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_7709470
_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         'C58 H40 N14 O2 Os2, 2(Cl O4), C H2 Cl2'
_chemical_formula_sum            'C59 H42 Cl4 N14 O10 Os2'
_chemical_formula_weight         1629.26
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-08-11 deposited with the CCDC.	2022-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                75.546(2)
_cell_angle_beta                 89.585(2)
_cell_angle_gamma                88.763(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1356(2)
_cell_length_b                   14.8336(4)
_cell_length_c                   17.2502(4)
_cell_measurement_reflns_used    27215
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.1880
_cell_measurement_theta_min      2.0890
_cell_volume                     3006.29(12)
_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 1.3 (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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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   -110.00  25.00   0.50    8.00    --  -20.00   0.00 -36.00  270
  2  \w   -110.00  19.00   0.50    8.00    --  -20.00 -72.00 -36.00  258
  3  \w    -73.00   5.00   0.50    8.00    --  -20.00 -72.00 108.00  156
  4  \w    -58.50   0.00   0.50    8.00    --  -20.00  72.00-108.00  117
  5  \w    -39.00  -9.00   0.50    8.00    --  -20.00 -72.00  36.00   60
  6  \w    -39.00  -9.00   0.50    8.00    --  -20.00 -72.00-108.00   60
  7  \w   -110.00  53.00   0.50    8.00    --  -20.00   0.00 108.00  326
  8  \w    -59.00  31.00   0.50    8.00    --  -20.00  72.00 108.00  180
  9  \w    -46.00  -6.00   0.50    8.00    --  -20.00  72.00 -36.00   80
 10  \w    -61.00  16.00   0.50    8.00    --  -20.00 -72.00-180.00  154
 11  \w    -59.00  -5.50   0.50    8.00    --  -20.00  72.00  36.00  107
 12  \w    -59.00 -28.50   0.50    8.00    --  -20.00  72.00-180.00   61
 13  \w   -110.00  14.00   0.50    8.00    --  -20.00   0.00-108.00  248
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0543548000
_diffrn_orient_matrix_UB_12      -0.0170535000
_diffrn_orient_matrix_UB_13      0.0061183000
_diffrn_orient_matrix_UB_21      -0.0211189000
_diffrn_orient_matrix_UB_22      0.0463156000
_diffrn_orient_matrix_UB_23      -0.0073742000
_diffrn_orient_matrix_UB_31      -0.0041584000
_diffrn_orient_matrix_UB_32      0.0018693000
_diffrn_orient_matrix_UB_33      -0.0413673000
_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  0.0694
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55837
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.678
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.472
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63229
_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 dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_description       block
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.096
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.615
_refine_diff_density_min         -1.950
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         10553
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0535P)^2^+14.0546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8910
_reflns_number_total             10553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00184e2.cif
_cod_data_source_block           1
_cod_original_cell_volume        3006.30(12)
_cod_database_code               7709470
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.722
_shelx_estimated_absorpt_t_min   0.673
_reflns_odcompleteness_completeness 91.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.06
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.001
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(N14) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
3.a Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B)
3.b Aromatic/amide H refined with riding coordinates:
 C50(H50), C45(H45), C51(H51), C12(H12), C27(H27), C17(H17), C20(H20),
 C21(H21), C41(H41), C47(H47), C58(H58), C22(H22), C9(H9), C11(H11), C31(H31),
 C26(H26), C30(H30), C18(H18), C28(H28), C16(H16), C46(H46), C57(H57), C49(H49),
  C19(H19), C29(H29), C15(H15), C40(H40), C32(H32), C37(H37), C38(H38),
 C25(H25), C55(H55), C48(H48), C52(H52), C39(H39), C35(H35), C36(H36), C42(H42),
  C56(H56), C10(H10)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              28774
_shelx_hkl_checksum              20946
_shelx_fab_checksum              15328
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.836
_oxdiff_exptl_absorpt_empirical_full_min 0.575