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_4344428
_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         'C63 H47 N6 O2 Os, 2.5(C H2 Cl2), F6 P'
_chemical_formula_sum            'C65.5 H52 Cl5 F6 N6 O2 Os P'
_chemical_formula_weight         1467.55
_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             2014-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.943(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   52.130(18)
_cell_length_b                   8.757(2)
_cell_length_c                   26.681(9)
_cell_measurement_reflns_used    16402
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.3688
_cell_measurement_theta_min      4.2497
_cell_volume                     12151(6)
_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 0.962
_diffrn_measured_fraction_theta_max 0.966
_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      0.0087
_diffrn_orient_matrix_UB_12      -0.0072
_diffrn_orient_matrix_UB_13      0.0358
_diffrn_orient_matrix_UB_21      0.0033
_diffrn_orient_matrix_UB_22      -0.1118
_diffrn_orient_matrix_UB_23      -0.0232
_diffrn_orient_matrix_UB_31      0.0190
_diffrn_orient_matrix_UB_32      0.0012
_diffrn_orient_matrix_UB_33      -0.0030
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_laue_measured_fraction_full 0.962
_diffrn_reflns_laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_h_min       -62
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            106506
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.198
_diffrn_reflns_theta_min         1.175
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.415
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5055
_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    1.604
_exptl_crystal_description       plate
_exptl_crystal_F_000             5864
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.609
_refine_diff_density_min         -1.404
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1562
_refine_ls_number_reflns         21159
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.245
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0885
_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^)+(0.0221P)^2^+113.1199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18650
_reflns_number_total             21159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01828_si_003.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 4344428--4344429.cif.'
_cod_original_cell_volume        12151(7)
_cod_database_code               4344428
_shelxl_version_number           2013-4
_diffrn_number_total             27209
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl8-C67 = Cl7-C67
 1.76 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl8 \\sim C67 \\sim Cl7: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(Cl8) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(Cl7) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B), C68(H68A,H68B), C66(H66A,H66B), C64(H64A,H64B), C65(H65A,H65B)
4.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C7A(H7A), C8A(H8A), C9A(H9A),
 C12A(H12A), C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A),
 C18A(H18A), C19A(H19A), C22A(H22A), C24A(H24A), C28A(H28A), C29A(H29A),
 C30A(H30A), C31A(H31A), C33A(H33A), C34A(H34A), C36A(H36A), C37A(H37A),
 C39A(H39A), C40A(H40A), C42A(H42A), C43A(H43A), C45A(H45A), C46A(H46A),
 C48A(H48A), C49A(H49A), C51A(H51A), C52A(H52A), C54A(H54A), C55A(H55A),
 C58A(H58A), C59A(H59A), C61A(H61A), C62A(H62A), 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), C51(H51), C52(H52),
  C54(H54), C55(H55), C58(H58), C59(H59), C61(H61), C62(H62)
4.c Idealised Me refined as rotating group:
 C56A(H56A,H56B,H56C), C63A(H63A,H63B,H63C), C56(H56D,H56E,H56F), C63(H63D,
 H63E,H63F)
;
_shelx_res_checksum              16075
_shelx_hkl_checksum              41661