Hemilabile β-Aminophosphine Ligands Derived from 1,3,5-Triaza-7-phosphaadamantane: Application in Aqueous Ruthenium Catalyzed Nitrile Hydration
Wei-Chih Lee; Jeremiah M. Sears; Raphel A. Enow; Kelly Eads; Donald A. Krogstad; Brian J. Frost; Inorganic Chemistry 52 (2013) 1737–1746; doi:10.1021/ic301160x

data_4333796
_publ_contact_author_address
; 
Department of Chemistry
University of Nevada
Reno NV 89557 USA 
;
_publ_contact_author_email       frost@unr.edu
_publ_contact_author_fax         +1-775-784-1993
_publ_contact_author_name        'Brian J. Frost'
_publ_contact_author_phone       +1-775-784-6804
_publ_section_title
;
 Hemilabile \b-Aminophosphine Ligands Derived from
 1,3,5-Triaza-7-phosphaadamantane: Application in Aqueous Ruthenium
 Catalyzed Nitrile Hydration
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1737
_journal_page_last               1746
_journal_paper_doi               10.1021/ic301160x
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C32 H35 Cl F6 N4 P2 Ru'
_chemical_formula_weight         788.10
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 112.9960(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0947(3)
_cell_length_b                   28.9462(7)
_cell_length_c                   11.8438(3)
_cell_measurement_reflns_used    8916
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.05
_cell_measurement_theta_min      2.19
_cell_volume                     3185.77(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            60111
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.9032
_exptl_absorpt_correction_T_min  0.7811
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         9284
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+4.1027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                8647
_reflns_number_total             9284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301160x_si_002_5.cif
_cod_data_source_block           bjf407
_cod_database_code               4333796