Tris(<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylguanidinium) nonabromodiantimonate(III)
Bujak, Maciej; Zaleski, Jacek; Acta Crystallographica Section E 63 (2007) m102–m104; doi:10.1107/S1600536806051920

data_2211831
_publ_section_title
;
 Tris(<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylguanidinium)
 nonabromodiantimonate(III)
;
_journal_coeditor_code           HB2224
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m102
_journal_page_last               m104
_journal_paper_doi               10.1107/S1600536806051920
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C5 H14 N3)3 [Sb2 Br9]'
_chemical_formula_moiety         '3(C5 H14 N3 +), Br9 Sb2 3-'
_chemical_formula_sum            'C15 H42 Br9 N9 Sb2'
_chemical_formula_weight         1311.27
_chemical_name_systematic
;
Tris(N,N,N',N'-tetramethylguanidinium) nonabromodiantimonate(III)
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.064(5)
_cell_angle_beta                 88.199(4)
_cell_angle_gamma                85.024(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9824(5)
_cell_length_b                   12.1782(7)
_cell_length_c                   15.0405(8)
_cell_measurement_reflns_used    5556
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.34
_cell_volume                     1895.56(18)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2004)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2001)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur CCD'
_diffrn_measurement_method       \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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_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            11715
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.932
_exptl_absorpt_correction_T_max  0.194
_exptl_absorpt_correction_T_min  0.088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(XPREP in SHELXTL; Sheldrick, 1990'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.297
_exptl_crystal_density_meas      2.30(2)
_exptl_crystal_density_method    'flotation in CCl~4~/CHBr~3~'
_exptl_crystal_description       pillar
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.710
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         6607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0249P)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0665
_reflns_number_gt                4616
_reflns_number_total             6607
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2224.cif
_cod_data_source_block           I
_cod_original_cell_volume        1895.56(17)
_cod_database_code               2211831
_cod_database_fobs_code          2211831