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_4313808
_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_sum            'C27 H26 B Cl2 N7 Os P'
_chemical_formula_weight         751.43
_chemical_name_common            BB-III-O4
_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                 96.9000(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7560(4)
_cell_length_b                   15.1720(4)
_cell_length_c                   20.9130(11)
_cell_measurement_reflns_used    366
_cell_measurement_temperature    130(2)
_cell_volume                     2758.1(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    SIR92
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.840
_diffrn_measured_fraction_theta_max 0.840
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_sigmaI/netI    0.1229
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11165
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    4.907
_exptl_absorpt_correction_T_max  0.6502
_exptl_absorpt_correction_T_min  0.5384
_exptl_absorpt_correction_type   HKL-SCALEPACK
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.698
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.187
_refine_ls_extinction_coef       0.00010(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                3855
_reflns_number_total             5974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026260u_3.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] 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^)+(0.0000P)^2^+0.0000P] 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_database_code               4313808