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_7703136
_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         'C94 H74 Cl6 Cu6 N12 O6'
_chemical_formula_sum            'C94 H74 Cl6 Cu6 N12 O6'
_chemical_formula_weight         2061.59
_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                 100.272(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.0564(7)
_cell_length_b                   16.4701(4)
_cell_length_c                   19.3195(4)
_cell_measurement_reflns_used    8609
_cell_measurement_temperature    120(3)
_cell_measurement_theta_max      29.0190
_cell_measurement_theta_min      3.4090
_cell_volume                     9097.4(4)
_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(3)
_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     -3.00  43.00   1.00   75.00    --  -19.25  37.00 120.00   46
  2  \w    -88.00   9.00   1.00   75.00    --  -19.25 -77.00 -30.00   97
  3  \w    -20.00  13.00   1.00   75.00    --   18.94 -99.00-150.00   33
  4  \w    -19.00   7.00   1.00   75.00    --   18.94 -99.00-180.00   26
  5  \w     10.00  60.00   1.00   75.00    --   18.94 -99.00-180.00   50
;
_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      0.0060577000
_diffrn_orient_matrix_UB_12      -0.0408297000
_diffrn_orient_matrix_UB_13      0.0091023000
_diffrn_orient_matrix_UB_21      -0.0162245000
_diffrn_orient_matrix_UB_22      -0.0136311000
_diffrn_orient_matrix_UB_23      -0.0295724000
_diffrn_orient_matrix_UB_31      0.0177636000
_diffrn_orient_matrix_UB_32      0.0014802000
_diffrn_orient_matrix_UB_33      -0.0208408000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18958
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         3.137
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.614
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85232
_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    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             4184
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         7987
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0350P)^2^+56.9700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6734
_reflns_number_total             7987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04263f2.cif
_cod_data_source_block           '[CuIIpz(OMe)]6+H2O+48H'
_cod_depositor_comments
'Adding full bibliography for 7703129--7703138.cif.'
_cod_database_code               7703136
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Cu Cl'
_chemical_oxdiff_usercomment     CU6CL6+H20+48H
_reflns_odcompleteness_completeness 99.72
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2A-C5 = Cl2B-C5
 1.75 with sigma of 0.01
 H3A-O3A
 0.84 with sigma of 0.001
 O1B-H1B
 0.84 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C31B) \\sim Ueq, Uanis(C30B) \\sim Ueq, Uanis(C32B) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C46A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O3B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.001
Uanis(C48B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O1A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.001
Uanis(C22A) = Uanis(C22B)
Uanis(C27A) = Uanis(C27B)
Uanis(C26B) = Uanis(C26A)
Uanis(C25B) = Uanis(C25A)
Uanis(C24A) = Uanis(C24B)
Uanis(C23A) = Uanis(C23B)
Uanis(C32A) = Uanis(C32B)
Uanis(C31B) = Uanis(C31A)
Uanis(C30B) = Uanis(C30A)
Uanis(O3A) = Uanis(O3B)
Uanis(O1A) = Uanis(O1B)
4. Others
 Fixed Sof: O1B(0.35) O3B(0.35) C46A(0.65) H46A(0.65) H46B(0.65) H46C(0.65)
 C48B(0.35) H48A(0.35) H48B(0.35) H48C(0.35) C22A(0.75) C27A(0.75) H27A(0.75)
 C26A(0.75) H26A(0.75) C25A(0.75) H25A(0.75) C24A(0.75) H24A(0.75) C23A(0.75)
 H23A(0.75) C28B(0.65) C29B(0.65) H29B(0.65) C30B(0.65) H30B(0.65) C31B(0.65)
 H31B(0.65) C32B(0.65) H32B(0.65) C33B(0.65) H33B(0.65) C28A(0.35) C29A(0.35)
 H29A(0.35) C30A(0.35) H30A(0.35) C31A(0.35) H31A(0.35) C32A(0.35) H32A(0.35)
 C33A(0.35) H33A(0.35) 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) Cl2A(0.25)
 Cl2B(0.75) O3A(0.65) O1A(0.65) H1B(0.35) H3A(0.65)
5.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C44(H44), C20(H20), C14(H14), C12(H12), C13(H13), C19(H19),
 C11(H11), C35(H35), C17(H17), C36(H36), C39(H39), C15(H15), C18(H18), C42(H42),
  C38(H38), C45(H45), C37(H37), C43(H43), C41(H41), C27A(H27A), C26A(H26A),
 C25A(H25A), C24A(H24A), C23A(H23A), C29B(H29B), C30B(H30B), C31B(H31B),
 C32B(H32B), C33B(H33B), C29A(H29A), C30A(H30A), C31A(H31A), C32A(H32A),
 C33A(H33A), C27B(H27B), C26B(H26B), C25B(H25B), C24B(H24B), C23B(H23B)
5.b Fitted hexagon refined as free rotating group:
 C22A(C27A,C26A,C25A,C24A,C23A), C28B(C29B,C30B,C31B,C32B,C33B), C28A(C29A,
 C30A,C31A,C32A,C33A), C22B(C27B,C26B,C25B,C24B,C23B)
5.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C46A(H46A,H46B,H46C), C48B(H48A,H48B,H48C)
;
_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 1.142
_oxdiff_exptl_absorpt_empirical_full_min 0.863