[Ga@Bi<sub>10</sub>(NbMes)<sub>2</sub>]<sup>3-</sup>: a linear Nb-Ga<sup>I</sup>-Nb filament coordinated by a bismuth cage.
Qiao, Lei; Yang, Tao; Frenking, Gernot; Sun, Zhong-Ming; Chemical communications (Cambridge, England) 59 (2023) 4024–4027; doi:10.1039/d3cc00631j

data_7131395
_publ_section_title
;
 [Ga@Bi<sub>10</sub>(NbMes)<sub>2</sub>]<sup>3-</sup>: a linear
 Nb-Ga<sup>I</sup>-Nb filament coordinated by a bismuth cage.
;
_journal_issue                   27
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4024
_journal_page_last               4027
_journal_paper_doi               10.1039/d3cc00631j
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety
'C18 H24 Bi10 Ga Nb2, 3(C18 H36 K N2 O6), 0.5(C7 H8), 0.5[C7H8]'
_chemical_formula_sum            'C79 H140 Bi10 Ga K3 N6 Nb2 O18'
_chemical_formula_weight         3924.60
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-03-01 deposited with the CCDC.	2023-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                89.942(2)
_cell_angle_beta                 86.298(2)
_cell_angle_gamma                76.288(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0159(3)
_cell_length_b                   15.5134(4)
_cell_length_c                   27.2898(8)
_cell_measurement_reflns_used    10715
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.4990
_cell_measurement_theta_min      3.7280
_cell_volume                     5341.6(2)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.963
_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 -10.00   0.50    0.50    --    0.00 -77.00-120.00   74
  2  \w     -4.00  48.00   0.50    0.50    --    0.00  77.00 -90.00  104
  3  \w    -20.00  33.00   0.50    0.50    --    0.00 -82.00  90.00  106
  4  \w     -7.00  26.00   0.50    0.50    --    0.00 -77.00-120.00   66
  5  \w    -36.00  32.00   0.50    0.50    --    0.00 -82.00 -30.00  136
  6  \w    -39.00 -12.00   0.50    0.50    --    0.00 -82.00 150.00   54
  7  \w    -20.00  31.00   0.50    0.50    --    0.00 -19.00 -30.00  102
  8  \w    -88.00 -36.00   0.50    0.50    --    0.00 -19.00 -30.00  104
  9  \w     12.00  44.00   0.50    0.50    --  101.30 -82.00 -90.00   64
 10  \w     76.00 191.00   0.50    0.50    --  101.30  19.00   0.00  230
 11  \w    119.00 182.00   0.50    0.50    --  101.30  38.00 -60.00  126
 12  \w     94.00 121.00   0.50    0.50    --  101.30  82.00-150.00   54
 13  \w     41.00 137.00   0.50    0.50    --  101.30 -82.00 120.00  192
 14  \w     66.00 174.00   0.50    0.50    --  101.30  19.00  60.00  216
 15  \w     83.00 109.00   0.50    0.50    --  101.30 -82.00  60.00   52
 16  \w     13.00  38.00   0.50    0.50    --  101.30 -82.00-150.00   50
 17  \w     26.00  79.00   0.50    0.50    --  101.30 -82.00  60.00  106
 18  \w     56.00 118.00   0.50    0.50    --  101.30 -82.00   0.00  124
 19  \w     49.00 132.00   0.50    0.50    --  101.30 -82.00 -90.00  166
 20  \w     81.00 138.00   0.50    0.50    --  101.30 -82.00-150.00  114
 21  \w    101.00 176.00   0.50    0.50    --  101.30  19.00  90.00  150
 22  \w    155.00 191.00   0.50    0.50    --  101.30  82.00-150.00   72
 23  \w     13.00 124.00   0.50    0.50    --  101.30 -57.00 120.00  222
 24  \w     83.00 109.00   0.50    0.50    --  101.30 -82.00 -60.00   52
 25  \w     12.00  99.00   0.50    0.50    --  101.30 -57.00 -90.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.1006
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            58304
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.987
_diffrn_reflns_theta_min         3.503
_exptl_absorpt_coefficient_mu    35.072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22843
_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            'metallic dark black'
_exptl_crystal_density_diffrn    2.440
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.103
_refine_diff_density_min         -1.937
_refine_diff_density_rms         0.265
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.478(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2194
_refine_ls_number_reflns         27556
_refine_ls_number_restraints     6510
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.069
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0341P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1236
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                23405
_reflns_number_total             27556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00631j2.cif
_cod_data_source_block           Bi10GaNb2Mes2
_cod_depositor_comments          'Adding full bibliography for 7131395.cif.'
_cod_database_code               7131395
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.334
_shelx_estimated_absorpt_t_min   0.227
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.522(5)
 0.478(5)
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. Restrained distances
 C13-C14
 1.53 with sigma of 0.01
 C11-C12 = C57_$1-C58_$1
 1.53 with sigma of 0.01
4. 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
Uanis(C135) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C129) \\sim Ueq, Uanis(C130) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.02
5. Others
 Sof(Bi3B)=1-FVAR(1)
 Sof(Bi3A)=FVAR(1)
 Sof(Bi8B)=1-FVAR(2)
 Sof(Bi8A)=FVAR(2)
 Sof(Bi2B)=1-FVAR(3)
 Sof(Bi2A)=FVAR(3)
 Sof(Bi6B)=1-FVAR(4)
 Sof(Bi6A)=FVAR(4)
 Sof(Bi5B)=1-FVAR(5)
 Sof(Bi5A)=FVAR(5)
 Sof(Bi0B)=1-FVAR(6)
 Sof(Bi0A)=FVAR(6)
 Sof(Bi7B)=1-FVAR(7)
 Sof(Bi7A)=FVAR(7)
 Sof(Bi9B)=1-FVAR(8)
 Sof(Bi9A)=FVAR(8)
 Sof(Bi1B)=1-FVAR(9)
 Sof(Bi1A)=FVAR(9)
 Sof(Bi4B)=1-FVAR(10)
 Sof(Bi4A)=FVAR(10)
6.a Secondary CH2 refined with riding coordinates:
 C92(H92A,H92B), C69(H69A,H69B), C71(H71A,H71B), C4(H4A,H4B), C108(H10A,H10B),
 C107(H10C,H10D), C105(H10E,H10F), C16(H16A,H16B), C38(H38A,H38B), C89(H89A,
 H89B), C32(H32A,H32B), C25(H25A,H25B), C37(H37A,H37B), C91(H91A,H91B),
 C70(H70A,H70B), C64(H64A,H64B), C36(H36A,H36B), C60(H60A,H60B), C44(H44A,H44B),
  C54(H54A,H54B), C72(H72A,H72B), C63(H63A,H63B), C21(H21A,H21B), C5(H5A,H5B),
 C46(H46A,H46B), C26(H26A,H26B), C40(H40A,H40B), C35(H35A,H35B), C2(H2A,H2B),
 C15(H15A,H15B), C51(H51A,H51B), C68(H68A,H68B), C39(H39A,H39B), C47(H47A,H47B),
  C66(H66A,H66B), C61(H61A,H61B), C97(H97A,H97B), C57(H57A,H57B), C17(H17A,
 H17B), C43(H43A,H43B), C20(H20A,H20B), C30(H30A,H30B), C95(H95A,H95B),
 C98(H98A,H98B), C102(H10G,H10H), C33(H33A,H33B), C106(H10I,H10J), C100(H10K,
 H10L), C99(H99A,H99B), C103(H10M,H10N), C53(H53A,H53B), C45(H45A,H45B),
 C58(H58A,H58B), C23(H23A,H23B), C104(H10O,H10P), C81(H81A,H81B), C28(H28A,
 H28B), C34(H34A,H34B), C62(H62A,H62B), C86(H86A,H86B), C29(H29A,H29B),
 C93(H93A,H93B), C24(H24A,H24B), C101(H10Q,H10R), C84(H84A,H84B), C83(H83A,
 H83B), C55(H55A,H55B), C50(H50A,H50B), C22(H22A,H22B), C19(H19A,H19B),
 C87(H87A,H87B), C18(H18A,H18B), C31(H31A,H31B), C85(H85A,H85B), C56(H56A,H56B),
  C94(H94A,H94B), C42(H42A,H42B), C96(H96A,H96B), C8(H8A,H8B), C9(H9A,H9B),
 C52(H52A,H52B), C1(H1A,H1B), C48(H48A,H48B), C6(H6A,H6B), C12(H12J,H12K),
 C3(H3A,H3B), C88(H88A,H88B), C13(H13A,H13B), C27(H27A,H27B), C67(H67A,H67B),
 C7(H7A,H7B), C59(H59A,H59B), C11(H11J,H11K), C79(H79A,H79B), C77(H77A,H77B),
 C10(H10S,H10T), C41(H41A,H41B), C80(H80A,H80B), C82(H82A,H82B), C65(H65A,H65B),
  C90(H90A,H90B), C78(H78A,H78B), C74(H74A,H74B), C14(H14A,H14B), C49(H49A,
 H49B), C73(H73A,H73B), C75(H75A,H75B), C76(H76A,H76B)
6.b Aromatic/amide H refined with riding coordinates:
 C130(H130), C114(H114), C120(H120), C141(H141), C132(H132), C112(H112),
 C110(H110), C137(H137), C128(H128), C118(H118), C139(H139), C122(H122),
 C5AA(H5AA), C1AA(H1AA), C4AA(H4AA), C3AA(H3AA), C2AA(H2AA)
6.c Idealised Me refined as rotating group:
 C135(H13C,H13D,H13E), C116(H11A,H11B,H11C), C124(H12A,H12B,H12C), C115(H11D,
 H11E,H11F), C126(H12D,H12E,H12F), C134(H13F,H13G,H13H), C117(H11G,H11H,H11I),
 C133(H13I,H13J,H13K), C142(H14C,H14D,H14E), C143(H14F,H14G,H14H), C125(H12G,
 H12H,H12I), C144(H14I,H14J,H14K), C6AA(H6AA,H6AB,H6AC)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 57 electrons were 
found in a volume of 365\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C7H8] per Asymmetric Unit 
which account for 50 electrons 
per unit cell.
;
_shelx_res_checksum              83550
_shelx_hkl_checksum              61415
_shelx_fab_checksum              76835
_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
;