Thermal Induced Charge Transfer in Quinoid-bridged Linear Cu3 Compound
Liu, Xiao-Lin; Zhang, Xiao-Yi; Zhao, Hai-Xia; Long, La-Sheng; Zheng, Lansun; Dalton Transactions  (2022) –; doi:10.1039/D2DT01980A

data_7710977
_publ_section_title
;
 Thermal Induced Charge Transfer in Quinoid-bridged Linear Cu3 Compound
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01980A
_journal_year                    2022
_chemical_formula_moiety         '2(C5 H13 Br N), C24 H4 Cl8 Cu3 O18'
_chemical_formula_sum            'C34 H30 Br2 Cl8 Cu3 N2 O18'
_chemical_formula_weight         1388.64
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-21
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-22 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                98.008(2)
_cell_angle_beta                 94.863(2)
_cell_angle_gamma                95.210(2)
_cell_formula_units_Z            1
_cell_length_a                   7.1490(2)
_cell_length_b                   12.4532(4)
_cell_length_c                   12.4560(4)
_cell_measurement_reflns_used    8102
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.4500
_cell_measurement_theta_min      3.6080
_cell_volume                     1088.23(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_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_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     85.00 114.00   0.50    0.40    --  111.75  30.00  90.00   58
  2  \w     86.00 122.00   0.50    0.40    --  111.75  45.00 120.00   72
  3  \w    140.00 177.00   0.50    0.40    --  111.75  45.00 120.00   74
  4  \w     98.00 152.00   0.50    0.40    --  111.75  45.00 -60.00  108
  5  \w    112.00 156.00   0.50    0.40    --  111.75  61.00-180.00   88
  6  \w     97.00 176.00   0.50    0.40    --  111.75  30.00-120.00  158
  7  \w     85.00 177.00   0.50    0.40    --  111.75  30.00-180.00  184
  8  \w     85.00 176.00   0.50    0.40    --  111.75  30.00 -90.00  182
  9  \w    123.00 161.00   0.50    0.40    --  111.75  15.00  60.00   76
 10  \w     82.00 119.00   0.50    0.40    --  111.75  15.00  60.00   74
 11  \w    120.00 158.00   0.50    0.40    --  111.75  30.00  90.00   76
 12  \w    105.00 174.00   0.50    0.40    --  111.75  30.00 150.00  138
 13  \w   -122.00 -20.00   0.50    0.10    --  -43.10 -38.00   0.00  204
 14  \w    -90.00 -52.00   0.50    0.10    --  -43.10 -38.00-120.00   76
 15  \w   -117.00 -91.00   0.50    0.10    --  -43.10-125.00 -30.00   52
 16  \w   -157.00 -80.00   0.50    0.40    --  -90.25 -45.00  60.00  154
 17  \w     -6.00  29.00   0.50    0.10    --  -43.10  38.00-180.00   70
 18  \w    -91.00 -60.00   0.50    0.40    --  -90.25 125.00-150.00   62
 19  \w    -49.00 -14.00   0.50    0.40    --  -90.25  45.00-150.00   70
 20  \w    -46.00 -21.00   0.50    0.40    --  -90.25  45.00  30.00   50
 21  \w    -43.00  33.00   0.50    0.10    --  -43.10  38.00 150.00  152
 22  \w     38.00  70.00   0.50    0.40    --  111.75 -61.00 150.00   64
 23  \w     57.00  94.00   0.50    0.40    --  111.75 -77.00 150.00   74
 24  \w     47.00  78.00   0.50    0.40    --  111.75 -77.00 120.00   62
 25  \w     37.00  64.00   0.50    0.40    --  111.75 -77.00  30.00   54
 26  \w     46.00  73.00   0.50    0.40    --  111.75 -77.00 -30.00   54
 27  \w     74.00 103.00   0.50    0.40    --  111.75 -77.00   0.00   58
 28  \w     41.00  66.00   0.50    0.40    --  111.75 -77.00   0.00   50
 29  \w     37.00  70.00   0.50    0.40    --  111.75 -61.00  90.00   66
 30  \w    -29.00  72.00   0.50    0.10    --   43.10 -77.00 -30.00  202
 31  \w     38.00  70.00   0.50    0.40    --  111.75 -61.00  30.00   64
 32  \w     63.00 104.00   0.50    0.40    --  111.75 -77.00 -90.00   82
 33  \w     45.00  71.00   0.50    0.40    --  111.75 -61.00-120.00   52
 34  \w     37.00  71.00   0.50    0.40    --  111.75 -61.00 -90.00   68
 35  \w     43.00  84.00   0.50    0.40    --  111.75 -77.00-120.00   82
 36  \w     38.00  70.00   0.50    0.40    --  111.75 -61.00-180.00   64
 37  \w     79.00 130.00   0.50    0.40    --  111.75-143.00 -56.69  102
 38  \w     66.00 123.00   0.50    0.40    --  111.75-133.00-161.90  114
 39  \w     40.00  86.00   0.50    0.40    --  111.75-125.00 -90.00   92
 40  \w     67.00 101.00   0.50    0.40    --  111.75-125.00-120.00   68
 41  \w     60.00  98.00   0.50    0.10    --   43.10-125.00-150.00   76
 42  \w     41.00  66.00   0.50    0.40    --  111.75-125.00 -30.00   50
 43  \w     48.00  83.00   0.50    0.40    --  111.75-125.00   0.00   70
 44  \w     80.00 113.00   0.50    0.40    --  111.75-125.00  90.00   66
 45  \w     61.00  94.00   0.50    0.40    --  111.75-125.00 120.00   66
 46  \w     76.00 115.00   0.50    0.40    --  111.75-125.00 150.00   78
 47  \w     67.00 108.00   0.50    0.40    --  111.75 -94.00   0.00   82
 48  \w     91.00 117.00   0.50    0.40    --  111.75-125.00   0.00   52
 49  \w     73.00 116.00   0.50    0.40    --  111.75-125.00 -30.00   86
 50  \w     46.00  72.00   0.50    0.40    --  111.75 -94.00  30.00   52
 51  \w     36.00  94.00   0.50    0.40    --  111.75 -94.00  90.00  116
 52  \w     38.00  64.00   0.50    0.40    --  111.75 -94.00   0.00   52
 53  \w     81.00 117.00   0.50    0.40    --  111.75-125.00-150.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0294657000
_diffrn_orient_matrix_UB_12      0.1253047000
_diffrn_orient_matrix_UB_13      0.0265061000
_diffrn_orient_matrix_UB_21      0.0758402000
_diffrn_orient_matrix_UB_22      0.0058767000
_diffrn_orient_matrix_UB_23      -0.1114003000
_diffrn_orient_matrix_UB_31      -0.2016550000
_diffrn_orient_matrix_UB_32      0.0064388000
_diffrn_orient_matrix_UB_33      -0.0513874000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14696
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.401
_diffrn_reflns_theta_min         3.601
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.081
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53992
_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            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.119
_exptl_crystal_description       block
_exptl_crystal_F_000             685
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.173
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0455P)^2^+3.8118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4230
_reflns_number_total             4491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01980a2.cif
_cod_data_source_block           11
_cod_database_code               7710977
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.660
_shelx_estimated_absorpt_t_min   0.660
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O9(H9A,H9B)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C13(H13A,H13B)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              84496
_shelx_hkl_checksum              19364
_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 1.730
_oxdiff_exptl_absorpt_empirical_full_min 0.750