[V4Mo3O14(NAr)3(μ2-NAr)3](2-): the first polyarylimido-stabilized molybdovanadate cluster.
Huang, Yichao; Zhang, Jiangwei; Ge, Jingxuan; Sui, Chong; Hao, Jian; Wei, Yongge; Chemical communications (Cambridge, England) 53 (2017) 2551–2554; doi:10.1039/c7cc00166e

data_7119518
_publ_section_title
;
 [V4Mo3O14(NAr)3(\m2-NAr)3](2-): the first polyarylimido-stabilized
 molybdovanadate cluster.
;
_journal_issue                   17
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2551
_journal_page_last               2554
_journal_paper_doi               10.1039/c7cc00166e
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C36 H29 Mo3 N6 O14 V4,2(C16 H36 N)'
_chemical_formula_sum            'C68 H102 Mo3 N8 O14 V4'
_chemical_formula_weight         1747.16
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc13ph7j
_audit_creation_date             2015-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2015-02-23 deposited with the CCDC.
2017-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                107.438(6)
_cell_angle_beta                 92.843(5)
_cell_angle_gamma                108.583(5)
_cell_formula_units_Z            2
_cell_length_a                   13.4643(7)
_cell_length_b                   16.5903(11)
_cell_length_c                   21.0115(14)
_cell_measurement_reflns_used    3716
_cell_measurement_temperature    98(5)
_cell_measurement_theta_max      29.3430
_cell_measurement_theta_min      2.9242
_cell_volume                     4189.3(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      98(5)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -10.00   18.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.8148   37.0000  -60.0000 28

  2 omega  -42.00   49.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1273  -77.0000 -120.0000 91

  3 omega   17.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1273   55.0000  101.0000 73

  4 omega  -32.00   17.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1273  -37.0000  -90.0000 49

  5 omega   -9.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1273   77.0000    0.0000 100

  6 omega   19.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1273  -77.0000 -180.0000 28

  7 omega  -18.00   10.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1273  -77.0000  150.0000 28

  8 omega   -4.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1273   77.0000  150.0000 91
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0031631000
_diffrn_orient_matrix_UB_12      0.0266064000
_diffrn_orient_matrix_UB_13      -0.0203331000
_diffrn_orient_matrix_UB_21      -0.0471655000
_diffrn_orient_matrix_UB_22      0.0038579000
_diffrn_orient_matrix_UB_23      0.0119816000
_diffrn_orient_matrix_UB_31      0.0305778000
_diffrn_orient_matrix_UB_32      0.0395548000
_diffrn_orient_matrix_UB_33      0.0269524000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_unetI/netI     0.1509
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36311
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.159
_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     838
_refine_ls_number_reflns         16442
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1028P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1011
_reflns_number_gt                9495
_reflns_number_total             16442
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc00166e2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7119518--7119521.cif.'
_cod_original_cell_volume        4189.3(4)
_cod_database_code               7119518
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C66-C65 = C65-C64B = C48-C47 = C69B-C70B = C68B-C69B
 1.53 with sigma of 0.01
3. Rigid bond restraints
 N8, C63B, C64B, C67B, C68B, C70B, C65, C69B, C66
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
N8 \\sim C63B \\sim C64B \\sim C67B \\sim C68B \\sim C70B \\sim C65 \\sim C69B
\\sim C66: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C61B) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C40B) \\sim Ueq, Uanis(C59B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C39) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44B) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C53) = Uanis(C51) = Uanis(C52) = Uanis(C54)
5. Others
 Sof(H50C)=Sof(H50D)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=
 Sof(H54C)=1-FVAR(1)
 Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=
 Sof(H52C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C37(H37A,H37B), C41(H41A,H41B), C45(H45A,H45B), C38(H38A,
 H38B), C59B(H59A,H59B), C42(H42A,H42B), C50(H50A,H50B), C50(H50C,H50D),
 C63B(H63A,H63B), C39(H39A,H39B), C46(H46A,H46B), C57(H57A,H57B), C56(H56A,
 H56B), C55(H55A,H55B), C60B(H60A,H60B), C64B(H64A,H64B), C51(H51A,H51B),
 C43(H43A,H43B), C67B(H67A,H67B), C68B(H68A,H68B), C65(H65A,H65B), C69B(H69A,
 H69B), C61B(H61A,H61B), C47(H47A,H47B), C53(H53A,H53B)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C24(H24), C23(H23), C35(H35), C32(H32), C12(H12), C3(H3), C2(H2),
 C33(H33), C18(H18), C30(H30), C28(H28), C29(H29), C26(H26), C10(H10), C6(H6),
 C5(H5), C36(H36), C34(H34), C11(H11), C27(H27), C20(H20), C17(H17), C9(H9),
 C14(H14), C16(H16), C4(H4), C22(H22), C15(H15), C21(H21)
6.c Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C48(H48A,H48B,H48C), C40B(H40A,H40B,H40C), C70B(H70A,
 H70B,H70C), C44B(H44A,H44B,H44C), C52(H52A,H52B,H52C), C62(H62A,H62B,H62C),
 C66(H66A,H66B,H66C), C54(H54A,H54B,H54C)
;