A systematic investigation of structural transformation in a copper pyrazolato system: a case study.
Chen, Jing-Huo; Wei, Donghui; Yang, Guang; Ma, Jian-Gong; Cheng, Peng; Dalton transactions (Cambridge, England : 2003) 49 (2020) 1116–1123; doi:10.1039/c9dt04263f

data_7703135
_publ_section_title
;
 A systematic investigation of structural transformation in a copper
 pyrazolato system: a case study.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1116
_journal_page_last               1123
_journal_paper_doi               10.1039/c9dt04263f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C96 H78 Cl6 Cu6 N12 O6'
_chemical_formula_sum            'C96 H78 Cl6 Cu6 N12 O6'
_chemical_formula_weight         2089.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-10-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-11-04 deposited with the CCDC.	2019-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.1273(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.1746(6)
_cell_length_b                   16.6071(4)
_cell_length_c                   19.2602(4)
_cell_measurement_reflns_used    10675
_cell_measurement_temperature    120(10)
_cell_measurement_theta_max      28.9210
_cell_measurement_theta_min      3.4240
_cell_volume                     9186.3(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'XL (Sheldrick, 2018)'
_computing_structure_solution    'XS (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(10)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega   48.00   82.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  178.0000 -120.0000 34

  2 omega   60.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  178.0000 -180.0000 26

  3 omega  -59.00   -1.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185  -19.0000 -120.0000 58

  4 omega  -58.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185   19.0000  -60.0000 101
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0194145000
_diffrn_orient_matrix_UB_12      0.0187215000
_diffrn_orient_matrix_UB_13      -0.0211644000
_diffrn_orient_matrix_UB_21      -0.0151631000
_diffrn_orient_matrix_UB_22      -0.0272116000
_diffrn_orient_matrix_UB_23      0.0132203000
_diffrn_orient_matrix_UB_31      -0.0017590000
_diffrn_orient_matrix_UB_32      0.0270909000
_diffrn_orient_matrix_UB_33      0.0278533000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33733
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         3.104
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.599
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       block
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.401
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1141
_refine_ls_number_reflns         16027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+0.1396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12685
_reflns_number_total             16027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04263f2.cif
_cod_data_source_block           '[CuIIpz(OMe)]6'
_cod_depositor_comments
'Adding full bibliography for 7703129--7703138.cif.'
_cod_original_cell_volume        9186.3(3)
_cod_database_code               7703135
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C1H1O1N1Cl1Cu1
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C86(H86), C38(H38), C36(H36), C22(H22), C26(H26), C32(H32), C39(H39),
 C42(H42), C41(H41), C30(H30), C20(H20), C50(H50), C64(H64), C23(H23), C74(H74),
  C75(H75), C35(H35), C24(H24), C21(H21), C33(H33), C40(H40), C58(H58),
 C87(H87), C68(H68), C88(H88), C80(H80), C29(H29), C62(H62), C56(H56), C72(H72),
  C51(H51), C27(H27), C81(H81), C84(H84), C83(H83), C65(H65), C66(H66),
 C54(H54), C45(H45), C28(H28), C70(H70), C57(H57), C44(H44), C48(H48), C63(H63),
  C76(H76), C59(H59), C53(H53), C78(H78), C89(H89), C34(H34), C60(H60),
 C82(H82), C69(H69), C71(H71), C77(H77), C52(H52), C47(H47), C46(H46), C90(H90)
2.b Idealised Me refined as rotating group:
 C95(H95A,H95B,H95C), C94(H94A,H94B,H94C), C93(H93A,H93B,H93C), C96(H96A,H96B,
 H96C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C)
;
_olex2_submission_special_instructions 'No special instructions were received'