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_7709472
_publ_section_title
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 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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-03-30
_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                90
_cell_angle_beta                 93.9530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.48690(10)
_cell_length_b                   18.5944(2)
_cell_length_c                   33.9047(4)
_cell_measurement_reflns_used    43707
_cell_measurement_temperature    150.00(2)
_cell_measurement_theta_max      27.7870
_cell_measurement_theta_min      2.0370
_cell_volume                     6595.61(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -94.27  89.73   1.00    2.00  81.02  -9.84  31.50    --   184
  2  \w   -100.81  15.19   1.00    2.00    --   -9.84 -59.25  20.08  116
  3  \w   -100.81  15.19   1.00    2.00    --   -9.84 -59.25-123.92  116
  4  \w   -100.81  15.19   1.00    2.00    --   -9.84 -59.25  92.08  116
  5  \w   -100.81  15.19   1.00    2.00    --   -9.84 -59.25 -51.92  116
  6  \f     32.08 216.08   1.00    2.00  15.81  -9.84 -59.25    --   184
;
_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      -0.0159189000
_diffrn_orient_matrix_UB_12      -0.0037516000
_diffrn_orient_matrix_UB_13      0.0198849000
_diffrn_orient_matrix_UB_21      -0.0036419000
_diffrn_orient_matrix_UB_22      0.0379369000
_diffrn_orient_matrix_UB_23      0.0017655000
_diffrn_orient_matrix_UB_31      -0.0658312000
_diffrn_orient_matrix_UB_32      -0.0011943000
_diffrn_orient_matrix_UB_33      -0.0064027000
_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  0.0780
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            153473
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.628
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.076
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    1.641
_exptl_crystal_description       block
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.84
_exptl_crystal_size_mid          0.68
_exptl_crystal_size_min          0.54
_refine_diff_density_max         1.389
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         11607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0421P)^2^+30.5935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10375
_reflns_number_total             11607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00184e2.cif
_cod_data_source_block           2
_cod_database_code               7709472
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.217
_shelx_estimated_absorpt_t_min   0.131
_reflns_odcompleteness_completeness 89.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.80
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C39(H39), C19(H19), C29(H29), C10(H10), C28(H28),
 C49(H49), C20(H20), C46(H46), C50(H50), C25(H25), C48(H48), C42(H42), C45(H45),
  C38(H38), C22(H22), C9(H9), C26(H26), C55(H55), C16(H16), C21(H21), C18(H18),
 C47(H47), C40(H40), C35(H35), C15(H15), C57(H57), C17(H17), C30(H30), C56(H56),
  C41(H41), C27(H27), C51(H51), C36(H36), C32(H32), C58(H58), C37(H37),
 C52(H52), C31(H31)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              55701
_shelx_hkl_checksum              92184
_shelx_fab_checksum              26490
_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 2.282
_oxdiff_exptl_absorpt_empirical_full_min 0.621