction_max    0.969
_diffrn_reflns_Laue_measured_fraction_full   0.938
_diffrn_reflns_point_group_measured_fraction_max   0.969
_diffrn_reflns_point_group_measured_fraction_full  0.938
_reflns_number_total              4653
_reflns_number_gt                 4321
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_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.
;
 
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0539P)²+0.4170P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          4653
_refine_ls_number_parameters      181
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0412
_refine_ls_R_factor_gt            0.0384
_refine_ls_wR_factor_ref          0.1076
_refine_ls_wR_factor_gt           0.1051
_refine_ls_goodness_of_fit_ref    1.063
_refine_ls_restrained_S_all       1.063
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
O1 O 0.76232(5) 0.44462(5) -0.00234(6) 0.01676(12) Uani 1 1 d . . . . .
O2 O 0.71098(5) 0.19466(5) 0.04490(6) 0.01677(12) Uani 1 1 d . . . . .
O3 O 0.21832(6) 0.04745(5) 0.17796(6) 0.01948(13) Uani 1 1 d . . . . .
C1 C 0.67774(6) 0.29954(7) 0.10035(7) 0.01315(13) Uani 1 1 d . . . . .
H1 H 0.7493 0.3190 0.1841 0.016 Uiso 1 1 calc R U . . .
C2 C 0.65266(7) 0.41414(7) 0.01409(7) 0.01522(13) Uani 1 1 d . . . . .
H2A H 0.5821 0.3958 -0.0692 0.018 Uiso 1 1 calc R U . . .
H2B H 0.6286 0.4870 0.0518 0.018 Uiso 1 1 calc R U . . .
C3 C 0.79833(7) 0.33973(7) -0.05563(8) 0.01765(14) Uani 1 1 d . . . . .
H3A H 0.8763 0.3607 -0.0635 0.021 Uiso 1 1 calc R U . . .
H3B H 0.7316 0.3224 -0.1415 0.021 Uiso 1 1 calc R U . . .
C4 C 0.81996(7) 0.22334(7) 0.02577(8) 0.01825(15) Uani 1 1 d . . . . .
H4A H 0.8399 0.1509 -0.0157 0.022 Uiso 1 1 calc R U . . .
H4B H 0.8926 0.2375 0.1087 0.022 Uiso 1 1 calc R U . . .
C5 C 0.56420(7) 0.26521(7) 0.12082(7) 0.01284(12) Uani 1 1 d . . . . .
C6 C 0.49134(7) 0.15920(7) 0.06262(7) 0.01441(13) Uani 1 1 d . . . . .
H6 H 0.5124 0.1087 0.0076 0.017 Uiso 1 1 calc R U . . .
C7 C 0.38842(7) 0.12718(7) 0.08468(7) 0.01414(13) Uani 1 1 d . . . . .
H7 H 0.3403 0.0543 0.0457 0.017 Uiso 1 1 calc R U . . .
C8 C 0.35541(6) 0.20193(6) 0.16411(7) 0.01240(12) Uani 1 1 d . . . . .
C9 C 0.42717(7) 0.30920(7) 0.22043(7) 0.01458(13) Uani 1 1 d . . . . .
H9 H 0.4047 0.3614 0.2733 0.017 Uiso 1 1 calc R U . . .
C10 C 0.53111(7) 0.33989(7) 0.19961(7) 0.01511(13) Uani 1 1 d . . . . .
H10 H 0.5799 0.4122 0.2393 0.018 Uiso 1 1 calc R U . . .
C11 C 0.25005(6) 0.15898(7) 0.19239(7) 0.01332(13) Uani 1 1 d . . . . .
C12 C 0.18471(6) 0.24937(7) 0.24157(7) 0.01291(13) Uani 1 1 d . . . . .
C13 C 0.14206(7) 0.20398(7) 0.32817(7) 0.01460(13) Uani 1 1 d . . . . .
H13 H 0.1572 0.1187 0.3558 0.018 Uiso 1 1 calc R U . . .
C14 C 0.07748(7) 0.28365(8) 0.37374(7) 0.01641(14) Uani 1 1 d . . . . .
H14 H 0.0503 0.2530 0.4339 0.020 Uiso 1 1 calc R U . . .
C15 C 0.05246(7) 0.40778(8) 0.33184(8) 0.01867(15) Uani 1 1 d . . . . .
H15 H 0.0072 0.4616 0.3622 0.022 Uiso 1 1 calc R U . . .
C16 C 0.09408(8) 0.45283(7) 0.24503(9) 0.01984(15) Uani 1 1 d . . . . .
H16 H 0.0767 0.5375 0.2159 0.024 Uiso 1 1 calc R U . . .
C17 C 0.16104(7) 0.37467(7) 0.20055(7) 0.01627(14) Uani 1 1 d . . . . .
H17 H 0.1905 0.4064 0.1425 0.020 Uiso 1 1 calc R U . . .
 
 
_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
O1 C2 1.4268(9) . ?
O1 C3 1.4269(9) . ?
O2 C1 1.4256(9) . ?
O2 C4 1.4318(9) . ?
O3 C11 1.2288(9) . ?
C1 C5 1.5059(10) . ?
C1 C2 1.5244(10) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.5115(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.3945(10) . ?
C5 C6 1.3991(10) . ?
C6 C7 1.3903(9) . ?
C6 H6 0.9500 . ?
C7 C8 1.4002(10) . ?
C7 H7 0.9500 . ?
C8 C9 1.3999(10) . ?
C8 C11 1.4913(9) . ?
C9 C10 1.3903(10) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.4935(10) . ?
C12 C17 1.3980(10) . ?
C12 C13 1.3998(10) . ?
C13 C14 1.3904(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.3897(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.3923(11) . ?
C15 H15 0.9500 . ?
C16 C17 1.3932(10) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
 
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 O1 C3 110.09(6) . . ?
C1 O2 C4 110.50(6) . . ?
O2 C1 C5 108.96(6) . . ?
O2 C1 C2 109.33(6) . . ?
C5 C1 C2 111.58(6) . . ?
O2 C1 H1 109.0 . . ?
C5 C1 H1 109.0 . . ?
C2 C1 H1 109.0 . . ?
O1 C2 C1 110.07(6) . . ?
O1 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
O1 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.2 . . ?
O1 C3 C4 111.08(6) . . ?
O1 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
O1 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
O2 C4 C3 110.78(6) . . ?
O2 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
O2 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
C10 C5 C6 119.23(6) . . ?
C10 C5 C1 119.56(6) . . ?
C6 C5 C1 121.20(6) . . ?
C7 C6 C5 120.51(6) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C8 120.27(7) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C9 C8 C7 119.09(6) . . ?
C9 C8 C11 122.39(6) . . ?
C7 C8 C11 118.38(6) . . ?
C10 C9 C8 120.48(6) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C5 120.41(7) . . ?
C9 C10 H10 119.8 . . ?
C5 C10 H10 119.8 . . ?
O3 C11 C8 119.79(6) . . ?
O3 C11 C12 119.45(6) . . ?
C8 C11 C12 120.73(6) . . ?
C17 C12 C13 119.63(6) . . ?
C17 C12 C11 122.39(6) . . ?
C13 C12 C11 117.94(6) . . ?
C14 C13 C12 120.01(7) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C15 C14 C13 120.44(7) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 119.61(7) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C15 C16 C17 120.50(7) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C16 C17 C12 119.79(7) . . ?
C16 C17 H17 120.1 . . ?
C12 C17 H17 120.1 . . ?
 
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
C4 O2 C1 C5 -179.14(6) . . . . ?
C4 O2 C1 C2 58.68(8) . . . . ?
C3 O1 C2 C1 58.82(8) . . . . ?
O2 C1 C2 O1 -59.89(7) . . . . ?
C5 C1 C2 O1 179.51(6) . . . . ?
C2 O1 C3 C4 -56.89(8) . . . . ?
C1 O2 C4 C3 -57.02(8) . . . . ?
O1 C3 C4 O2 55.83(9) . . . . ?
O2 C1 C5 C10 165.25(6) . . . . ?
C2 C1 C5 C10 -73.94(8) . . . . ?
O2 C1 C5 C6 -14.47(9) . . . . ?
C2 C1 C5 C6 106.34(8) . . . . ?
C10 C5 C6 C7 -1.14(11) . . . . ?
C1 C5 C6 C7 178.57(7) . . . . ?
C5 C6 C7 C8 0.95(11) . . . . ?
C6 C7 C8 C9 0.19(11) . . . . ?
C6 C7 C8 C11 -175.69(6) . . . . ?
C7 C8 C9 C10 -1.13(11) . . . . ?
C11 C8 C9 C10 174.57(7) . . . . ?
C8 C9 C10 C5 0.94(11) . . . . ?
C6 C5 C10 C9 0.20(11) . . . . ?
C1 C5 C10 C9 -179.52(7) . . . . ?
C9 C8 C11 O3 -155.21(7) . . . . ?
C7 C8 C11 O3 20.53(10) . . . . ?
C9 C8 C11 C12 23.09(10) . . . . ?
C7 C8 C11 C12 -161.17(7) . . . . ?
O3 C11 C12 C17 -144.49(8) . . . . ?
C8 C11 C12 C17 37.20(10) . . . . ?
O3 C11 C12 C13 33.01(10) . . . . ?
C8 C11 C12 C13 -145.30(7) . . . . ?
C17 C12 C13 C14 -0.55(11) . . . . ?
C11 C12 C13 C14 -178.12(7) . . . . ?
C12 C13 C14 C15 1.37(11) . . . . ?
C13 C14 C15 C16 -0.93(12) . . . . ?
C14 C15 C16 C17 -0.34(13) . . . . ?
C15 C16 C17 C12 1.16(12) . . . . ?
C13 C12 C17 C16 -0.71(11) . . . . ?
C11 C12 C17 C16 176.75(7) . . . . ?
 
_refine_diff_density_max    0.457
_refine_diff_density_min   -0.187
_refine_diff_density_rms    0.044



