Coordination-induced conformation diversity for pharmaceutical polymorph control
Kang, Juan; Wang, Yongli; Chen, Yifu; Huang, Xin; Yin, Qiuxiang; Wang, Na; Hao, Hongxun; CrystEngComm 21 (2019) 6585–; doi:10.1039/C9CE01310E

data_7234204
_publ_section_title
;
 Coordination-induced conformation diversity for pharmaceutical polymorph
 control
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6585
_journal_paper_doi               10.1039/C9CE01310E
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C36 H48 Co N12 Na2 O16 S8, 2(H2 O)'
_chemical_formula_sum            'C36 H52 Co N12 Na2 O18 S8'
_chemical_formula_weight         1302.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-29 deposited with the CCDC.    2019-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.800(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4803(5)
_cell_length_b                   7.7683(4)
_cell_length_c                   27.2802(15)
_cell_measurement_reflns_used    5179
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.6530
_cell_measurement_theta_min      1.8450
_cell_volume                     2644.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.805
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -97.00  32.00   0.50    2.00    --  -13.65 -25.00 -31.00  258
  2  \w    -89.00   6.00   0.50    2.00    --  -13.65 -57.00-120.00  190
  3  \w     39.00  67.00   0.50    2.00    --   12.17 178.00-120.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0237480000
_diffrn_orient_matrix_UB_12      -0.0184928000
_diffrn_orient_matrix_UB_13      0.0231059000
_diffrn_orient_matrix_UB_21      0.0482823000
_diffrn_orient_matrix_UB_22      -0.0231039000
_diffrn_orient_matrix_UB_23      -0.0116770000
_diffrn_orient_matrix_UB_31      0.0180229000
_diffrn_orient_matrix_UB_32      0.0862173000
_diffrn_orient_matrix_UB_33      0.0018311000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.805
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            9243
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.080
_diffrn_reflns_theta_min         2.726
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43d (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       block
_exptl_crystal_F_000             1346
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.169
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         9243
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0535
_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/[\s^2^(Fo^2^)+(0.0716P)^2^+1.6206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7191
_reflns_number_total             9243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01310e2.cif
_cod_data_source_block           kj-15-2_twin1_hklf5_sq
_cod_depositor_comments
'Adding full bibliography for 7234202--7234204.cif.'
_cod_database_code               7234204
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 98.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6115
 0.3885
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O4-H4A
 0.9 with sigma of 0.02
 O4-H4B
 0.9 with sigma of 0.02
 O4_$1-H4B_$1
 0.9 with sigma of 0.02
 O4_$1-H4A_$1
 0.9 with sigma of 0.02
 H6A-N6
 0.92 with sigma of 0.02
 H6B-N6
 0.92 with sigma of 0.02
 H2A-O2
 0.9 with sigma of 0.01
 H2B-O2
 0.9 with sigma of 0.01
 H4A-H4B
 1.6 with sigma of 0.04
 H2B-H2A
 1.5 with sigma of 0.01
 Na1-O3A \\sim Na1-O3
 with sigma of 0.01
4. Others
 Sof(O3)=Sof(H3A)=Sof(H3B)=1-FVAR(1)
 Sof(O3A)=Sof(H3AA)=Sof(H3AB)=FVAR(1)
5.a Free rotating group:
 O1(H1A,H1B), O3A(H3AA,H3AB), O3(H3A,H3B)
5.b Rotating group:
 N1(H1C,H1D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18)
;
_shelx_res_checksum              45734
_platon_squeeze_void_probe_radius 1.20
_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 1.143
_oxdiff_exptl_absorpt_empirical_full_min 0.919