A step closer to the binary: the [Bi6I20](2-) anion.
Heine, Johanna; Dalton transactions (Cambridge, England : 2003) 44 (2015) 10069–10077; doi:10.1039/c5dt00813a

data_7034887
_publ_section_title
;
 A step closer to the binary: the [Bi6I20](2-) anion.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10069
_journal_page_last               10077
_journal_paper_doi               10.1039/c5dt00813a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'Bi3 I11, C44 H54 K2 N2 O12, C2 H3 N'
_chemical_formula_sum            'C46 H57 Bi3 I11 K2 N3 O12'
_chemical_formula_weight         2944.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-02 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.905(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4954(11)
_cell_length_b                   16.2145(6)
_cell_length_c                   23.3300(13)
_cell_measurement_reflns_used    4827
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      1.69
_cell_volume                     7365.3(6)
_computing_data_collection       'STOE X-AREA'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Stoe IPDS-II'
_diffrn_measurement_method       'area detetor, \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2233
_diffrn_reflns_av_unetI/netI     0.1311
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            79147
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.853
_diffrn_reflns_theta_min         1.328
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    11.923
_exptl_absorpt_correction_T_max  0.5364
_exptl_absorpt_correction_T_min  0.0857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.656
_exptl_crystal_description       block
_exptl_crystal_F_000             5280
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.126
_refine_diff_density_min         -2.195
_refine_diff_density_rms         0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         15628
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0637P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9570
_reflns_number_total             15628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00813a2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7034884--7034887.cif.'
_cod_database_code               7034887
_shelx_estimated_absorpt_t_max   0.199
_shelx_estimated_absorpt_t_min   0.099
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 K2-C28 = K2-C29 = K2-C39 = K1-C10 = K1-C1 = K1-C11
 -3.65 with sigma of 0.02
 K1-C20 = K2-C38
 -3.65 with sigma of 0.02
 K2-C39
 -3.65 with sigma of 0.02
 K2-C28
 -3.65 with sigma of 0.02
 K2-C30
 -3.65 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C22 \\sim C21: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C20 \\sim C19: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C28 \\sim C27: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C9 \\sim C10: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C11 \\sim C12: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C38(H38A,H38B), C30(H30A,H30B), C29(H29A,H29B), C9(H9A,H9B),
 C40(H40A,H40B), C37(H37A,H37B), C27(H27A,H27B), C19(H19A,H19B), C39(H39A,H39B),
  C12(H12A,H12B), C20(H20A,H20B), C11(H11A,H11B), C1(H1A,H1B), C10(H10A,H10B),
 C28(H28A,H28B)
4.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C16(H16), C18(H18), C33(H33), C17(H17), C15(H15), C34(H34), C5(H5),
 C26(H26), C25(H25), C35(H35), C23(H23), C6(H6), C24(H24), C7(H7), C8(H8)
4.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C42(H42A,H42B,H42C), C46(H46A,H46B,H46C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'