[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_7119519
_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
'Mo2.5 O9.5 V0.5, Mo2.38 O9.5 V0.62, 2(C16 H36 N), C16 H35 N'
_chemical_formula_sum            'C48 H107 Mo5 N3 O19 V'
_chemical_formula_weight         1555.66
_chemical_name_systematic        Mo5V1
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-10-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-10-31 deposited with the CCDC.
2017-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.089(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.2304(18)
_cell_length_b                   18.5275(10)
_cell_length_c                   27.1217(13)
_cell_measurement_reflns_used    4894
_cell_measurement_temperature    102.8
_cell_measurement_theta_max      29.6124
_cell_measurement_theta_min      3.0333
_cell_volume                     13511.6(15)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      102.8
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.825
_diffrn_measurement_details
;
  1 omega  -80.00  -16.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2918  -77.0000   60.0000 64

  2 omega  -40.00   33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6043  -37.0000  -60.0000 73

  3 omega   34.00   60.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6043 -104.0000  -24.0000 26

  4 omega   -1.00   72.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6043   37.0000  -90.0000 73
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0100038000
_diffrn_orient_matrix_UB_12      0.0329635000
_diffrn_orient_matrix_UB_13      0.0046214000
_diffrn_orient_matrix_UB_21      -0.0237002000
_diffrn_orient_matrix_UB_22      -0.0164644000
_diffrn_orient_matrix_UB_23      -0.0077777000
_diffrn_orient_matrix_UB_31      0.0057772000
_diffrn_orient_matrix_UB_32      -0.0104340000
_diffrn_orient_matrix_UB_33      0.0269547000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.1092
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.825
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            34705
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.825
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.678
_diffrn_reflns_theta_min         3.039
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91942
_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            orange
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       block
_exptl_crystal_F_000             6390
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.33
_refine_diff_density_max         1.466
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         15791
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+37.0363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9439
_reflns_number_total             15791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc00166e2.cif
_cod_data_source_block           exp_3682
_cod_depositor_comments
'Adding full bibliography for 7119518--7119521.cif.'
_cod_original_formula_sum        'C48 H107 Mo5 N3 O19 V1'
_cod_database_code               7119519
_chemical_oxdiff_formula         Mo
_shelx_estimated_absorpt_t_max   1.0
_shelx_estimated_absorpt_t_min   0.919
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Mo4, V42}
{V22, Mo6}
{Mo5, V4}
{Mo1, V60}
{Mo3, V18}
{Mo2, V39}
3. Restrained distances
 C0BA-C17
 1.5 with sigma of 0.02
 C17-C1C
 1.5 with sigma of 0.02
 C4AA-C1F
 1.5 with sigma of 0.02
 C9BA-C6CB
 1.5 with sigma of 0.02
 C9BA-C6CA
 1.5 with sigma of 0.02
 C6CA-C9BA
 1.53 with sigma of 0.02
 C6CB-C9BA
 1.53 with sigma of 0.02
 C1C-C17
 1.53 with sigma of 0.02
 C5CA-C3
 1.53 with sigma of 0.02
 C0BA-C17
 2.52 with sigma of 0.04
 C0BA-C1C
 2.52 with sigma of 0.04
 C-C1F
 2.52 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C4AA) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C6CA) = Uanis(C6CB)
Uanis(V22) = Uanis(Mo6)
Uanis(Mo5) = Uanis(V4)
Uanis(Mo1) = Uanis(V60)
Uanis(Mo3) = Uanis(V18)
Uanis(Mo2) = Uanis(V39)
Uanis(Mo4) = Uanis(V42)
5. Others
 Sof(H9BB)=1-FVAR(1)
 Sof(H9BA)=FVAR(1)
 Sof(V42)=1-FVAR(2)
 Sof(Mo4)=FVAR(2)
 Sof(Mo6)=1-FVAR(3)
 Sof(V22)=FVAR(3)
 Sof(V4)=1-FVAR(4)
 Sof(Mo5)=FVAR(4)
 Sof(V60)=1-FVAR(5)
 Sof(Mo1)=FVAR(5)
 Sof(V18)=1-FVAR(6)
 Sof(Mo3)=FVAR(6)
 Sof(V39)=1-FVAR(7)
 Sof(Mo2)=FVAR(7)
 Fixed Sof: C6CA(0.66666) H6CA(0.66666) H6CB(0.66666) H6CC(0.66666)
 C6CB(0.33333) H6CD(0.33333) H6CE(0.33333) H6CF(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C(HA,HB), C18(H18A,H18B), C20(H20A,H20B), C0AA(H0AA,H0AB),
 C1AA(H1AC,H1AD), C4(H4A,H4B), C3BA(H3BA,H3BB), C2AA(H2AA,H2AB), C3AA(H3AA,
 H3AB), C4AA(H4AA,H4AB), C5AA(H5AA,H5AB), C6AA(H6AA,H6AB), C8AA(H8AA,H8AB),
 C9AA(H9AA,H9AB), C0BA(H0BA,H0BB), C4BA(H4BA,H4BB), C19(H19A,H19B), C1(H1A,H1B),
  C5BA(H5BA,H5BB), C3(H3A,H3B), C6BA(H6BA,H6BB), C1A(H1AA,H1AB), C1B(H1BA,H1BB),
  C17(H17A,H17B)
6.b Aromatic/amide H refined with riding coordinates:
 C9BA(H9BA), C9BA(H9BB)
6.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C16(H16A,H16B,H16C), C1BA(H1BC,H1BD,H1BE), C2BA(H2BA,H2BB,
 H2BC), C5CA(H5CA,H5CB,H5CC), C8BA(H8BA,H8BB,H8BC), C2CA(H2CA,H2CB,H2CC),
 C3CA(H3CA,H3CB,H3CC), C6CA(H6CA,H6CB,H6CC), C6CB(H6CD,H6CE,H6CF), C1C(H1CA,
 H1CB,H1CC), C1D(H1DA,H1DB,H1DC), C1F(H1FA,H1FB,H1FC)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'