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_7703134
_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         'C77 H56 Cl5 Cu5 N10 O2'
_chemical_formula_sum            'C77 H56 Cl5 Cu5 N10 O2'
_chemical_formula_weight         1648.26
_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
_audit_creation_date             2019-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-04 deposited with the CCDC.	2019-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                72.065(6)
_cell_angle_beta                 68.528(6)
_cell_angle_gamma                86.629(6)
_cell_formula_units_Z            2
_cell_length_a                   16.2557(11)
_cell_length_b                   17.0114(12)
_cell_length_c                   17.9429(11)
_cell_measurement_reflns_used    4535
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      26.0310
_cell_measurement_theta_min      3.4550
_cell_volume                     4384.9(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'XL (Sheldrick, 2018)'
_computing_structure_solution    'XS (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(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    -54.00  43.00   1.00   40.00    --   18.55   0.00-180.00   97
  2  \w    -11.00  89.00   1.00   40.00    --   18.55  77.00 -60.00  100
  3  \w      6.00  60.00   1.00   40.00    --   18.55 -99.00  60.00   54
  4  \w     -8.00  20.00   1.00   40.00    --   18.55  19.00  30.00   28
  5  \w     36.00  89.00   1.00   40.00    --   18.55  19.00  30.00   53
  6  \w    -41.00   8.00   1.00   40.00    --  -19.56  57.00-120.00   49
  7  \w    -71.00  10.00   1.00   40.00    --  -19.56 -77.00 120.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0086514000
_diffrn_orient_matrix_UB_12      -0.0294698000
_diffrn_orient_matrix_UB_13      -0.0172761000
_diffrn_orient_matrix_UB_21      -0.0458165000
_diffrn_orient_matrix_UB_22      0.0067951000
_diffrn_orient_matrix_UB_23      0.0152629000
_diffrn_orient_matrix_UB_31      0.0057168000
_diffrn_orient_matrix_UB_32      0.0318302000
_diffrn_orient_matrix_UB_33      -0.0382438000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.1532
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32709
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.908
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic brownish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL P180605A1 in P-1 #2
CELL   16.2557   17.0114   17.9430     72.07     68.53     86.63
SPGR P-1
C101 0.246 0.283 0.376 !      24.01 eA-3
C102 0.121 0.263 0.300 !      22.50 eA-3
C103 0.441 0.921 0.471 !      19.01 eA-3
C104 0.466 0.099 0.341 !      17.81 eA-3
C105 0.707 0.143 0.312 !      15.10 eA-3
C106 0.762 0.185 0.124 !      11.43 eA-3
C107 0.922 0.409 0.278 !      11.29 eA-3
C108 0.855 0.231 0.389 !      10.53 eA-3
C109 0.984 0.109 0.245 !       9.57 eA-3
C110 0.732 0.151 0.158 !       8.39 eA-3
C111 0.029 0.188 0.078 !       7.56 eA-3
C112 0.515 0.997 0.373 !       6.27 eA-3
C113 1.003 0.453 0.061 !       6.27 eA-3
C114 0.999 0.400 0.030 !       6.05 eA-3
C115 0.218 0.333 0.278 !       6.04 eA-3
C116 0.873 0.333 0.390 !       5.18 eA-3
C117 0.685 0.206 0.222 !       5.15 eA-3
Q118 0.580 0.775 0.266 !       4.96 eA-3
Q119 0.560 0.823 0.310 !       4.47 eA-3
Q120 0.345 0.878 0.318 !       4.24 eA-3
Q121 0.511 0.673 0.283 !       3.93 eA-3
Q122 0.362 0.838 0.265 !       3.90 eA-3
Q123 0.437 0.535 0.156 !       3.70 eA-3
Q124 0.530 0.624 0.232 !       3.69 eA-3
Q125 0.422 0.584 0.201 !       3.55 eA-3
C126 0.904 0.314 0.265 !       3.53 eA-3
C127 0.950 0.504 0.085 !       3.51 eA-3
C128 0.955 0.184 0.187 !       3.29 eA-3
Q129 0.355 0.672 0.234 !       3.25 eA-3
Q130 0.719 0.565 0.489 !       3.22 eA-3
Q131 0.751 0.527 0.435 !       3.14 eA-3
Q132 0.329 0.727 0.286 !       3.06 eA-3
Q133 0.291 0.370 0.050 !       2.94 eA-3
Q134 0.610 0.129 0.051 !       2.71 eA-3
Q135 0.575 0.283 0.074 !       2.71 eA-3
C136 0.933 0.147 0.182 !       2.70 eA-3
Q137 0.636 0.340 0.393 !       2.65 eA-3
Q138 0.105 0.624 0.109 !       2.60 eA-3
C139 0.996 0.500 0.020 !       2.54 eA-3
C140 0.970 0.270 0.094 !       2.53 eA-3
Q141 0.377 0.313 0.360 !       2.39 eA-3
Q142 1.000 0.701 0.363 !       2.36 eA-3
C143 0.967 0.395 0.172 !       2.34 eA-3
C144 0.991 0.221 0.038 !       2.33 eA-3
Q145 0.386 0.680 0.404 !       2.32 eA-3
Q146 0.882 0.981 0.092 !       2.30 eA-3
C147 0.970 0.313 0.076 !       2.27 eA-3
Q148 0.631 0.560 0.379 !       2.26 eA-3
Q149 0.034 0.589 0.177 !       2.25 eA-3
C150 0.860 0.254 0.331 !       2.23 eA-3
Q151 0.034 0.858 0.397 !       2.23 eA-3
C152 0.980 0.243 0.158 !       2.20 eA-3
Q153 0.041 0.612 0.148 !       2.19 eA-3
C154 0.995 0.170 0.136 !       2.18 eA-3
Q155 0.840 0.921 0.377 !       2.18 eA-3
C156 0.468 0.030 0.388 !       2.15 eA-3
Q157 0.622 0.077 0.001 !       2.11 eA-3
C158 0.010 0.138 0.165 !       2.11 eA-3
C159 0.639 0.095 0.500 !       2.05 eA-3
C160 0.043 0.297 0.089 !       2.04 eA-3
Q161 0.987 0.707 0.019 !       2.03 eA-3
Q162 0.158 0.649 0.047 !       2.03 eA-3
C163 0.944 0.086 0.221 !       2.02 eA-3
C164 0.828 0.157 0.266 !       2.02 eA-3
Q165 0.551 0.518 0.169 !       2.02 eA-3
C166 0.796 0.133 0.163 !       2.00 eA-3
Q167 0.784 0.764 0.388 !       1.98 eA-3
Q168 0.674 0.579 0.174 !       1.97 eA-3
C169 0.827 0.193 0.111 !       1.95 eA-3
Q170 0.876 0.625 0.196 !       1.94 eA-3
Q171 0.765 0.888 0.422 !       1.94 eA-3
Q172 0.986 0.752 0.454 !       1.93 eA-3
C173 0.968 0.307 0.143 !       1.92 eA-3
Q174 0.500 0.747 0.110 !       1.90 eA-3
Q175 0.997 0.219 0.499 !       1.90 eA-3
C176 0.964 0.351 0.286 !       1.87 eA-3
Q177 0.109 0.797 0.167 !       1.87 eA-3
C178 0.048 0.186 0.157 !       1.87 eA-3
Q179 0.771 0.402 0.109 !       1.86 eA-3
Q180 0.855 0.360 0.047 !       1.86 eA-3
Q181 0.222 0.651 0.172 !       1.85 eA-3
C182 0.807 0.388 0.419 !       1.85 eA-3
C183 0.091 0.175 0.180 !       1.85 eA-3
C184 0.051 0.409 0.268 !       1.85 eA-3
C185 0.973 0.033 0.186 !       1.85 eA-3
Q186 0.300 0.812 0.449 !       1.84 eA-3
Q187 0.439 0.395 0.006 !       1.84 eA-3
C188 0.956 0.092 0.339 !       1.82 eA-3
C189 0.061 0.468 0.091 !       1.81 eA-3
C190 0.589 0.123 0.471 !       1.81 eA-3
C191 0.012 0.232 0.175 !       1.80 eA-3
C192 0.809 0.235 0.184 !       1.80 eA-3
Q193 0.489 0.359 0.425 !       1.79 eA-3
C194 0.246 0.238 0.252 !       1.78 eA-3
Q195 0.889 0.810 0.173 !       1.78 eA-3
C196 0.512 0.907 0.474 !       1.77 eA-3
C197 0.429 0.041 0.439 !       1.77 eA-3
Q198 0.861 0.798 0.374 !       1.76 eA-3
Q199 0.582 0.328 0.391 !       1.75 eA-3
;
_refine_diff_density_max         1.551
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         15431
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1420
_refine_ls_R_factor_gt           0.0914
_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^)+(0.0977P)^2^+15.6558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2115
_refine_ls_wR_factor_ref         0.2430
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9246
_reflns_number_total             15431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04263f2.cif
_cod_data_source_block           CuI3CuII2(OMe)2pz5
_cod_depositor_comments
'Adding full bibliography for 7703129--7703138.cif.'
_cod_database_code               7703134
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C N O Cu'
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.819
_reflns_odcompleteness_completeness 99.79
_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. Rigid bond restraints
 C54, C53
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.05
3. Uiso/Uaniso restraints and constraints
C53 \\sim C54: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(N10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C45(H45), C24(H24), C47(H47), C53(H53), C57(H57), C65(H65), C35(H35),
 C51(H51), C25(H25), C21(H21), C17(H17), C39(H39), C62(H62), C48(H48), C56(H56),
  C75(H75), C68(H68), C59(H59), C55(H55), C41(H41), C23(H23), C44(H44),
 C49(H49), C18(H18), C27(H27), C74(H74), C71(H71), C50(H50), C61(H61), C67(H67),
  C26(H26), C73(H73), C42(H42), C60(H60), C20(H20), C66(H66), C37(H37),
 C33(H33), C54(H54), C19(H19), C36(H36), C31(H31), C38(H38), C29(H29), C69(H69),
  C63(H63), C72(H72), C32(H32), C30(H30), C43(H43)
4.b Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C), C76(H76A,H76B,H76C)
;
_platon_squeeze_void_probe_radius 1.20
_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 1.362
_oxdiff_exptl_absorpt_empirical_full_min 0.736