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_7703138
_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           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 100.045(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.0762(6)
_cell_length_b                   16.6019(4)
_cell_length_c                   19.2306(5)
_cell_measurement_reflns_used    9564
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.9030
_cell_measurement_theta_min      3.2670
_cell_volume                     9140.7(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'XL (Sheldrick, 2018)'
_computing_structure_solution    'XS (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -48.00  -22.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9396  -77.0000   30.0000 26

  2 omega   -1.00   43.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9396  -77.0000   30.0000 44

  3 omega   35.00   94.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9396 -178.0000   60.0000 59

  4 omega  -87.00   16.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2521    0.0000  150.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0073604000
_diffrn_orient_matrix_UB_12      -0.0403733000
_diffrn_orient_matrix_UB_13      0.0069509000
_diffrn_orient_matrix_UB_21      0.0080529000
_diffrn_orient_matrix_UB_22      -0.0014459000
_diffrn_orient_matrix_UB_23      -0.0327421000
_diffrn_orient_matrix_UB_31      0.0222379000
_diffrn_orient_matrix_UB_32      0.0138895000
_diffrn_orient_matrix_UB_33      0.0168389000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17792
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.121
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         8057
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0480P)^2^+35.0510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7129
_reflns_number_total             8057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04263f2.cif
_cod_data_source_block           '[CuIIpz(OMe)]6+H2O+12H'
_cod_depositor_comments
'Adding full bibliography for 7703129--7703138.cif.'
_cod_database_code               7703138
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Cu Cl'
_chemical_oxdiff_usercomment     CU6CL6
_reflns_odcompleteness_completeness 99.75
_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. Restrained distances
 Cl3B-C8
 1.75 with sigma of 0.005
 Cl3A-C8
 1.75 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C0AA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C6B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C48A) \\sim Ueq, Uanis(C1AA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C1AA) \\sim Ueq, Uanis(C48A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C28B) = Uanis(C28A)
Uanis(C29B) = Uanis(C33A)
Uanis(C32A) = Uanis(C30B)
Uanis(C31A) = Uanis(C31B)
Uanis(C30A) = Uanis(C32B)
Uanis(C29A) = Uanis(C33B)
Uanis(C22A) = Uanis(C22B)
Uanis(C23A) = Uanis(C23B)
Uanis(C24A) = Uanis(C24B)
Uanis(C25B) = Uanis(C25A)
Uanis(C26B) = Uanis(C26A)
Uanis(C27B) = Uanis(C27A)
Uanis(C1AA) = Uanis(C48A)
Uanis(C0AA) = Uanis(C46A)
Uanis(C6A) = Uanis(C6B)
Uanis(Cl3B) = Uanis(Cl3A)
Uanis(Cl1B) = Uanis(Cl1A)
Uanis(C4A) = Uanis(C4B)
Uanis(C5B) = Uanis(C5A)
4. Others
 Sof(Cl3B)=1-FVAR(1)
 Sof(Cl3A)=FVAR(1)
 Sof(Cl1B)=1-FVAR(2)
 Sof(Cl1A)=FVAR(2)
 Fixed Sof: Cl2B(0.5) C5B(0.5) C6B(0.5) C22A(0.5) C23A(0.5) H23A(0.5)
 C24A(0.5) H24A(0.5) C25A(0.5) H25A(0.5) C26A(0.5) H26A(0.5) C27A(0.5)
 H27A(0.5) C4B(0.5) C32B(0.5) H32B(0.5) C33B(0.5) H33B(0.5) C28B(0.5) C29B(0.5)
 H29B(0.5) C30B(0.5) H30B(0.5) C31B(0.5) H31B(0.5) C28A(0.5) C33A(0.5)
 H33A(0.5) C32A(0.5) H32A(0.5) C31A(0.5) H31A(0.5) C30A(0.5) H30A(0.5)
 C29A(0.5) H29A(0.5) C22B(0.5) C23B(0.5) H23B(0.5) C24B(0.5) H24B(0.5)
 C25B(0.5) H25B(0.5) C26B(0.5) H26B(0.5) C27B(0.5) H27B(0.5) C6A(0.5) C5A(0.5)
 C4A(0.5) Cl2A(0.5) C1AA(0.25) H1AA(0.25) H1AB(0.25) H1AC(0.25) C48A(0.75)
 H48A(0.75) H48B(0.75) H48C(0.75) C46A(0.75) H46A(0.75) H46B(0.75) H46C(0.75)
 C0AA(0.25) H0AA(0.25) H0AB(0.25) H0AC(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C18(H18), C17(H17), C11(H11), C39(H39), C12(H12), C35(H35),
 C21(H21), C20(H20), C15(H15), C14(H14), C13(H13), C23A(H23A), C24A(H24A),
 C25A(H25A), C26A(H26A), C27A(H27A), C43(H43), C42(H42), C36(H36), C45(H45),
 C44(H44), C41(H41), C37(H37), C38(H38), C32B(H32B), C33B(H33B), C29B(H29B),
 C30B(H30B), C31B(H31B), C33A(H33A), C32A(H32A), C31A(H31A), C30A(H30A),
 C29A(H29A), C23B(H23B), C24B(H24B), C25B(H25B), C26B(H26B), C27B(H27B)
5.b Fitted hexagon refined as free rotating group:
 C22A(C23A,C24A,C25A,C26A,C27A), C32B(C33B,C28B,C29B,C30B,C31B), C28A(C33A,
 C32A,C31A,C30A,C29A), C22B(C23B,C24B,C25B,C26B,C27B)
5.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C1AA(H1AA,H1AB,H1AC), C48A(H48A,H48B,H48C), C46A(H46A,
 H46B,H46C), C0AA(H0AA,H0AB,H0AC)
;
_olex2_submission_special_instructions 'No special instructions were received'