Protonation and Deprotonation of TpOs(NHPh)Cl2: An Unusually Inert Amido Ligand
Jake D. Soper; Brian K. Bennett; Scott Lovell; James M. Mayer; Inorganic Chemistry 40 (2001) 1888–1893; doi:10.1021/ic001177x

data_4319511
_publ_contact_author
;
    J. M. Mayer
    Department of Chemistry
    University of Washington
    Seattle, WA 98195
    USA
;
_publ_contact_author_email       mayer@chem.washington.edu
_publ_section_title
;
 Protonation and Deprotonation of TpOs(NHPh)Cl2: An Unusually Inert Amido
 Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1888
_journal_page_last               1893
_journal_paper_doi               10.1021/ic001177x
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C17 H16 B F6 N7 O6 Os S2'
_chemical_formula_sum            'C17 H16 B F6 N7 O6 Os S2'
_chemical_formula_weight         793.50
_chemical_name_common            TpOs(NHPh)(OTf)2
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.580(8)
_cell_angle_beta                 90.034(8)
_cell_angle_gamma                70.000(7)
_cell_formula_units_Z            2
_cell_length_a                   9.491(1)
_cell_length_b                   11.604(2)
_cell_length_c                   13.231(2)
_cell_measurement_reflns_used    189
_cell_measurement_temperature    161(2)
_cell_volume                     1305.8(3)
_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      161(2)
_diffrn_measured_fraction_theta_full 0.726
_diffrn_measured_fraction_theta_max 0.726
_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  0.1005
_diffrn_reflns_av_sigmaI/netI    0.2080
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8409
_diffrn_reflns_theta_full        29.93
_diffrn_reflns_theta_max         29.93
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    5.139
_exptl_absorpt_correction_T_max  0.8208
_exptl_absorpt_correction_T_min  0.5775
_exptl_absorpt_correction_type   HKL-Scalepack
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.020
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.544
_refine_diff_density_min         -2.175
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       0.0033(5)
_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   0.874
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.1388
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                2887
_reflns_number_total             5489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001177x.cif
_cod_data_source_block           TpOs(NHPh)(OTf)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_database_code               4319511