Synthesis and characterisation of the ternary intermetalloid clusters {M@[As<sub>8</sub>(ZnMes)<sub>4</sub>]}<sup>3-</sup> (M = Nb, Ta) from binary [M@As<sub>8</sub>]<sup>3-</sup> precursors.
Zhang, Wei-Qiang; Morgan, Harry W. T.; McGrady, John E.; Sun, Zhong-Ming; Chemical science 13 (2022) 6744–6748; doi:10.1039/d2sc01748b

data_1566977
_publ_section_title
;
 Synthesis and characterisation of the ternary intermetalloid clusters
 {M@[As<sub>8</sub>(ZnMes)<sub>4</sub>]}<sup>3-</sup> (M = Nb, Ta) from
 binary [M@As<sub>8</sub>]<sup>3-</sup> precursors.
;
_journal_issue                   22
_journal_name_full               'Chemical science'
_journal_page_first              6744
_journal_page_last               6748
_journal_paper_doi               10.1039/d2sc01748b
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety
'C36 H44 As8 Ta Zn4, 3(C18 H36 K N2 O6), C2 H8 N2'
_chemical_formula_sum            'C92 H160 As8 K3 N8 O18 Ta Zn4'
_chemical_formula_weight         2825.36
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-22
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-01 deposited with the CCDC.	2022-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.2903(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0926(2)
_cell_length_b                   32.8161(4)
_cell_length_c                   22.5199(3)
_cell_measurement_reflns_used    18594
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.5840
_cell_measurement_theta_min      3.7690
_cell_volume                     12240.8(3)
_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  'SHELXL 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 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 0.984
_diffrn_measured_fraction_theta_max 0.998
_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    -39.00  10.00   0.50    0.50    --    0.00 -82.00 -30.00   98
  2  \w      9.00  34.00   0.50    0.50    --    0.00 -82.00 120.00   50
  3  \w    -20.00   7.00   0.50    0.50    --    0.00 -57.00  90.00   54
  4  \w    -38.00   5.00   0.50    0.50    --    0.00 -82.00 120.00   86
  5  \w    -83.00 -48.00   0.50    0.50    --    0.00 -57.00  90.00   70
  6  \w    -21.00  16.00   0.50    0.50    --    0.00 -82.00-180.00   74
  7  \w     81.00 125.00   0.50    1.00    --  101.90  82.00-150.00   88
  8  \w     41.00 133.00   0.50    1.00    --  101.90 -77.00-120.00  184
  9  \w     51.00 125.00   0.50    1.00    --  101.90 -57.00-120.00  148
 10  \w    130.00 187.00   0.50    1.00    --  101.90  57.00  30.00  114
 11  \w     36.00  82.00   0.50    1.00    --  101.90 -38.00-120.00   92
 12  \w     93.00 125.00   0.50    1.00    --  101.90 -38.00-120.00   64
 13  \w     75.00 160.00   0.50    1.00    --  101.90  57.00 120.00  170
 14  \w     80.00 114.00   0.50    1.00    --  101.90  57.00  30.00   68
 15  \w    129.00 187.00   0.50    1.00    --  101.90  38.00  60.00  116
 16  \w     80.00 125.00   0.50    1.00    --  101.90  38.00  60.00   90
;
_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      0.0303066000
_diffrn_orient_matrix_UB_12      -0.0296019000
_diffrn_orient_matrix_UB_13      -0.0424901000
_diffrn_orient_matrix_UB_21      -0.0066046000
_diffrn_orient_matrix_UB_22      0.0341415000
_diffrn_orient_matrix_UB_23      -0.0479840000
_diffrn_orient_matrix_UB_31      0.0876935000
_diffrn_orient_matrix_UB_32      0.0127537000
_diffrn_orient_matrix_UB_33      0.0295426000
_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  0.0482
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            63830
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.998
_diffrn_reflns_theta_min         3.792
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    6.255
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46860
_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            red-brown
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       strip
_exptl_crystal_F_000             5704
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.504
_refine_diff_density_min         -1.844
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1219
_refine_ls_number_reflns         21784
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+30.1707P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17541
_reflns_number_total             21784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01748b2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 1566976--1566977.cif.'
_cod_database_code               1566977
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.79
_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 N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H7D-H53B
 2.58 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C12(H12A,H12B), C16(H16A,H16B), C23(H23A,H23B), C5(H5A,H5B),
 C17(H17A,H17B), C29(H29A,H29B), C15(H15A,H15B), C27(H27A,H27B), C30(H30A,H30B),
  C6(H6A,H6B), C46(H46A,H46B), C47(H47A,H47B), C11(H11A,H11B), C45(H45A,H45B),
 C36(H36A,H36B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B), C40(H40A,H40B),
  C38(H38A,H38B), C10(H10A,H10B), C35(H35A,H35B), C42(H42A,H42B), C26(H26A,
 H26B), C41(H41A,H41B), C39(H39A,H39B), C9(H9A,H9B), C48(H48A,H48B), C28(H28A,
 H28B), C34(H34A,H34B), C37(H37A,H37B), C54(H54A,H54B), C53(H53A,H53B), C4(H4A,
 H4B), C13(H13A,H13B), C33(H33A,H33B), C32(H32A,H32B), C31(H31A,H31B), C8(H8A,
 H8B), C25(H25A,H25B), C92(H92A,H92B), C14(H14A,H14B), C3(H3A,H3B), C7(H7A,H7B),
  C20(H20A,H20B), C43(H43A,H43B), C1(H1A,H1B), C44(H44A,H44B), C2(H2A,H2B),
 C50(H50A,H50B), C49(H49A,H49B), C91(H91A,H91B), C19(H19A,H19B), C51(H51A,H51B),
  C52(H52A,H52B)
3.b Aromatic/amide H refined with riding coordinates:
 C58(H58), C85(H85), C79(H79), C61(H61), C76(H76), C88(H88), C70(H70), C67(H67)
3.c X=CH2 refined with riding coordinates:
 N8(H8C,H8D), N7(H7C,H7D)
3.d Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C90(H90A,H90B,H90C), C63(H63A,H63B,H63C), C81(H81A,H81B,
 H81C), C84(H84A,H84B,H84C), C75(H75A,H75B,H75C), C57(H57A,H57B,H57C), C72(H72A,
 H72B,H72C), C60(H60A,H60B,H60C), C87(H87A,H87B,H87C), C78(H78A,H78B,H78C),
 C69(H69A,H69B,H69C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40251
_shelx_hkl_checksum              17671
_shelx_fab_checksum              65981
_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 3.017
_oxdiff_exptl_absorpt_empirical_full_min 0.525