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_4333794
_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            'C22 H33 N4 O3 P'
_chemical_formula_weight         432.49
_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                93.5580(10)
_cell_angle_beta                 94.4570(10)
_cell_angle_gamma                101.4310(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7968(2)
_cell_length_b                   10.6329(3)
_cell_length_c                   12.3025(3)
_cell_measurement_reflns_used    9113
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.07
_cell_measurement_theta_min      2.37
_cell_volume                     1120.95(5)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega'
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32997
_diffrn_reflns_theta_full        30.12
_diffrn_reflns_theta_max         30.12
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_T_max  0.9824
_exptl_absorpt_correction_T_min  0.9517
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         6596
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+0.5538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1281
_reflns_number_gt                5918
_reflns_number_total             6596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301160x_si_002_3.cif
_cod_data_source_block           bjf414
_cod_database_code               4333794