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_7234203
_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 H38 N12 Ni2 O11 S8'
_chemical_formula_sum            'C36 H38 N12 Ni2 O11 S8'
_chemical_formula_weight         1188.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-05 deposited with the CCDC.    2019-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.444(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0094(4)
_cell_length_b                   12.8836(6)
_cell_length_c                   17.3263(7)
_cell_measurement_reflns_used    5375
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      76.2030
_cell_measurement_theta_min      3.4550
_cell_volume                     2678.36(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (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      159.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.942
_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     19.00 118.00   0.50    0.66    --   46.12  84.00 -73.00  198
  2  \w     73.00 118.00   0.50    0.66    --   46.12 125.00-150.00   90
  3  \w     73.00 118.00   0.50    0.66    --   46.12 125.00-120.00   90
  4  \w     81.00 178.00   0.50    2.64    --  107.31  84.00 -73.00  194
  5  \w     93.00 155.00   0.50    2.64    --  107.31  45.00 -60.00  124
  6  \w     73.00  98.00   0.50    0.66    --   46.12 125.00 120.00   50
  7  \w    -26.00  73.00   0.50    0.66    --   46.12 -84.00 166.00  198
  8  \w     35.00 134.00   0.50    2.64    --  107.31 -84.00 166.00  198
  9  \w     38.00  89.00   0.50    2.64    --  107.31-125.00 150.00  102
 10  \w     36.00 107.00   0.50    2.64    --  107.31 -94.00   0.00  142
 11  \w    -73.00  27.00   0.50    0.66    --  -46.12  84.00 -73.00  200
 12  \w   -118.00 -19.00   0.50    0.66    --  -46.12 -84.00 166.00  198
 13  \w   -118.00 -24.00   0.50    2.64    -- -100.00  15.00-150.00  188
 14  \w   -114.00 -25.00   0.50    2.64    -- -100.00  30.00 -60.00  178
 15  \w   -117.00 -83.00   0.50    2.64    -- -100.00 -15.00   0.00   68
 16  \w   -127.00 -27.00   0.50    2.64    -- -100.00  84.00 -73.00  200
 17  \w   -173.00 -73.00   0.50    2.64    -- -100.00 -84.00 166.00  200
 18  \w   -173.00-144.00   0.50    2.64    -- -100.00 -15.00   0.00   58
 19  \w   -164.00 -87.00   0.50    2.64    -- -100.00 -94.00-120.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0871412000
_diffrn_orient_matrix_UB_12      -0.0730117000
_diffrn_orient_matrix_UB_13      -0.0389102000
_diffrn_orient_matrix_UB_21      0.0934867000
_diffrn_orient_matrix_UB_22      -0.0757802000
_diffrn_orient_matrix_UB_23      -0.0205774000
_diffrn_orient_matrix_UB_31      -0.0126976000
_diffrn_orient_matrix_UB_32      -0.0567623000
_diffrn_orient_matrix_UB_33      0.0773309000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1412
_diffrn_reflns_av_unetI/netI     0.0954
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25790
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.175
_diffrn_reflns_theta_min         3.430
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.328
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0799
_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^)+(0.1453P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1988
_refine_ls_wR_factor_ref         0.2335
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3275
_reflns_number_total             5352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01310e2.cif
_cod_data_source_block           kj-40-1
_cod_depositor_comments
'Adding full bibliography for 7234202--7234204.cif.'
_cod_database_code               7234203
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.918
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. 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
2. Others
 Fixed Sof: H5A(0.5) H5B(0.5)
 Fixed X: H5A(0.7876) H5B(0.68944)
 Fixed Y: H5A(0.296529) H5B(0.2958)
 Fixed Z: H5A(0.22561) H5B(0.26008)
3.a Rotating group:
 O6(H6A,H6B), N1(H1A,H1B), N5(H5C,H5D)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C17(H17), C18(H18)
;
_shelx_res_checksum              78550
_shelx_fab_checksum              88042
_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 3.770
_oxdiff_exptl_absorpt_empirical_full_min 0.352