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_7703129
_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         'C45 H30 Cl3 Cu3 N6'
_chemical_formula_sum            'C45 H30 Cl3 Cu3 N6'
_chemical_formula_weight         951.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/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                 98.2710(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1550(2)
_cell_length_b                   21.1155(3)
_cell_length_c                   14.4734(3)
_cell_measurement_reflns_used    7148
_cell_measurement_temperature    120(10)
_cell_measurement_theta_max      28.4870
_cell_measurement_theta_min      3.1790
_cell_volume                     3978.52(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -47.00  -7.00   1.00   20.00    --   18.94 -57.00  30.00   40
  2  \w    -19.00  56.00   1.00   20.00    --   18.94 -99.00   0.00   75
  3  \w    -77.00   2.00   1.00   20.00    --  -19.25 -37.00  90.00   79
  4  \w      1.00  46.00   1.00   20.00    --   18.94  77.00  60.00   45
;
_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      -0.0205249000
_diffrn_orient_matrix_UB_12      -0.0300064000
_diffrn_orient_matrix_UB_13      -0.0147244000
_diffrn_orient_matrix_UB_21      0.0303284000
_diffrn_orient_matrix_UB_22      -0.0144652000
_diffrn_orient_matrix_UB_23      0.0388039000
_diffrn_orient_matrix_UB_31      -0.0403037000
_diffrn_orient_matrix_UB_32      0.0044473000
_diffrn_orient_matrix_UB_33      0.0270319000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16007
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         3.004
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86506
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         7002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0218P)^2^+1.3986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5945
_reflns_number_total             7002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04263f2.cif
_cod_data_source_block           (CuIpz)3
_cod_depositor_comments
'Adding full bibliography for 7703129--7703138.cif.'
_cod_original_cell_volume        3978.53(12)
_cod_database_code               7703129
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Cu Cl'
_chemical_oxdiff_usercomment     4-Cl-CU
_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
2.a Aromatic/amide H refined with riding coordinates:
 C45(H45), C32(H32), C11(H11), C37(H37), C41(H41), C39(H39), C12(H12),
 C35(H35), C20(H20), C15(H15), C13(H13), C24(H24), C29(H29), C33(H33), C42(H42),
  C44(H44), C14(H14), C26(H26), C27(H27), C21(H21), C23(H23), C36(H36),
 C31(H31), C38(H38), C25(H25), C17(H17), C18(H18), C43(H43), C30(H30), C19(H19)
;
_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 1.250
_oxdiff_exptl_absorpt_empirical_full_min 0.775