;   () –; doi:10.1039/D3DT00929G

data_1569094
_journal_paper_doi               10.1039/D3DT00929G
_chemical_formula_moiety         'C56 H40 N10 O2 Os2 S2, 2(F6 P), C3 H6 O'
_chemical_formula_sum            'C59 H46 F12 N10 O3 Os2 P2 S2'
_chemical_formula_weight         1677.52
_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                115.641(2)
_cell_angle_beta                 92.209(2)
_cell_angle_gamma                110.913(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5131(2)
_cell_length_b                   16.6520(3)
_cell_length_c                   18.5981(3)
_cell_measurement_reflns_used    51281
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      31.6290
_cell_measurement_theta_min      1.7040
_cell_volume                     3430.48(14)
_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      110(1)
_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   -339.92  20.08   0.60    1.00  15.81  -9.84 -59.25    --   600
  2  \w    -65.46  -0.06   0.60    1.00    --  -19.34  94.56 145.16  109
  3  \w    -60.89   0.31   0.60    1.00    --  -14.77  94.56 -34.84  102
  4  \w   -100.81  15.59   0.60    1.00    --   -9.84 -59.25 -51.92  194
  5  \w   -100.81  15.59   0.60    1.00    --   -9.84 -59.25 164.08  194
  6  \w    -65.46  -0.06   0.60    1.00    --  -19.34  94.56  73.16  109
  7  \w   -100.81  15.59   0.60    1.00    --   -9.84 -59.25  20.08  194
  8  \w    -65.46  -0.06   0.60    1.00    --  -19.34  94.56   1.16  109
  9  \f   -349.73  10.27   0.60    1.00   6.61  -9.84 -31.50    --   600
;
_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      -0.0429140000
_diffrn_orient_matrix_UB_12      -0.0388832000
_diffrn_orient_matrix_UB_13      0.0013357000
_diffrn_orient_matrix_UB_21      0.0361258000
_diffrn_orient_matrix_UB_22      -0.0218186000
_diffrn_orient_matrix_UB_23      0.0011151000
_diffrn_orient_matrix_UB_31      0.0136334000
_diffrn_orient_matrix_UB_32      0.0266127000
_diffrn_orient_matrix_UB_33      0.0434263000
_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  0.0826
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            127162
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.657
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.889
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20532
_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    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.48
_refine_diff_density_max         1.900
_refine_diff_density_min         -1.803
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         12074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0267P)^2^+49.0071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10967
_reflns_number_total             12074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00929g2.cif
_cod_data_source_block           '[3](PF6)2'
_cod_original_cell_volume        3430.47(12)
_cod_database_code               1569094
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.257
_shelx_estimated_absorpt_t_min   0.211
_reflns_odcompleteness_completeness 79.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.84
_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:
 C40(H40), C15(H15), C7(H7), C6(H6), C13(H13), C55(H55), C8(H8), C43(H43),
 C56(H56), C50(H50), C28(H28), C37(H37), C27(H27), C36(H36), C16(H16), C9(H9),
 C49(H49), C45(H45), C44(H44), C23(H23), C47(H47), C46(H46), C34(H34), C19(H19),
  C24(H24), C35(H35), C25(H25), C20(H20), C14(H14), C38(H38), C17(H17),
 C53(H53), C39(H39), C30(H30), C33(H33), C54(H54), C48(H48), C26(H26), C29(H29),
  C18(H18)
2.b Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C59(H59A,H59B,H59C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7000
_shelx_fab_checksum              39377
_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 2.433
_oxdiff_exptl_absorpt_empirical_full_min 0.480