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_7703137
_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         'C92 H70 Cl6 Cu6 N12 O6'
_chemical_formula_sum            'C92 H70 Cl6 Cu6 N12 O6'
_chemical_formula_weight         2033.54
_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                 100.387(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.0392(8)
_cell_length_b                   16.3390(8)
_cell_length_c                   19.2980(6)
_cell_measurement_reflns_used    7213
_cell_measurement_temperature    120(4)
_cell_measurement_theta_max      28.4460
_cell_measurement_theta_min      3.3380
_cell_volume                     9006.3(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(4)
_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      8.00  75.00   1.00   87.50    --   18.94  57.00 -90.00   67
  2  \w     -2.00  81.00   1.00   87.50    --   18.94  19.00-120.00   83
  3  \w     -8.00  32.00   1.00   87.50    --   18.94 -99.00  60.00   40
  4  \w    -90.00 -53.00   1.00   87.50    --  -19.25-178.00-150.00   37
;
_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      -0.0064678000
_diffrn_orient_matrix_UB_12      0.0299296000
_diffrn_orient_matrix_UB_13      0.0231017000
_diffrn_orient_matrix_UB_21      -0.0239514000
_diffrn_orient_matrix_UB_22      -0.0095014000
_diffrn_orient_matrix_UB_23      -0.0119458000
_diffrn_orient_matrix_UB_31      0.0011443000
_diffrn_orient_matrix_UB_32      -0.0299441000
_diffrn_orient_matrix_UB_33      0.0268513000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16616
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.155
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.629
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87469
_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    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             4120
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.646
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         7907
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0763
_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^)+(0.0334P)^2^+179.1290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6539
_reflns_number_total             7907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04263f2.cif
_cod_data_source_block           '[CuIIpz(OMe)]6+H2O+96H'
_cod_depositor_comments
'Adding full bibliography for 7703129--7703138.cif.'
_cod_database_code               7703137
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Cu Cl'
_chemical_oxdiff_usercomment     cu6cl6+h2o+96H
_reflns_odcompleteness_completeness 99.67
_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, All O(H) groups
2. Restrained distances
 H46C_$1-H31
 2 with sigma of 0.02
 H31-H46B_$1
 2.1 with sigma of 0.02
 H46B_$1-H31
 2.1 with sigma of 0.005
 O1-C46A
 1.42 with sigma of 0.01
 C46A-Cu1 \\sim C46A-Cu2
 with sigma of 0.02
3. Rigid bond restraints
 C30, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C32, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C29, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C28, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C29, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu3, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C31 \\sim C30: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C31 \\sim C32: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C28 \\sim C33: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C28 \\sim C29: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C29 \\sim C30: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Cu3 \\sim O3: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C46A) \\sim Ueq, Uanis(C47A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C46A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: H1(0.75) C46A(0.25) H46A(0.25) H46B(0.25) H46C(0.25) H2(0.25)
 C47A(0.75) H47A(0.75) H47B(0.75) H47C(0.75)
6.a Riding coordinates:
 O3(H3), O1(H1), O2(H2)
6.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C17(H17), C11(H11), C19(H19), C24(H24), C37(H37), C12(H12),
 C21(H21), C13(H13), C36(H36), C35(H35), C23(H23), C20(H20), C39(H39), C15(H15),
  C44(H44), C14(H14), C41(H41), C27(H27), C43(H43), C38(H38), C42(H42),
 C45(H45), C25(H25), C26(H26), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
6.c Fitted hexagon refined as free rotating group:
 C28(C29,C30,C31,C32,C33)
6.d Idealised Me refined as rotating group:
 C46A(H46A,H46B,H46C), C47A(H47A,H47B,H47C)
;
_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 1.162
_oxdiff_exptl_absorpt_empirical_full_min 0.783