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_7703133
_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         '2(C93.5 H73 Cl6 Cu6 N12 O6)'
_chemical_formula_sum            'C187 H146 Cl12 Cu12 N24 O12'
_chemical_formula_weight         4109.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-10-29
_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                 100.186(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   29.0473(9)
_cell_length_b                   16.4211(7)
_cell_length_c                   19.2985(7)
_cell_measurement_reflns_used    7387
_cell_measurement_temperature    120(10)
_cell_measurement_theta_max      28.6940
_cell_measurement_theta_min      3.7140
_cell_volume                     9060.1(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'XL (Sheldrick, 2018)'
_computing_structure_solution    'XS (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -43.00  30.00   1.00   75.00    --  -19.25  37.00  90.00   73
  2  \w    -43.00  21.00   1.00   75.00    --  -19.25  19.00  30.00   64
  3  \w     37.00  70.00   1.00   75.00    --   18.94 178.00-150.00   33
  4  \w     36.00  94.00   1.00   75.00    --   18.94 178.00 -60.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0166769000
_diffrn_orient_matrix_UB_12      -0.0199237000
_diffrn_orient_matrix_UB_13      0.0257709000
_diffrn_orient_matrix_UB_21      0.0039962000
_diffrn_orient_matrix_UB_22      -0.0290722000
_diffrn_orient_matrix_UB_23      -0.0254627000
_diffrn_orient_matrix_UB_31      0.0179202000
_diffrn_orient_matrix_UB_32      0.0249697000
_diffrn_orient_matrix_UB_33      -0.0091090000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17004
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         3.143
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.620
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.506
_exptl_crystal_description       block
_exptl_crystal_F_000             4168
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         7954
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      2.567
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0444P)^2^+73.8793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6326
_reflns_number_total             7954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04263f2.cif
_cod_data_source_block           '[CuIIpz(OMe)]6+H2O+72H'
_cod_depositor_comments
'Adding full bibliography for 7703129--7703138.cif.'
_cod_database_code               7703133
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Cu Cl'
_chemical_oxdiff_usercomment     CU6CL6+H20
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3A-H3A
 0.84 with sigma of 0.005
 O1B-H1B
 1.84 with sigma of 0.005
 C4-C22A \\sim C4-C22B
 with sigma of 0.02
 C6-C28A \\sim C6-C28B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C48B) \\sim Ueq, Uanis(O3B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O1A) \\sim Ueq, Uanis(C46A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C48B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C32A) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C30A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C28A) = Uanis(C28B)
Uanis(C33B) = Uanis(C33A)
Uanis(C32B) = Uanis(C32A)
Uanis(C31A) = Uanis(C31B)
Uanis(C30A) = Uanis(C30B)
Uanis(C29A) = Uanis(C29B)
Uanis(C22A) = Uanis(C22B)
Uanis(C27A) = Uanis(C27B)
Uanis(C26A) = Uanis(C26B)
Uanis(C25A) = Uanis(C25B)
Uanis(C24B) = Uanis(C24A)
Uanis(C23A) = Uanis(C23B)
Uanis(O3B) = Uanis(O3A)
Uanis(O1A) = Uanis(O1B)
4. Others
 Fixed Sof: Cl2A(0.75) O1B(0.5) H1B(0.5) O3B(0.25) C22A(0.75) C27A(0.75)
 H27A(0.75) C26A(0.75) H26A(0.75) C23A(0.75) H23A(0.75) C25A(0.75) H25A(0.75)
 C24A(0.75) H24A(0.75) C48B(0.25) H48A(0.25) H48B(0.25) H48C(0.25) O3A(0.75)
 H3A(0.75) C46A(0.5) H46A(0.5) H46B(0.5) H46C(0.5) O1A(0.5) C28A(0.75)
 C33A(0.75) H33A(0.75) C29A(0.75) H29A(0.75) C30A(0.75) H30A(0.75) C32A(0.75)
 H32A(0.75) C31A(0.75) H31A(0.75) C28B(0.25) C33B(0.25) H33B(0.25) C32B(0.25)
 H32B(0.25) C31B(0.25) H31B(0.25) C30B(0.25) H30B(0.25) C29B(0.25) H29B(0.25)
 C22B(0.25) C27B(0.25) H27B(0.25) C26B(0.25) H26B(0.25) C25B(0.25) H25B(0.25)
 C24B(0.25) H24B(0.25) C23B(0.25) H23B(0.25) Cl2B(0.25)
5.a Riding coordinates:
 O1B(H1B), O3A(H3A)
5.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C17(H17), C11(H11), C12(H12), C39(H39), C21(H21),
 C37(H37), C14(H14), C13(H13), C35(H35), C43(H43), C36(H36), C15(H15), C38(H38),
  C20(H20), C44(H44), C27A(H27A), C26A(H26A), C41(H41), C23A(H23A), C25A(H25A),
 C42(H42), C45(H45), C24A(H24A), C33A(H33A), C29A(H29A), C30A(H30A), C32A(H32A),
  C31A(H31A), C33B(H33B), C32B(H32B), C31B(H31B), C30B(H30B), C29B(H29B),
 C27B(H27B), C26B(H26B), C25B(H25B), C24B(H24B), C23B(H23B)
5.c Fitted hexagon refined as free rotating group:
 C28B(C33B,C32B,C31B,C30B,C29B), C22B(C27B,C26B,C25B,C24B,C23B)
5.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C48B(H48A,H48B,H48C), C46A(H46A,H46B,H46C)
;
_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 1.410
_oxdiff_exptl_absorpt_empirical_full_min 0.730