[(Ph)3PBr][Br7], [(Bz)(Ph)3P]2[Br8], [(n-Bu)3MeN]2[Br20], [C4MPyr]2[Br20], and [(Ph)3PCl]2[Cl2I14]: Extending the Horizon of Polyhalides via Synthesis in Ionic Liquids
Michael Wolff; Alexander Okrut; Claus Feldmann; Inorganic Chemistry 50 (2011) 11683–11694; doi:10.1021/ic201291k

data_4326848
_publ_contact_author_address
'Inst. fuer Anorg. Chemie, KIT, Engesserstr. 15, D-76131 Karlsruhe, Germany'
_publ_contact_author_email       claus.feldmann@kit.edu
_publ_contact_author_name        'Claus Feldmann'
_publ_contact_author_phone       +49-721-608-2855
_publ_section_title
;
 [(Ph)3PBr][Br7], [(Bz)(Ph)3P]2[Br8], [(n-Bu)3MeN]2[Br20],
 [C4MPyr]2[Br20], and [(Ph)3PCl]2[Cl2I14]: Extending the Horizon of
 Polyhalides via Synthesis in Ionic Liquids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11683
_journal_page_last               11694
_journal_paper_doi               10.1021/ic201291k
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C13 H30 Br10 N'
_chemical_formula_weight         999.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 96.67(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.340(3)
_cell_length_b                   10.242(2)
_cell_length_c                   33.154(7)
_cell_measurement_reflns_used    3771
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      1.85
_cell_volume                     5510.9(19)
_computing_cell_refinement       'CELL, SELECT (STOE)'
_computing_data_collection       'EXPOSE (STOE)'
_computing_data_reduction        'INTEGRATE (STOE)'
_computing_molecular_graphics    'DIAMOND, Crystal Impact'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5626
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    14.543
_exptl_absorpt_correction_T_max  0.219
_exptl_absorpt_correction_T_min  0.037
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-RED, Data Reduction Program, Version 1.14, Stoe & Cie GmbH, Darmstadt 1999.;
 X-SHAPE, Crystal Optimisation for numerical Absorption Correction, Version 
1.06, Stoe & Cie GmbH, Darmstadt 1999.
;
_exptl_crystal_density_diffrn    2.409
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.1260
_exptl_crystal_size_mid          0.0881
_exptl_crystal_size_min          0.0644
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       0.00011(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   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5626
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0674P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                3771
_reflns_number_total             5626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201291k_si_002.cif
_cod_data_source_block           mw282
_cod_original_cell_volume        5511.3(19)
_cod_database_code               4326848