Electrochromic behavior of fac-tricarbonyl rhenium complexes
Zhou, Qian-hua; Pan, Ming-yue; He, Qi; Tang, Qian; Chow, Cheuk-fai; Gong, Cheng-bin; New Journal of Chemistry 46 (2022) 1072–1079; doi:10.1039/D1NJ04955K

data_7061136
_publ_section_title
;
 Electrochromic behavior of fac-tricarbonyl rhenium complexes
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1072
_journal_page_last               1079
_journal_paper_doi               10.1039/D1NJ04955K
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         '2(C15.5 H10 Cl0.5 N O3.5 Re0.5)'
_chemical_formula_sum            'C31 H20 Cl N2 O7 Re'
_chemical_formula_weight         754.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2021-12-09 deposited with the CCDC.	2021-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.965(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5221(4)
_cell_length_b                   20.0965(7)
_cell_length_c                   16.7407(5)
_cell_measurement_reflns_used    12882
_cell_measurement_temperature    287.64(16)
_cell_measurement_theta_max      26.8220
_cell_measurement_theta_min      3.8280
_cell_volume                     3080.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      287.64(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.860
_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    -10.00  84.00   1.00   23.08    --   16.35  77.00-120.00   94
  2  \w    -10.00  84.00   1.00   23.08    --   16.35  77.00  90.00   94
  3  \w    -10.00  80.00   1.00   23.08    --   16.35  77.00   0.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0770766000
_diffrn_orient_matrix_UB_12      -0.0021182000
_diffrn_orient_matrix_UB_13      0.0087560000
_diffrn_orient_matrix_UB_21      -0.0066237000
_diffrn_orient_matrix_UB_22      -0.0322842000
_diffrn_orient_matrix_UB_23      -0.0177718000
_diffrn_orient_matrix_UB_31      -0.0035885000
_diffrn_orient_matrix_UB_32      0.0140797000
_diffrn_orient_matrix_UB_33      -0.0393776000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.860
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18864
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.161
_diffrn_reflns_theta_min         3.495
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.080
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       plate
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.216
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         7336
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0440P)^2^+3.7150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5249
_reflns_number_total             7336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj04955k2.cif
_cod_data_source_block           gcb
_cod_depositor_comments          'Adding full bibliography for 7061136.cif.'
_cod_database_code               7061136
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 O1 N1 Re1'
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.496
_reflns_odcompleteness_completeness 98.49
_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. Restrained distances
 C2-O2 \\sim C1-O1
 with sigma of 0.001
3. Others
 Sof(Re2A)=0.5*(1-FVAR(2))
 Sof(Re2)=0.5*FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C21(H21), C24(H24), C30(H30), C8(H8), C23(H23), C14(H14), C5(H5),
 C26(H26), C27(H27), C11(H11), C7(H7), C13(H13), C10(H10)
4.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C32(H32A,H32B,H32C)
;
_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 1.937
_oxdiff_exptl_absorpt_empirical_full_min 0.495