Preparation of the Octahedral d6Amido Complex TpRu(CO)(PPh3)(NHPh) (Tp = Hydridotris(pyrazolyl)borate): Solid-State Structural Characterization and Reactivity
K. N. Jayaprakash; T. Brent Gunnoe; Paul D. Boyle; Inorganic Chemistry 40 (2001) 6481–6486; doi:10.1021/ic010785p

data_4320676
_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
;
 Preparation of the Octahedral d6Amido Complex TpRu(CO)(PPh3)(NHPh) (Tp =
 Hydridotris(pyrazolyl)borate): Solid-State Structural Characterization
 and Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6481
_journal_page_last               6486
_journal_paper_doi               10.1021/ic010785p
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C44.50 H43 B N7 O P Ru '
_chemical_formula_sum            'C44.5 H43 B N7 O P Ru'
_chemical_formula_weight         834.72
_chemical_name_systematic
;
(hydridotris(pyrazolyl)borate)(triphenylphosphine)
(carbonmonoxide)ruthenium(II) phenylamido
;
_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                 99.292(15)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   12.0038(14)
_cell_length_b                   22.169(2)
_cell_length_c                   14.9766(19)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    148
_cell_measurement_theta_max      18.00
_cell_measurement_theta_min      16.50
_cell_volume                     3933.2(8)
_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       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6880
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.20
_diffrn_standards_decay_%        1.3
_diffrn_standards_interval_time  80
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .48
_exptl_absorpt_correction_T_max  .9996
_exptl_absorpt_correction_T_min  .8950
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'NRCVAX ABSORP'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       prism
_exptl_crystal_F_000             1720.21
_exptl_crystal_size_max          .38
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .30
_refine_diff_density_max         .67
_refine_diff_density_min         -.55
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.40
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         5452
_refine_ls_R_factor_all          .037
_refine_ls_R_factor_obs          .037
_refine_ls_shift/esd_max         .000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     '1/(\s^2^(F)+ .0003F^2^) '
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .039
_refine_ls_wR_factor_obs         .039
_reflns_number_observed          5459
_reflns_number_total             6880
_reflns_observed_criterion       'Inet > 1.0\s(Inet)'
_cod_data_source_file            ic010785p.cif
_cod_data_source_block           3
_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        'C44.50 H43 B N7 O P Ru '
_cod_database_code               4320676