;   () –; doi:10.1039/D3DT00929G

data_1569092
_journal_paper_doi               10.1039/D3DT00929G
_chemical_formula_moiety         'C60 H44 N14 O2 Os2 S2, 2(Cl O4)'
_chemical_formula_sum            'C60 H44 Cl2 N14 O10 Os2 S2'
_chemical_formula_weight         1636.51
_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             2022-09-26
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-09-28 deposited with the CCDC.	2023-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                69.494(5)
_cell_angle_beta                 75.258(4)
_cell_angle_gamma                66.084(5)
_cell_formula_units_Z            1
_cell_length_a                   10.4463(5)
_cell_length_b                   11.9209(6)
_cell_length_c                   13.9309(8)
_cell_measurement_reflns_used    12337
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      24.9760
_cell_measurement_theta_min      1.9410
_cell_volume                     1472.50(15)
_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 (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      N~2~
_diffrn_ambient_temperature      150.00(10)
_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   -349.73  10.27   0.50    3.00   6.61  -9.84 -31.50    --   720
  2  \w    -65.46   0.04   0.50    3.00    --  -19.34  94.56 145.16  131
  3  \w    -60.89   0.11   0.50    3.00    --  -14.77  94.56 -34.84  122
  4  \w   -100.81  15.69   0.50    3.00    --   -9.84 -59.25  20.08  233
  5  \f    -10.27 349.73   0.50    3.00  81.02  -9.84  31.50    --   720
  6  \w    -65.46   0.04   0.50    3.00    --  -19.34  94.56  73.16  131
  7  \w   -100.81  15.69   0.50    3.00    --   -9.84 -59.25-123.92  233
  8  \w    -65.46   0.04   0.50    3.00    --  -19.34  94.56   1.16  131
;
_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      -0.0362568000
_diffrn_orient_matrix_UB_12      0.0393153000
_diffrn_orient_matrix_UB_13      0.0336905000
_diffrn_orient_matrix_UB_21      -0.0145384000
_diffrn_orient_matrix_UB_22      -0.0524272000
_diffrn_orient_matrix_UB_23      0.0386450000
_diffrn_orient_matrix_UB_31      0.0639369000
_diffrn_orient_matrix_UB_32      -0.0173635000
_diffrn_orient_matrix_UB_33      0.0194526000
_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     0.0294
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            48607
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.574
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.546
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70819
_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    1.845
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0217
_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^)+(0.0175P)^2^+1.4265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4779
_reflns_number_total             5191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00929g2.cif
_cod_data_source_block           '[4](ClO4)2'
_cod_database_code               1569092
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 79.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.96
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C20(H20), C19(H19), C6(H6), C11(H11), C10(H10), C9(H9), C23(H23),
 C15(H15), C21(H21), C18(H18), C12(H12), C16(H16), C30(H30), C26(H26), C17(H17),
  C8(H8), C7(H7), C22(H22), C29(H29), C28(H28), C27(H27)
;
_shelx_res_checksum              59572
_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 1.938
_oxdiff_exptl_absorpt_empirical_full_min 0.732