[Bi<sub>6</sub>Mo<sub>3</sub>(CO)<sub>9</sub>]<sup>4-</sup>: a multiple local σ-aromatic cluster containing a distorted Bi<sub>6</sub> triangular prism.
Qiao, Lei; Chen, Dandan; Zhu, Jun; Muñoz-Castro, Alvaro; Sun, Zhong-Ming; Chemical communications (Cambridge, England) 57 (2021) 3656–3659; doi:10.1039/d1cc00734c

data_7128008
_publ_section_title
;
 [Bi<sub>6</sub>Mo<sub>3</sub>(CO)<sub>9</sub>]<sup>4-</sup>: a multiple
 local \s-aromatic cluster containing a distorted Bi<sub>6</sub>
 triangular prism.
;
_journal_issue                   30
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3656
_journal_page_last               3659
_journal_paper_doi               10.1039/d1cc00734c
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'Bi6 C9 Mo3 O9, 2(C18 H36 K N2 O6), C18 H35.045 K N2 O6, C17 H33.46 K N2 O5'
_chemical_formula_sum            'C81 H144.01 Bi6 K4 Mo3 N8 O33'
_chemical_formula_weight         3456.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-01-06
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-01-11 deposited with the CCDC.	2021-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                76.0792(11)
_cell_angle_beta                 77.6588(10)
_cell_angle_gamma                62.9932(15)
_cell_formula_units_Z            2
_cell_length_a                   15.0576(2)
_cell_length_b                   16.1907(3)
_cell_length_c                   30.1290(3)
_cell_measurement_reflns_used    34028
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.6290
_cell_measurement_theta_min      3.9480
_cell_volume                     6305.52(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.3-beta (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3-beta (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -47.00  -3.50   0.50    0.50    --    0.00 -77.00  90.00   87
  2  \w    -89.00 -25.00   0.50    0.50    --    0.00 -38.00 -60.00  128
  3  \w     -6.00  39.50   0.50    0.50    --    0.00  82.00  60.00   91
  4  \w    -32.00  33.50   0.50    0.50    --    0.00 -82.00 -60.00  131
  5  \w    -34.00   3.50   0.50    0.50    --    0.00  82.00 120.00   75
  6  \w     -3.00  24.50   0.50    0.50    --    0.00 -82.00   0.00   55
  7  \w    -39.00  -7.50   0.50    0.50    --    0.00 -82.00  60.00   63
  8  \w    -31.00  32.50   0.50    0.50    --    0.00 -82.00-180.00  127
  9  \w    -16.00  22.00   0.50    0.50    --    0.00 -38.00 -60.00   76
 10  \w     13.00 124.50   0.50    2.00    --  101.30 -57.00 120.00  223
 11  \w     89.00 115.00   0.50    2.00    --  101.30 -57.00 -90.00   52
 12  \w     12.00  71.50   0.50    2.00    --  101.30 -57.00 -90.00  119
 13  \w     14.00 125.00   0.50    2.00    --  101.30 -38.00 -90.00  222
 14  \w     60.00 103.50   0.50    2.00    --  101.30 -82.00 -90.00   87
 15  \w     82.00 109.50   0.50    2.00    --  101.30 -82.00  60.00   55
 16  \w     23.00  76.50   0.50    2.00    --  101.30 -82.00  60.00  107
 17  \w     27.00 133.00   0.50    2.00    --  101.30 -82.00 120.00  212
 18  \w     21.00 108.50   0.50    2.00    --  101.30 -38.00 120.00  175
 19  \w     96.00 136.00   0.50    2.00    --  101.30 -82.00-180.00   80
 20  \w     34.00 128.00   0.50    2.00    --  101.30 -82.00 -30.00  188
 21  \w     78.00 157.50   0.50    2.00    --  101.30  38.00  90.00  159
 22  \w     47.00 109.00   0.50    2.00    --  101.30 -82.00  30.00  124
 23  \w     69.00 177.00   0.50    2.00    --  101.30  19.00  60.00  216
 24  \w     16.00  41.50   0.50    2.00    --  101.30 -82.00 -90.00   51
 25  \w     82.00 107.50   0.50    2.00    --  101.30 -82.00-150.00   51
 26  \w    117.00 142.50   0.50    2.00    --  101.30  77.00 -60.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0051566000
_diffrn_orient_matrix_UB_12      -0.0952040000
_diffrn_orient_matrix_UB_13      0.0188637000
_diffrn_orient_matrix_UB_21      -0.0819230000
_diffrn_orient_matrix_UB_22      0.0275129000
_diffrn_orient_matrix_UB_23      -0.0308108000
_diffrn_orient_matrix_UB_31      0.0815116000
_diffrn_orient_matrix_UB_32      -0.0436306000
_diffrn_orient_matrix_UB_33      -0.0388726000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            61639
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.998
_diffrn_reflns_theta_min         3.976
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    20.173
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       block
_exptl_crystal_F_000             3300
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         7.002
_refine_diff_density_min         -5.144
_refine_diff_density_rms         0.435
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1327
_refine_ls_number_reflns         22367
_refine_ls_number_restraints     7370
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0927
_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^)+(0.1612P)^2^+209.6449P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2488
_refine_ls_wR_factor_ref         0.2556
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19401
_reflns_number_total             22367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00734c2.cif
_cod_data_source_block           complex_1
_cod_depositor_comments
'Adding full bibliography for 7128008--7128009.cif.'
_cod_original_cell_volume        6305.52(17)
_cod_database_code               7128008
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 N7-C37 = N7-C48 = N7-C49 = N8-C43 = N8-C54
 1.49 with sigma of 0.01
 N7'-C37' = N7'-C48' = N7'-C49 = N8'-C43' = N8'-C54'
 1.49 with sigma of 0.01
 C37-C38 = C39-C40 = C41-C42 = C53-C54 = C51-C52
 1.54 with sigma of 0.01
 C37'-C38' = C39-C40' = C41'-C42 = C53'-C54' = C51'-C52
 1.54 with sigma of 0.01
 C49-C50
 1.54 with sigma of 0.01
 O13-C50 = O13-C51 = O14-C52 = O14-C53
 1.43 with sigma of 0.01
 O13-C51' = O14'-C52 = O14'-C53'
 1.43 with sigma of 0.01
 O18-C44 = O18-C45 = O17-C46 = O17-C47
 1.43 with sigma of 0.01
 O18'-C44' = O17'-C46' = O17'-C47
 1.43 with sigma of 0.01
 O15-C40 = O15-C41
 1.43 with sigma of 0.01
 O15'-C40' = O15'-C41'
 1.43 with sigma of 0.01
 N7-C49
 1.49 with sigma of 0.01
 N8-C43
 1.49 with sigma of 0.01
 C44-C43
 1.54 with sigma of 0.01
 O18'-C45
 1.43 with sigma of 0.01
 C55'-N5' = C66'-N5' = C65'-N5' = C60'-N6
 1.49 with sigma of 0.01
 C55-N5 = C66-N5 = C67-N5 = C60-N6 = C61-N6 = C72-N6
 1.49 with sigma of 0.01
 C69-C70 = C67-C68 = C69'-C70' = C67'-C68'
 1.54 with sigma of 0.01
 C55'-C56' = C59-C60' = C63-C64' = C65'-C66' = C71'-C72
 1.54 with sigma of 0.01
 C55-C56 = C59-C60 = C61-C62 = C63-C64 = C65-C66 = C71-C72
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 3.8A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(K3) = Uanis(K3')
Uanis(K4) = Uanis(K4')
Uanis(O14) = Uanis(O14')
Uanis(O15) = Uanis(O15')
Uanis(O17) = Uanis(O17')
Uanis(O18) = Uanis(O18')
Uanis(O20) = Uanis(O20')
Uanis(O21) = Uanis(O21')
Uanis(O22) = Uanis(O22')
Uanis(O28) = Uanis(O28')
Uanis(O30) = Uanis(O30')
Uanis(N5) = Uanis(N5')
Uanis(N7) = Uanis(N7')
Uanis(N8) = Uanis(N8')
Uanis(C37) = Uanis(C37')
Uanis(C38) = Uanis(C38')
Uanis(C40) = Uanis(C40')
Uanis(C41) = Uanis(C41')
Uanis(C43) = Uanis(C43')
Uanis(C44) = Uanis(C44')
Uanis(C46) = Uanis(C46')
Uanis(C48) = Uanis(C48')
Uanis(C51) = Uanis(C51')
Uanis(C53) = Uanis(C53')
Uanis(C54) = Uanis(C54')
Uanis(C55) = Uanis(C55')
Uanis(C56) = Uanis(C56')
Uanis(C60) = Uanis(C60')
Uanis(C64) = Uanis(C64')
Uanis(C65) = Uanis(C65')
Uanis(C66) = Uanis(C66')
Uanis(C67) = Uanis(C67')
Uanis(C68) = Uanis(C68')
Uanis(C69) = Uanis(C69')
Uanis(C70) = Uanis(C70')
Uanis(C71) = Uanis(C71')
4. Others
 Sof(K3')=Sof(O14')=Sof(O15')=Sof(O17')=Sof(O18')=Sof(N7')=Sof(N8')=Sof(C37')=
 Sof(H37c)=Sof(H37d)=Sof(C38')=Sof(H38c)=Sof(H38d)=Sof(H39c)=Sof(H39d)=
 Sof(C40')=Sof(H40c)=Sof(H40d)=Sof(C41')=Sof(H41c)=Sof(H41d)=Sof(H42c)=
 Sof(H42d)=Sof(C43')=Sof(H43a)=Sof(H43b)=Sof(C44')=Sof(H44c)=Sof(H44d)=
 Sof(H45c)=Sof(H45d)=Sof(C46')=Sof(H46c)=Sof(H46d)=Sof(H47c)=Sof(H47d)=
 Sof(C48')=Sof(H48c)=Sof(H48d)=Sof(H49c)=Sof(H49d)=Sof(C51')=Sof(H51c)=
 Sof(H51d)=Sof(H52c)=Sof(H52d)=Sof(C53')=Sof(H53c)=Sof(H53d)=Sof(C54')=
 Sof(H54c)=Sof(H54d)=1-FVAR(1)
 Sof(K3)=Sof(O14)=Sof(O15)=Sof(O17)=Sof(O18)=Sof(N7)=Sof(N8)=Sof(C37)=
 Sof(H37a)=Sof(H37b)=Sof(C38)=Sof(H38a)=Sof(H38b)=Sof(H39a)=Sof(H39b)=Sof(C40)=
 Sof(H40a)=Sof(H40b)=Sof(C41)=Sof(H41a)=Sof(H41b)=Sof(H42a)=Sof(H42b)=Sof(C43)=
 Sof(C44)=Sof(H44a)=Sof(H44b)=Sof(H45a)=Sof(H45b)=Sof(C46)=Sof(H46a)=Sof(H46b)=
 Sof(H47a)=Sof(H47b)=Sof(C48)=Sof(H48a)=Sof(H48b)=Sof(H49a)=Sof(H49b)=Sof(C51)=
 Sof(H51a)=Sof(H51b)=Sof(H52a)=Sof(H52b)=Sof(C53)=Sof(H53a)=Sof(H53b)=Sof(C54)=
 Sof(H54a)=Sof(H54b)=FVAR(1)
 Sof(K4')=Sof(O20')=Sof(O21')=Sof(O22')=Sof(N5')=Sof(C55')=Sof(H55c)=Sof(H55d)=
 Sof(C56')=Sof(H56c)=Sof(H56d)=Sof(H59c)=Sof(H59d)=Sof(C60')=Sof(H60c)=
 Sof(H60d)=Sof(H62c)=Sof(H62d)=Sof(H63c)=Sof(H63d)=Sof(C64')=Sof(H64c)=
 Sof(H64d)=Sof(C65')=Sof(H65')=Sof(C66')=Sof(H66c)=Sof(H66d)=Sof(C67')=
 Sof(H67c)=Sof(H67d)=Sof(C68')=Sof(H68c)=Sof(H68d)=Sof(C69')=Sof(H69c)=
 Sof(H69d)=Sof(C70')=Sof(H70c)=Sof(H70d)=Sof(C71')=Sof(H71c)=Sof(H71d)=
 Sof(H72c)=Sof(H72d)=1-FVAR(2)
 Sof(K4)=Sof(O20)=Sof(O21)=Sof(O22)=Sof(N5)=Sof(C55)=Sof(H55a)=Sof(H55b)=
 Sof(C56)=Sof(H56a)=Sof(H56b)=Sof(H59a)=Sof(H59b)=Sof(C60)=Sof(H60a)=Sof(H60b)=
 Sof(H62a)=Sof(H62b)=Sof(H63a)=Sof(H63b)=Sof(C64)=Sof(H64a)=Sof(H64b)=Sof(C65)=
 Sof(H65a)=Sof(H65b)=Sof(C66)=Sof(H66a)=Sof(H66b)=Sof(C67)=Sof(H67a)=Sof(H67b)=
 Sof(C68)=Sof(H68a)=Sof(H68b)=Sof(C69)=Sof(H69a)=Sof(H69b)=Sof(C70)=Sof(H70a)=
 Sof(H70b)=Sof(C71)=Sof(H71a)=Sof(H71b)=Sof(H72a)=Sof(H72b)=FVAR(2)
 Sof(O28')=Sof(O30')=1-FVAR(3)
 Sof(O28)=Sof(O30)=FVAR(3)
 Fixed Sof: O23(0.5) O24(0.5) C57(0.5) H57a(0.5) H57b(0.5) C58(0.5) H58a(0.5)
 H58b(0.5)
5.a Ternary CH refined with riding coordinates:
 C65'(H65')
5.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b),
 C7(H7a,H7b), C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C11(H11a,H11b),
 C12(H12a,H12b), C13(H13a,H13b), C14(H14a,H14b), C15(H15a,H15b), C16(H16a,H16b),
  C17(H17a,H17b), C18(H18a,H18b), C19(H19a,H19b), C20(H20a,H20b), C21(H21a,
 H21b), C22(H22a,H22b), C23(H23a,H23b), C24(H24a,H24b), C25(H25a,H25b),
 C26(H26a,H26b), C27(H27a,H27b), C28(H28a,H28b), C29(H29a,H29b), C30(H30a,H30b),
  C31(H31a,H31b), C32(H32a,H32b), C33(H33a,H33b), C34(H34a,H34b), C35(H35a,
 H35b), C36(H36a,H36b), C37(H37a,H37b), C38(H38a,H38b), C37'(H37c,H37d),
 C38'(H38c,H38d), C39(H39a,H39b), C39(H39c,H39d), C40(H40a,H40b), C41(H41a,
 H41b), C40'(H40c,H40d), C41'(H41c,H41d), C42(H42c,H42d), C42(H42a,H42b),
 C44(H44a,H44b), C43'(H43a,H43b), C44'(H44c,H44d), C45(H45a,H45b), C45(H45c,
 H45d), C46(H46a,H46b), C46'(H46c,H46d), C47(H47c,H47d), C47(H47a,H47b),
 C48(H48a,H48b), C48'(H48c,H48d), C49(H49a,H49b), C49(H49c,H49d), C50(H50a,
 H50b), C51(H51a,H51b), C51'(H51c,H51d), C52(H52a,H52b), C52(H52c,H52d),
 C53(H53a,H53b), C54(H54a,H54b), C53'(H53c,H53d), C54'(H54c,H54d), C55(H55a,
 H55b), C56(H56a,H56b), C55'(H55c,H55d), C56'(H56c,H56d), C57(H57a,H57b),
 C58(H58a,H58b), C59(H59a,H59b), C59(H59c,H59d), C60(H60a,H60b), C60'(H60c,
 H60d), C61(H61a,H61b), C62(H62c,H62d), C62(H62a,H62b), C63(H63a,H63b),
 C63(H63c,H63d), C64(H64a,H64b), C65(H65a,H65b), C66(H66a,H66b), C67(H67a,H67b),
  C68(H68a,H68b), C69(H69a,H69b), C70(H70a,H70b), C71(H71a,H71b), C64'(H64c,
 H64d), C66'(H66c,H66d), C67'(H67c,H67d), C68'(H68c,H68d), C69'(H69c,H69d),
 C70'(H70c,H70d), C71'(H71c,H71d), C72(H72a,H72b), C72(H72c,H72d)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              35165
_shelx_fab_checksum              33776
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.994
_oxdiff_exptl_absorpt_empirical_full_min 0.421