Influence of Filled dπ-Manifold and L/L' Ligands on the Structure, Basicity, and Bond Rotations of the Octahedral and d6 Amido Complexes TpRu(L)(L')(NHPh) (Tp = Hydridotris(pyrazolyl)borate; L = L' = PMe3or P(OMe)3, or L = CO and L' = PPh3): Solid-State Structures of [TpRu(PMe3)2(NH2Ph)][OTf], [TpRu{P(OMe)3}2(NH2Ph)][OTf], and TpRu{P(OMe)3}2(NHPh)
David Conner; K. N. Jayaprakash; T. Brent Gunnoe; Paul D. Boyle; Inorganic Chemistry 41 (2002) 3042–3049; doi:10.1021/ic020163j

data_4318047
_publ_contact_author_address
;
North Carolina State University
Department of Chemistry
Campus Box 8204
Raleigh, NC 27695-8204
;
_publ_contact_author_email       brent_gunnoe@ncsu.edu
_publ_contact_author_fax         '1 (919) 5158909'
_publ_contact_author_name        'T. Brent Gunnoe'
_publ_contact_author_phone       '1 (919) 5133704'
_publ_section_title
;
 Influence of Filled d\p-Manifold and L/L' Ligands on the Structure,
 Basicity, and Bond Rotations of the Octahedral and d6 Amido Complexes
 TpRu(L)(L')(NHPh) (Tp = Hydridotris(pyrazolyl)borate; L = L' = PMe3or
 P(OMe)3, or L = CO and L' = PPh3): Solid-State Structures of
 [TpRu(PMe3)2(NH2Ph)][OTf], [TpRu{P(OMe)3}2(NH2Ph)][OTf], and
 TpRu{P(OMe)3}2(NHPh)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3042
_journal_page_last               3049
_journal_paper_doi               10.1021/ic020163j
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C22 H35 B F3 N7 O9 P2 Ru S '
_chemical_formula_sum            'C22 H35 B F3 N7 O9 P2 Ru S'
_chemical_formula_weight         804.43
_chemical_name_systematic
;
[TpRu{P(OMe)3}2NH2Ph][OTf] (5).
;
_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'
_cell_angle_alpha                90.0
_cell_angle_beta                 92.307(5)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   9.1753(6)
_cell_length_b                   23.7851(18)
_cell_length_c                   15.3015(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    148
_cell_measurement_theta_max      18.00
_cell_measurement_theta_min      17.00
_cell_volume                     3336.6(4)
_computing_cell_refinement       'Nonius CAD4 Argus'
_computing_data_collection       'Nonius CAD4 Argus'
_computing_data_reduction        'NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      148
_diffrn_measurement_device       'Nonius CAD-4    '
_diffrn_measurement_method       'Omega scan b/P/b        '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5817
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.20
_diffrn_standards_decay_%        3.8
_diffrn_standards_interval_time  80
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .70
_exptl_absorpt_correction_T_max  .9960
_exptl_absorpt_correction_T_min  .8771
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'NRCVAX ABSORP'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       prism
_exptl_crystal_F_000             1637.37
_exptl_crystal_size_max          .32
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .14
_refine_diff_density_max         .43
_refine_diff_density_min         -.77
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.61
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         5025
_refine_ls_R_factor_all          .025
_refine_ls_R_factor_obs          .025
_refine_ls_shift/esd_max         .002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     '1/(\s^2^(F)+ .0002F^2^) '
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .030
_refine_ls_wR_factor_obs         .030
_reflns_number_observed          5028
_reflns_number_total             5817
_reflns_observed_criterion       'Inet > 1.0\s(Inet)'
_cod_data_source_file            ic020163j_3.cif
_cod_data_source_block           5
_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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C22 H35 B F3 N7 O9 P2 Ru S '
_cod_database_code               4318047