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_7703131
_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         'C60 H40 Cl4 Cu4 N8, 3.75(C H2 Cl2)'
_chemical_formula_sum            'C63.75 H47.5 Cl11.5 Cu4 N8'
_chemical_formula_weight         1587.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_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                77.698(3)
_cell_angle_beta                 83.790(2)
_cell_angle_gamma                80.707(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0449(2)
_cell_length_b                   15.1382(5)
_cell_length_c                   23.2997(8)
_cell_measurement_reflns_used    10273
_cell_measurement_temperature    120(10)
_cell_measurement_theta_max      28.8230
_cell_measurement_theta_min      3.4700
_cell_volume                     3406.19(18)
_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(10)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -54.00   45.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9396  -37.0000   90.0000 99

  2 omega  -17.00   60.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9396  -99.0000    0.0000 77

  3 omega  -54.00   33.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9396  -37.0000    0.0000 87

  4 omega   -7.00   89.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9396   77.0000 -120.0000 96

  5 omega   -6.00   33.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9396   77.0000  120.0000 39
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0683242000
_diffrn_orient_matrix_UB_12      0.0080331000
_diffrn_orient_matrix_UB_13      -0.0051257000
_diffrn_orient_matrix_UB_21      0.0142070000
_diffrn_orient_matrix_UB_22      -0.0340555000
_diffrn_orient_matrix_UB_23      -0.0173919000
_diffrn_orient_matrix_UB_31      -0.0167264000
_diffrn_orient_matrix_UB_32      0.0335134000
_diffrn_orient_matrix_UB_33      -0.0254515000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22985
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.129
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.728
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86227
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       block
_exptl_crystal_F_000             1595
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.650
_refine_diff_density_min         -1.869
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         11906
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0701
_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^)+(0.0713P)^2^+23.3705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.1801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10208
_reflns_number_total             11906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04263f2.cif
_cod_data_source_block           (CuIpz)4
_cod_depositor_comments
'Adding full bibliography for 7703129--7703138.cif.'
_cod_original_cell_volume        3406.22(19)
_cod_original_formula_sum        'C63.75 H47.50 Cl11.50 Cu4 N8'
_cod_database_code               7703131
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Cu Cl'
_reflns_odcompleteness_completeness 99.81
_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 C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Cl6B-C61
 1.75 with sigma of 0.005
 Cl6A-C61
 1.75 with sigma of 0.005
 Cl8B-C62
 1.75 with sigma of 0.005
 Cl8A-C62
 1.75 with sigma of 0.005
 Cl12-C65 = Cl6-C65
 1.72 with sigma of 0.01
 Cl8B-C62 \\sim Cl8A-C62
 with sigma of 0.02
 Cl6B-C61 \\sim Cl6A-C61
 with sigma of 0.02
3. Rigid bond restraints
 C64, Cl11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl11 \\sim C64: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C60) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C35) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C52)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C64) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cl6A) \\sim Ueq, Uanis(Cl6B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl6B) \\sim Ueq, Uanis(Cl6A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(Cl8B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl12) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cl8B) = Uanis(Cl8A)
Uanis(Cl6A) = Uanis(Cl6B)
Uanis(Cl12) = Uanis(Cl6)
Uanis(Cl12) = Uanis(C65)
5. Others
 Fixed Sof: Cl6B(0.75) H61C(0.75) H61D(0.75) H61A(0.25) H61B(0.25) H62C(0.75)
 H62D(0.75) H62A(0.25) H62B(0.25) Cl8B(0.75) Cl8A(0.25) Cl11(0.5) C64(0.25)
 H64A(0.25) H64B(0.25) Cl6A(0.25) Cl12(0.5) C65(0.5) H65C(0.25) H65D(0.25)
 H65A(0.25) H65B(0.25) Cl6(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C61(H61C,H61D), C61(H61A,H61B), C63(H63A,H63B), C62(H62C,H62D), C62(H62A,
 H62B), C64(H64A,H64B), C65(H65C,H65D), C65(H65A,H65B)
6.b Aromatic/amide H refined with riding coordinates:
 C40(H40), C38(H38), C46(H46), C30(H30), C44(H44), C24(H24), C22(H22),
 C21(H21), C16(H16), C14(H14), C26(H26), C36(H36), C48(H48), C57(H57), C39(H39),
  C15(H15), C47(H47), C45(H45), C18(H18), C50(H50), C42(H42), C41(H41),
 C54(H54), C20(H20), C56(H56), C35(H35), C23(H23), C28(H28), C32(H32), C60(H60),
  C33(H33), C51(H51), C29(H29), C17(H17), C59(H59), C27(H27), C34(H34),
 C58(H58), C52(H52), C53(H53)
;
_olex2_submission_special_instructions 'No special instructions were received'