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_4313807
_publ_contact_author
;
       Mayer, James M.
    Department of Chemistry, BOX 351700
    University of Washington
    Seattle, WA 98195
    USA
;
_publ_contact_author_email       mayer@chem.washington.edu
_publ_section_title
;
 Osmium Phosphiniminato Complexes: Synthesis, Protonation, Structure, and
 Redox-Coupled Hydrolytic Scission of N-P Bonds
;
_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 H26 B Cl1 N7 Os P+ OTf-'
_chemical_formula_sum            'C28 H26 B Cl F3 N7 O3 Os P S'
_chemical_formula_weight         900.50
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.467(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0427(8)
_cell_length_b                   9.8788(2)
_cell_length_c                   19.5069(8)
_cell_measurement_reflns_used    625
_cell_measurement_temperature    161(2)
_cell_volume                     3351.0(2)
_computing_cell_refinement       'HKL SCALEPACK'
_computing_data_collection       KappaCCD
_computing_data_reduction        DENZO
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      161(2)
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f rotation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_av_sigmaI/netI    0.0947
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            164702
_diffrn_reflns_theta_full        30.48
_diffrn_reflns_theta_max         30.48
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    4.134
_exptl_absorpt_correction_T_max  0.8860
_exptl_absorpt_correction_T_min  0.4632
_exptl_absorpt_correction_type   SCALEPACK
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.900
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         9614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0471P)^2^+5.6844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                6576
_reflns_number_total             9614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026260u_2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+5.6844P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+5.6844P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

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 
;
_cod_original_formula_sum        'C28 H26 B Cl1 F3 N7 O3 Os P S'
_cod_database_code               4313807