Cubic and Spirocyclic Radicals Containing a Tetraimidophosphate Dianion [P(NR)3(NR')].2-
Andrea F. Armstrong; Tristram Chivers; Heikki M. Tuononen; Masood Parvez; René T. Boeré; Inorganic Chemistry 44 (2005) 7981–7991; doi:10.1021/ic051128q

data_4309899
_publ_contact_author_address
; Department of Chemistry
  University of Calgary
  Calgary Alberta T2N 1N4
  Canada
;
_publ_contact_author_email       chivers@ucalgary.ca
_publ_contact_author_fax         '001 403 289 9488'
_publ_contact_author_name        'Dr Tristram Chivers'
_publ_contact_author_phone       '001 403 220 5741'
_publ_section_title
;
Cubic and Spirocyclic Radicals Containing a Tetraimidophosphate Dianion
[P(NR)3(NR')].2-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7981
_journal_page_last               7991
_journal_paper_doi               10.1021/ic051128q
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C21 H45 N4 P Si'
_chemical_formula_weight         412.67
_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                 101.7596(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.5001(3)
_cell_length_b                   22.8914(7)
_cell_length_c                   20.9785(5)
_cell_measurement_temperature    173(2)
_cell_volume                     4936.6(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_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  0.0922
_diffrn_reflns_av_sigmaI/netI    0.0994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32448
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.9812
_exptl_absorpt_correction_T_min  0.9580
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         10914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0634
_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^)+(0.0817P)^2^+3.5889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1864
_reflns_number_gt                6417
_reflns_number_total             10914
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051128qsi20050707_121411.cif
_cod_data_source_block           compound1b
_cod_database_code               4309899