Diosmium compounds containing bis(imidazole)-p-quinone bridging ligands
Dhara, Suman; Ansari, Mohd. Asif; Schwederski, Brigitte; Filippou, Vasileios; Kaim, Wolfgang; Lahiri, Goutam Kumar; Dalton Transactions  (2022) –; doi:10.1039/D2DT00184E

data_7709471
_publ_section_title
;
 Diosmium compounds containing bis(imidazole)-p-quinone bridging ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00184E
_journal_year                    2022
_chemical_formula_moiety         'C31 H23 N6 O Os, Cl O4'
_chemical_formula_sum            'C31 H23 Cl N6 O5 Os'
_chemical_formula_weight         785.20
_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             2021-05-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-11 deposited with the CCDC.	2022-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                101.594(2)
_cell_angle_beta                 106.424(2)
_cell_angle_gamma                94.7480(10)
_cell_formula_units_Z            2
_cell_length_a                   9.43780(10)
_cell_length_b                   12.8016(2)
_cell_length_c                   13.6171(3)
_cell_measurement_reflns_used    28519
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.6490
_cell_measurement_theta_min      1.6360
_cell_volume                     1528.72(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -339.92  20.08   1.00    3.00  15.81  -9.84 -59.25    --   360
  2  \w    -64.97 -10.97   1.00    3.00    --   -9.90 109.93 133.90   54
  3  \w    -60.71  -7.71   1.00    3.00    --   -9.90 102.93  -2.37   53
  4  \w   -100.81  15.19   1.00    3.00    --   -9.84 -59.25 164.08  116
  5  \w    -54.83   2.17   1.00    3.00    --   -9.90  92.35 -96.41   57
  6  \w   -100.81  15.19   1.00    3.00    --   -9.84 -59.25  20.08  116
  7  \w    -51.63  20.37   1.00    3.00    --   -9.90  86.45  91.55   72
  8  \w    -45.37  31.63   1.00    3.00    --   -9.90  75.16-169.78   77
  9  \w    -48.00  27.00   1.00    3.00    --   -9.90  79.79 -26.21   75
 10  \w    -49.82  23.18   1.00    3.00    --   -9.90  83.20-131.37   73
 11  \w   -100.81  15.19   1.00    3.00    --   -9.84 -59.25-123.92  116
 12  \f   -349.73  10.27   1.00    3.00   6.61  -9.84 -31.50    --   360
 13  \w    -24.93  51.07   1.00    3.00    --    9.90 -85.85  51.47   76
 14  \w   -100.81  15.19   1.00    3.00    --   -9.84 -59.25  92.08  116
 15  \w   -100.81  15.19   1.00    3.00    --   -9.84 -59.25 -51.92  116
 16  \f    -10.27 349.73   1.00    3.00  81.02  -9.84  31.50    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0292002000
_diffrn_orient_matrix_UB_12      0.0511083000
_diffrn_orient_matrix_UB_13      0.0351919000
_diffrn_orient_matrix_UB_21      0.0137904000
_diffrn_orient_matrix_UB_22      -0.0248165000
_diffrn_orient_matrix_UB_23      0.0432314000
_diffrn_orient_matrix_UB_31      0.0723521000
_diffrn_orient_matrix_UB_32      -0.0065913000
_diffrn_orient_matrix_UB_33      -0.0036819000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            95989
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.604
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.308
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.84
_exptl_crystal_size_mid          0.66
_exptl_crystal_size_min          0.54
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+3.4650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5082
_reflns_number_total             5381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00184e2.cif
_cod_data_source_block           3
_cod_database_code               7709471
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.204
_shelx_estimated_absorpt_t_min   0.123
_reflns_odcompleteness_completeness 92.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.75
_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.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C7(H7), C6(H6), C20(H20), C12(H12), C19(H19), C23(H23),
 C25(H25), C30(H30), C18(H18), C10(H10), C28(H28), C14(H14), C15(H15), C29(H29),
  C31(H31), C13(H13), C24(H24), C9(H9)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              92074
_shelx_hkl_checksum              88435
_shelx_fab_checksum              40648
_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 1.402
_oxdiff_exptl_absorpt_empirical_full_min 0.710