Radical and Non-Radical States of the [Os(PIQ)] Core (PIQ = 9,10-Phenanthreneiminoquinone): Iminosemiquinone to Iminoquinone Conversion Promoted o-Metalation Reaction.
Bera, Sachinath; Mondal, Sandip; Maity, Suvendu; Weyhermüller, Thomas; Ghosh, Prasanta; Inorganic chemistry 55 (2016) 4746–4756; doi:10.1021/acs.inorgchem.6b00040

data_4347340
_publ_section_title
;
 Radical and Non-Radical States of the [Os(PIQ)] Core (PIQ =
 9,10-Phenanthreneiminoquinone): Iminosemiquinone to Iminoquinone
 Conversion Promoted o-Metalation Reaction.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4746
_journal_page_last               4756
_journal_paper_doi               10.1021/acs.inorgchem.6b00040
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C52 H41 Br3 Cl4 N O Os P2'
_chemical_formula_weight         1329.53
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 118.1180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.3136(11)
_cell_length_b                   9.5495(4)
_cell_length_c                   23.6568(10)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    114(2)
_cell_measurement_theta_max      28.55
_cell_measurement_theta_min      2.89
_cell_volume                     4844.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      114(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35971
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.569
_diffrn_reflns_theta_min         2.586
_diffrn_source                   Mo
_exptl_absorpt_coefficient_mu    5.434
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2588
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.190
_exptl_transmission_factor_max   0.348
_exptl_transmission_factor_min   0.225
_refine_diff_density_max         2.679
_refine_diff_density_min         -2.062
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         12263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0079P)^2^+57.1861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11073
_reflns_number_total             12263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            4.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347340
_shelx_estimated_absorpt_t_min   0.115
_shelx_estimated_absorpt_t_max   0.425
_shelxl_version_number           2014/6
_shelx_res_checksum              14221
_shelx_hkl_checksum              57550