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_7034886
_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         'Bi6 I20, 2(C24 H30 N2 Na O6), 3(C2 H3 N)'
_chemical_formula_sum            'C54 H69 Bi6 I20 N7 Na2 O12'
_chemical_formula_weight         4846.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2015-03-30
_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                96.034(5)
_cell_angle_beta                 100.883(5)
_cell_angle_gamma                102.490(5)
_cell_formula_units_Z            2
_cell_length_a                   14.372(3)
_cell_length_b                   19.388(3)
_cell_length_c                   19.648(4)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.319
_cell_volume                     5187.9(17)
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            103600
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.437
_diffrn_reflns_theta_min         2.321
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    16.146
_exptl_absorpt_correction_T_max  0.745196
_exptl_absorpt_correction_T_min  0.394403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1709 before and 0.0511 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1704 before and 0.0577 after correction.
 The Ratio of minimum to maximum transmission is 0.53.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 103600 reflections, Rint = 0.0566
 (61448 with I > 3sig(I), Rint = 0.0469)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.102
_exptl_crystal_description       block
_exptl_crystal_F_000             4236
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.132
_refine_diff_density_max         3.734
_refine_diff_density_min         -1.763
_refine_diff_density_rms         0.371
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         18828
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+220.5093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1205
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15244
_reflns_number_total             18828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00813a2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7034884--7034887.cif.'
_cod_original_cell_volume        5187.9(16)
_cod_database_code               7034886
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6323(9) 0.3677(9)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C29) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C21(H21A,H21B), C32(H32A,H32B), C31(H31A,H31B), C13(H13A,
 H13B), C22(H22A,H22B), C24(H24A,H24B), C11(H11A,H11B), C12(H12A,H12B), C4(H4A,
 H4B), C23(H23A,H23B), C33(H33A,H33B), C14(H14A,H14B), C2(H2A,H2B), C3(H3A,H3B),
  C1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C39(H39), C27(H27), C37(H37), C17(H17), C29(H29), C26(H26),
 C18(H18), C16(H16), C6(H6), C36(H36), C8(H8), C9(H9), C28(H28), C38(H38),
 C7(H7)
4.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C42(H42A,H42B,
 H42C), C54(H54A,H54B,H54C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'