Hydrogen bis(tetraphenylimidodiphospinic acid) triiodide
Copolovici, Lucian; Varga, Richard A.; Lippolis, Vito; Silvestru, Cristian; Acta Crystallographica Section E 63 (2007) o4206–o4207; doi:10.1107/S1600536807047198

data_2216053
_publ_section_title
;
 Hydrogen bis(tetraphenylimidodiphospinic acid) triiodide
;
_journal_coeditor_code           LW2032
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4206
_journal_page_last               o4207
_journal_paper_doi               10.1107/S1600536807047198
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C48 H43 N2 O4 P4 +, I3 -'
_chemical_formula_moiety         'C48 H43 N2 O4 P4 +, I3 -'
_chemical_formula_sum            'C48 H43 I3 N2 O4 P4'
_chemical_formula_weight         1216.42
_chemical_name_systematic
;
Hydrogen bis(tetraphenylimidodiphospinic acid) triiodide
;
_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                91.451(2)
_cell_angle_beta                 96.411(2)
_cell_angle_gamma                108.696(2)
_cell_formula_units_Z            1
_cell_length_a                   10.2291(14)
_cell_length_b                   11.3075(15)
_cell_length_c                   11.3840(15)
_cell_measurement_reflns_used    3014
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      21.73
_cell_measurement_theta_min      2.34
_cell_volume                     1236.8(3)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2007)'
_computing_structure_refinement  'SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12050
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    2.068
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELXTL; Bruker, 2001)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.454
_refine_diff_density_min         -0.625
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4347
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+2.0708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                3662
_reflns_number_total             4347
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lw2032.cif
_cod_data_source_block           I
_cod_database_code               2216053
_cod_database_fobs_code          2216053