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_4347339
_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_compound_source        'dichloromethane, hexane'
_chemical_formula_moiety         'C50 H38 Br2 N O Os P2, 2(C H2 Cl2)'
_chemical_formula_sum            'C52 H42 Br2 Cl4 N O Os P2'
_chemical_formula_weight         1250.62
_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_block_code                FNG-PG-510-10
_audit_creation_date             2013-08-21
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 96.676(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.080(2)
_cell_length_b                   18.586(3)
_cell_length_c                   21.058(4)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9666
_cell_measurement_theta_min      2.3982
_cell_volume                     4695.9(14)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            138827
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.077
_diffrn_reflns_theta_min         1.466
_exptl_absorpt_coefficient_mu    4.754
_exptl_absorpt_correction_T_max  0.78031
_exptl_absorpt_correction_T_min  0.40363
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2452
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.275
_refine_diff_density_min         -2.266
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         15033
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0346P)^2^+16.9413P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13038
_reflns_number_total             15033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347339
_shelx_estimated_absorpt_t_min   0.517
_shelx_estimated_absorpt_t_max   0.833
_shelxl_version_number           2013-2
_shelx_res_checksum              33623
_shelx_hkl_checksum              11751