Organic-inorganic mixed-valence systems with strongly-coupled triarylamine and cyclometalated osmium
Hai-Jing Nie; Jiang-Yang Shao; Chang-Jiang Yao; Yu-Wu Zhong; Chem.Commun. 50 (2014) 10082–; doi:10.1039/C4cc04268A

data_7115534
_publ_section_title
;
 Organic-inorganic mixed-valence systems with strongly-coupled
 triarylamine and cyclometalated osmium
;
_journal_name_full               Chem.Commun.
_journal_page_first              10082
_journal_paper_doi               10.1039/C4cc04268A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C51 H41 N6 O8 Os, F6 P'
_chemical_formula_sum            'C51 H41 F6 N6 O8 Os P'
_chemical_formula_weight         1201.07
_chemical_name_systematic
;
 ?
;
_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             2014-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                106.442(4)
_cell_angle_beta                 90.995(3)
_cell_angle_gamma                94.554(4)
_cell_formula_units_Z            2
_cell_length_a                   9.349(2)
_cell_length_b                   14.949(4)
_cell_length_c                   20.583(5)
_cell_measurement_reflns_used    10521
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4829
_cell_measurement_theta_min      2.0651
_cell_volume                     2747.9(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 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0270
_diffrn_orient_matrix_UB_12      -0.0845
_diffrn_orient_matrix_UB_13      -0.0606
_diffrn_orient_matrix_UB_21      -0.0419
_diffrn_orient_matrix_UB_22      -0.0289
_diffrn_orient_matrix_UB_23      0.0481
_diffrn_orient_matrix_UB_31      -0.0465
_diffrn_orient_matrix_UB_32      0.0183
_diffrn_orient_matrix_UB_33      -0.0085
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34680
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.380
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.424
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5315
_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    1.452
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.836
_refine_diff_density_min         -1.439
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         12506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0462P)^2^+4.2250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11835
_reflns_number_total             12506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc04268a2.cif
_cod_data_source_block           sa3502_sq
_cod_database_code               7115534
_shelxl_version_number           2013-4
_diffrn_number_total             12517
_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), C13(H13), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C25(H25), C26(H26), C28(H28),
  C29(H29), C31(H31), C32(H32), C34(H34), C39(H39), C41(H41), C46(H46),
 C48(H48), C49(H49)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C30(H30A,H30B,H30C), C36(H36A,H36B,H36C), C44(H44A,H44B,
 H44C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              31012
_shelx_fab_checksum              70772