Osmium Phosphiniminato Complexes: Synthesis, Protonation, Structure, and Redox-Coupled Hydrolytic Scission of N-P Bonds
Brian K. Bennett; Erik Saganic; Scott Lovell; Werner Kaminsky; Amanda Samuel; James M. Mayer; Inorganic Chemistry 42 (2003) 4127–4134; doi:10.1021/ic026260u

data_4313806
_publ_contact_author
;
       Mayer, James M.
    Department of Chemistry, BOX 351700
    University of Washington
    Seattle, WA 98195
    USA
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_publ_contact_author_email       mayer@chem.washington.edu
_publ_section_title
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 Osmium Phosphiniminato Complexes: Synthesis, Protonation, Structure, and
 Redox-Coupled Hydrolytic Scission of N-P Bonds
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4127
_journal_page_last               4134
_journal_paper_doi               10.1021/ic026260u
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C27 H25 B Cl2 N7 Os P'
_chemical_formula_sum            'C27 H25 B Cl2 N7 Os P'
_chemical_formula_weight         750.42
_chemical_name_common            'ESI99 data2'
_chemical_name_systematic        'ESI99 data2'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.5000(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6640(3)
_cell_length_b                   15.3050(6)
_cell_length_c                   21.7270(10)
_cell_measurement_reflns_used    1013
_cell_measurement_temperature    130(2)
_cell_volume                     2747.71(19)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11017
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    4.926
_exptl_absorpt_correction_T_max  0.7979
_exptl_absorpt_correction_T_min  0.3844
_exptl_absorpt_correction_type   HKL-2000
_exptl_absorpt_process_details   'numerical, using redundancy'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.297
_refine_diff_density_min         -2.038
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0934
_reflns_number_gt                4339
_reflns_number_total             6326
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026260u_1.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
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The following automatic conversions were performed:
data name '_publ_contact_email' replaced with
'_publ_contact_author_email' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
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_cod_database_code               4313806