Formation and distortion of iodidoantimonates(III): the first isolated [SbI~6~]^3{-^} octahedron
Bujak, Maciej; Acta Crystallographica Section B 73 (2017) 432–442; doi:10.1107/S2052520617003420

data_2108107
_publ_section_title
;
 Formation and distortion of iodidoantimonates(III): the first isolated
 [SbI~6~]^3{-^} octahedron
;
_journal_coeditor_code           EB5060
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              432
_journal_page_last               442
_journal_paper_doi               10.1107/S2052520617003420
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         'C4 H12 N2 2+, 2(I -), I2'
_chemical_formula_sum            'C4 H12 I4 N2'
_chemical_formula_weight         595.76
_chemical_name_systematic
;
 Piperazine-1,4-diium diiodide diiodine
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.087(7)
_cell_angle_beta                 67.276(7)
_cell_angle_gamma                69.593(7)
_cell_formula_units_Z            1
_cell_length_a                   6.4948(5)
_cell_length_b                   7.4032(6)
_cell_length_c                   8.0819(5)
_cell_measurement_reflns_used    2137
_cell_measurement_temperature    85.0(5)
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      3.13
_cell_volume                     314.73(5)
_computing_cell_refinement
'CrysAlis Pro ver. 171.34.44 (Oxford Diffraction Ltd., 2010)'
_computing_data_collection
'CrysAlis CCD ver. 171.33.57 (Oxford Diffraction Ltd., 2010)'
_computing_data_reduction
'CrysAlis Pro ver. 171.34.44 (Oxford Diffraction Ltd., 2010)'
_computing_molecular_graphics    'Mercury (C.F.Macrae at al., 2008)'
_computing_publication_material  'SHELXL-97 (G.M.Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (G.M.Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (G.M.Sheldrick, 2008)'
_diffrn_ambient_temperature      85.0(5)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       \w--scan
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2215
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    9.854
_exptl_absorpt_correction_T_max  0.40
_exptl_absorpt_correction_T_min  0.23
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 CrysAlis Pro ver. 171.33.57 (Oxford Diffraction Ltd., 2010)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             262
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.731
_refine_ls_extinction_coef       0.0111(7)
_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   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         1285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0218
_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\^)+(0.0234P)\^2\^+0.0000P] where
 P=(Fo\^2\^+2Fc\^2\^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0540
_reflns_number_gt                1201
_reflns_number_total             1285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            eb5060sup1.cif
_cod_data_source_block           PDD_85K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2108107
_cod_database_fobs_code          2108107