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_7710978
_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         'C24 H4 Cl8 Cu3 O18, 2(C5 H13 Br N)'
_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     iterative
_audit_creation_date             2022-01-20
_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                98.477(2)
_cell_angle_beta                 95.120(2)
_cell_angle_gamma                95.417(2)
_cell_formula_units_Z            1
_cell_length_a                   7.2675(2)
_cell_length_b                   12.4908(3)
_cell_length_c                   12.5292(3)
_cell_measurement_reflns_used    5618
_cell_measurement_temperature    299.99(10)
_cell_measurement_theta_max      75.8100
_cell_measurement_theta_min      3.6060
_cell_volume                     1113.75(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.952
_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    -42.00 -16.00   0.50    0.68    --  -43.10  38.00 -90.00   52
  2  \w    -16.00  20.00   0.50    0.68    --  -43.10  19.00 -90.00   72
  3  \w      4.00  34.00   0.50    0.68    --  -43.10  38.00 -90.00   60
  4  \w    -44.00 -13.00   0.50    2.73    --  -90.25  45.00 -30.00   62
  5  \w    -64.00 -15.00   0.50    2.73    --  -90.25  61.00  60.00   98
  6  \w    -70.00 -32.00   0.50    2.73    --  -90.25  61.00   0.00   76
  7  \w    -91.00 -47.00   0.50    2.73    --  -90.25 125.00 120.00   88
  8  \w   -114.00  -6.00   0.50    0.68    --  -43.10 -19.00  90.00  216
  9  \w    -25.00  66.00   0.50    0.68    --   43.10 -57.00  90.00  182
 10  \w     48.00  93.00   0.50    0.68    --   43.10-125.00 -30.00   90
 11  \w     36.00  75.00   0.50    2.73    --  111.75 -94.00-120.00   78
 12  \w     44.00 104.00   0.50    2.73    --  111.75 -77.00 -60.00  120
 13  \w     70.00 103.00   0.50    2.73    --  111.75 -94.00 -30.00   66
 14  \w     43.00  69.00   0.50    2.73    --  111.75 -61.00  30.00   52
 15  \w     41.00  67.00   0.50    2.73    --  111.75 -61.00 -30.00   52
 16  \w     53.00 122.00   0.50    2.73    --  111.75  15.00  60.00  138
 17  \w    141.00 169.00   0.50    2.73    --  111.75  15.00  60.00   56
 18  \w     86.00 155.00   0.50    2.73    --  111.75  61.00  30.00  138
 19  \w     87.00 150.00   0.50    2.73    --  111.75  45.00 -60.00  126
 20  \w    124.00 176.00   0.50    2.73    --  111.75   0.00-150.00  104
 21  \w     92.00 125.00   0.50    2.73    --  111.75 125.00-150.00   66
 22  \w    139.00 167.00   0.50    2.73    --  111.75 125.00-150.00   56
 23  \w     39.00  65.00   0.50    2.73    --  111.75 -61.00  90.00   52
 24  \w     36.00  81.00   0.50    2.73    --  111.75 -94.00 150.00   90
 25  \w     68.00 116.00   0.50    2.73    --  111.75-125.00 150.00   96
 26  \w     70.00 116.00   0.50    2.73    --  111.75-125.00  90.00   92
 27  \w     41.00  69.00   0.50    2.73    --  111.75 -61.00 120.00   56
 28  \w     41.00  68.00   0.50    2.73    --  111.75 -61.00  60.00   54
 29  \w     38.00  69.00   0.50    2.73    --  111.75 -61.00 150.00   62
 30  \w     39.00 117.00   0.50    2.73    --  111.75-125.00 -30.00  156
 31  \w     51.00  77.00   0.50    2.73    --  111.75 -94.00-150.00   52
 32  \w     59.00 109.00   0.50    2.73    --  111.75 -94.00-180.00  100
 33  \w     39.00 111.00   0.50    2.73    --  111.75-125.00 -60.00  144
 34  \w     37.00  69.00   0.50    2.73    --  111.75 -61.00-180.00   64
 35  \w     37.00 121.00   0.50    2.73    --  111.75   0.00-150.00  168
 36  \w   -107.00 -70.00   0.50    0.68    --  -43.10-125.00  90.00   74
 37  \w   -138.00-113.00   0.50    2.73    --  -90.25 -94.00-120.00   50
 38  \w   -118.00 -91.00   0.50    0.68    --  -43.10-125.00-150.00   54
;
_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      -0.1358037000
_diffrn_orient_matrix_UB_12      -0.0866048000
_diffrn_orient_matrix_UB_13      0.0362756000
_diffrn_orient_matrix_UB_21      0.1569241000
_diffrn_orient_matrix_UB_22      -0.0741497000
_diffrn_orient_matrix_UB_23      0.0087289000
_diffrn_orient_matrix_UB_31      0.0532109000
_diffrn_orient_matrix_UB_32      0.0523879000
_diffrn_orient_matrix_UB_33      0.1193207000
_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  0.0417
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_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            10326
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.316
_diffrn_reflns_theta_min         3.599
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.873
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
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    2.070
_exptl_crystal_description       plate
_exptl_crystal_F_000             685
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.188
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4443
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0608
_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^)+(0.1168P)^2^+1.4522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.1795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4031
_reflns_number_total             4443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01980a2.cif
_cod_data_source_block           exp_1049
_cod_database_code               7710978
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.843
_shelx_estimated_absorpt_t_min   0.665
_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. Restrained distances
 H9a-O4_$1
 2.05 with sigma of 0.01
 O3_$2-H9b
 2.13 with sigma of 0.01
3.a Rotating group:
 O9(H9a,H9b)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C13(H13a,H13b)
3.c Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C15(H15a,H15b,H15c)
;
_shelx_res_checksum              41142
_shelx_hkl_checksum              74797
_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 4.226
_oxdiff_exptl_absorpt_empirical_full_min 0.567