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_1566976
_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 Nb Zn4, 3(C18 H36 K N2 O6), C2 H8 N2, C2 H7 N2, C7 H8'
_chemical_formula_sum            'C101 H175 As8 K3 N10 Nb O18 Zn4'
_chemical_formula_weight         2888.55
_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     iterative
_audit_creation_date             2021-05-13
_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                 104.5190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9909(2)
_cell_length_b                   33.0617(4)
_cell_length_c                   22.6750(2)
_cell_measurement_reflns_used    30150
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.4250
_cell_measurement_theta_min      3.7280
_cell_volume                     12330.9(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 1.3-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 0.981
_diffrn_measured_fraction_theta_max 0.997
_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    -36.00   5.00   0.50    1.74    --  -35.00 -82.00 120.00   82
  2  \w   -103.00 -77.00   0.50    1.74    --  -35.00 -77.00 150.00   52
  3  \w    -31.00   2.00   0.50    1.74    --  -35.00 -82.00-120.00   66
  4  \w    -69.00  44.00   0.50    1.74    --  -35.00  57.00  60.00  226
  5  \w     84.00 133.00   0.50    1.74    --   43.40  82.00   0.00   98
  6  \w     11.00  37.00   0.50    1.74    --   43.40  77.00 150.00   52
  7  \w     22.00  48.00   0.50    1.74    --   43.40  77.00 -30.00   52
  8  \w     89.00 117.00   0.50    6.95    --  104.50  82.00-120.00   56
  9  \w     88.00 146.00   0.50    6.95    --  104.50  82.00-150.00  116
 10  \w    117.00 145.00   0.50    6.95    --  104.50 -45.00  60.00   56
 11  \w     18.00 100.00   0.50    6.95    --  104.50 -45.00  60.00  164
 12  \w     67.00 161.00   0.50    6.95    --  104.50  45.00 -30.00  188
 13  \w    163.00 192.00   0.50    6.95    --  104.50  82.00 -90.00   58
 14  \w     79.00 142.00   0.50    6.95    --  104.50  61.00-180.00  126
 15  \w    163.00 189.00   0.50    6.95    --  104.50  61.00-180.00   52
 16  \w    129.00 192.00   0.50    6.95    --  104.50  82.00-120.00  126
 17  \w    164.00 189.00   0.50    6.95    --  104.50  82.00-150.00   50
 18  \w     74.00 185.00   0.50    6.95    --  104.50  45.00 -60.00  222
;
_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      0.0717125000
_diffrn_orient_matrix_UB_12      0.0296105000
_diffrn_orient_matrix_UB_13      0.0066064000
_diffrn_orient_matrix_UB_21      0.0286333000
_diffrn_orient_matrix_UB_22      -0.0230917000
_diffrn_orient_matrix_UB_23      -0.0498459000
_diffrn_orient_matrix_UB_31      -0.0530875000
_diffrn_orient_matrix_UB_32      0.0275494000
_diffrn_orient_matrix_UB_33      -0.0489526000
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            62745
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.993
_diffrn_reflns_theta_min         3.740
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    5.397
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46202
_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            green
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       block
_exptl_crystal_F_000             5908
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1326
_refine_ls_number_reflns         21908
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+38.3699P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20269
_reflns_number_total             21908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01748b2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 1566976--1566977.cif.'
_cod_database_code               1566976
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 H5B-H8D
 2.38 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(C94) = Uanis(C94')
Uanis(N10) = Uanis(N10')
3. Others
 Sof(N10')=Sof(H10E)=Sof(H10F)=Sof(H93A)=Sof(C94')=Sof(H94C)=Sof(H94D)=1-FVAR(1)
 Sof(N10)=Sof(H10C)=Sof(H10D)=Sof(H93)=Sof(C94)=Sof(H94A)=Sof(H94B)=FVAR(1)
4.a 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), C39(H39A,H39B),
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B),
  C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,
 H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B),
 C54(H54A,H54B), C91(H91A,H91B), C92(H92A,H92B), C94(H94A,H94B), C94'(H94C,H94D)
4.b Aromatic/amide H refined with riding coordinates:
 C58(H58), C61(H61), C67(H67), C70(H70), C76(H76), C79(H79), C85(H85),
 C88(H88), C93(H93), C93(H93A), C95(H95), C96(H96), C97(H97), C98(H98),
 C101(H101)
4.c X=CH2 refined with riding coordinates:
 N7(H7C,H7D), N8(H8C,H8D), N9(H9C,H9D), N10(H10C,H10D), N10'(H10E,H10F)
4.d Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C60(H60A,H60B,H60C), C63(H63A,H63B,H63C), C66(H66A,H66B,
 H66C), C69(H69A,H69B,H69C), C72(H72A,H72B,H72C), C75(H75A,H75B,H75C), C78(H78A,
 H78B,H78C), C81(H81A,H81B,H81C), C84(H84A,H84B,H84C), C87(H87A,H87B,H87C),
 C90(H90A,H90B,H90C), C100(H10G,H10H,H10I)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3787
_shelx_hkl_checksum              21846
_shelx_fab_checksum              56334
_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 1.698
_oxdiff_exptl_absorpt_empirical_full_min 0.302