Intramolecular Hydrogen-Bonded Tertiary Phosphines as 1,3,5-Triaza-7-phosphaadamantane (PTA) Analogues
Allen T. Ekubo; Mark R. J. Elsegood; Andrew J. Lake; Martin B. Smith; Inorganic Chemistry 48 (2009) 2633–2638; doi:10.1021/ic801709z

data_4301662
_publ_section_title
;
Intramolecular Hydrogen-Bonded Tertiary Phosphines as
1,3,5-Triaza-7-phosphaadamantane (PTA) Analogues
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2633
_journal_page_last               2638
_journal_paper_doi               10.1021/ic801709z
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
'C35 H46 Cl2 N3 P Rh 1+, Sb F6 1-, 2(C H2 Cl2)'
_chemical_formula_sum            'C37 H50 Cl6 F6 N3 P Rh Sb'
_chemical_formula_weight         1119.13
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.887(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9106(3)
_cell_length_b                   14.7367(4)
_cell_length_c                   30.8857(9)
_cell_measurement_reflns_used    104486
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     4034.3(2)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type
'Bruker-Nonius Roper 2 CCD camera on \k-goniost'
_diffrn_measurement_method       '\f & \w 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  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            47660
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.578
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2007/2, Sheldrick, G.M., (2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         1.389
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.0028(3)
_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   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         9116
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+28.2608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1891
_refine_ls_wR_factor_ref         0.2031
_reflns_number_gt                6545
_reflns_number_total             9116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801709z_si_002_5.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4301662