Osmium Bisterpyridine Complexes with Redox-Active Amine Substituents: A Comparison Study with Ruthenium Analogues.
Sun, Meng-Jia; Shao, Jiang-Yang; Yao, Chang-Jiang; Zhong, Yu-Wu; Yao, Jiannian; Inorganic chemistry 54 (2015) 8136–8147; doi:10.1021/acs.inorgchem.5b01420

data_4344044
_publ_section_title
;
 Osmium Bisterpyridine Complexes with Redox-Active Amine Substituents: A
 Comparison Study with Ruthenium Analogues.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8136
_journal_page_last               8147
_journal_paper_doi               10.1021/acs.inorgchem.5b01420
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C58 H48 N8 O4 Os, 2(F6 P)'
_chemical_formula_sum            'C58 H48 F12 N8 O4 Os P2'
_chemical_formula_weight         1401.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                110.71(3)
_cell_angle_beta                 97.09(3)
_cell_angle_gamma                93.99(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0219(18)
_cell_length_b                   16.256(3)
_cell_length_c                   22.750(4)
_cell_measurement_reflns_used    8896
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      26.3713
_cell_measurement_theta_min      1.3427
_cell_volume                     3073.9(12)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2013)'
_computing_structure_solution
;
'SHELXS (Sheldrick, 2013)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0056
_diffrn_orient_matrix_UB_12      0.0730
_diffrn_orient_matrix_UB_13      -0.0854
_diffrn_orient_matrix_UB_21      -0.0372
_diffrn_orient_matrix_UB_22      0.0398
_diffrn_orient_matrix_UB_23      0.0371
_diffrn_orient_matrix_UB_31      0.0460
_diffrn_orient_matrix_UB_32      0.0048
_diffrn_orient_matrix_UB_33      0.0111
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12468
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.423
_diffrn_reflns_theta_min         1.914
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.214
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       plate
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         6.476
_refine_diff_density_min         -5.593
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         12468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0804
_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^)+(0.1392P)^2^+10.4731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2086
_refine_ls_wR_factor_ref         0.2107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12011
_reflns_number_total             12468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01420_si_003.cif
_cod_data_source_block           a_sq
_cod_depositor_comments          'Adding full bibliography for 4344044.cif.'
_cod_original_formula_sum        'C58 H48 F12 N8 O4 Os P2 '
_cod_database_code               4344044
_shelxl_version_number           2013-4
_diffrn_number_total             12471
_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:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C24(H24), C25(H25), C27(H27),
  C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C36(H36), C38(H38),
 C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C49(H49), C50(H50),
  C53(H53), C54(H54), C56(H56), C57(H57)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C29(H29A,H29B,H29C), C51(H51A,H51B,H51C), C58(H58A,H58B,
 H58C)
;
_shelx_res_checksum              29861
_shelx_hkl_checksum              92245
_shelx_fab_checksum              95682