Cyclometalated Osmium-Amine Electronic Communication through the p-Oligophenylene Wire.
Shen, Jun-Jian; Shao, Jiang-Yang; Gong, Zhong-Liang; Zhong, Yu-Wu; Inorganic chemistry 54 (2015) 10776–10784; doi:10.1021/acs.inorgchem.5b01828

data_4344429
_publ_section_title
;
 Cyclometalated Osmium-Amine Electronic Communication through the
 p-Oligophenylene Wire.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10776
_journal_page_last               10784
_journal_paper_doi               10.1021/acs.inorgchem.5b01828
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C57 H43 N6 O2 Os, F6 P'
_chemical_formula_sum            'C57 H43 F6 N6 O2 Os P'
_chemical_formula_weight         1179.14
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.784(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.214(3)
_cell_length_b                   15.470(3)
_cell_length_c                   24.639(5)
_cell_measurement_reflns_used    16355
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4838
_cell_measurement_theta_min      1.5608
_cell_volume                     5339.1(19)
_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 0.997
_diffrn_measured_fraction_theta_max 0.994
_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      -0.0009
_diffrn_orient_matrix_UB_12      0.0626
_diffrn_orient_matrix_UB_13      0.0343
_diffrn_orient_matrix_UB_21      0.0518
_diffrn_orient_matrix_UB_22      -0.0180
_diffrn_orient_matrix_UB_23      0.0342
_diffrn_orient_matrix_UB_31      0.0241
_diffrn_orient_matrix_UB_32      0.0221
_diffrn_orient_matrix_UB_33      -0.0250
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            42007
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         2.415
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.486
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5998
_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    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.361
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         12190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+10.2161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10924
_reflns_number_total             12190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01828_si_002.cif
_cod_data_source_block           sa3511_sq
_cod_depositor_comments
'Adding full bibliography for 4344428--4344429.cif.'
_cod_original_cell_volume        5339.2(19)
_cod_database_code               4344429
_shelxl_version_number           2013-4
_diffrn_number_total             12655
_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), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C24(H24),
  C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C36(H36),
 C37(H37), C39(H39), C40(H40), C42(H42), C43(H43), C45(H45), C46(H46), C48(H48),
  C49(H49), C52(H52), C53(H53), C55(H55), C56(H56)
2.b Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C57(H57A,H57B,H57C)
;
_shelx_res_checksum              35132
_shelx_hkl_checksum              64000
_shelx_fab_checksum              10923