[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_7119521
_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 H30 Mo3 N6 O14 V4, 2(C19 H30 N3), 2(C3 H7 N O)'
_chemical_formula_sum            'C80 H104 Mo3 N14 O16 V4'
_chemical_formula_weight         2009.35
_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
_audit_creation_date             2016-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-11-27 deposited with the CCDC.
2017-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                103.598(2)
_cell_angle_beta                 96.5613(17)
_cell_angle_gamma                105.634(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5610(3)
_cell_length_b                   14.4766(4)
_cell_length_c                   25.9310(6)
_cell_measurement_reflns_used    18921
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.6490
_cell_measurement_theta_min      4.4030
_cell_volume                     4333.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_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     31.00  82.00   1.00    1.00    --   40.81 -99.00 120.00   51
  2  \w     31.00  76.00   1.00    2.58    --  112.00 -95.00   0.00   45
  3  \w     57.00 108.00   1.00    2.58    --  112.00 -95.00  30.00   51
  4  \w    110.00 137.00   1.00    2.58    --  112.00 -30.00 -60.00   27
  5  \w     86.00 173.00   1.00    2.58    --  112.00  30.00 -90.00   87
  6  \w    100.00 152.00   1.00    2.58    --  112.00 125.00-180.00   52
  7  \w     84.00 178.00   1.00    2.58    --  112.00  30.00   0.00   94
  8  \w     95.00 121.00   1.00    2.58    --  112.00-125.00-150.00   26
  9  \w     56.00 108.00   1.00    2.58    --  112.00 -95.00 -60.00   52
 10  \w     56.00 134.00   1.00    2.58    --  112.00 -77.00  60.00   78
 11  \w     51.00  83.00   1.00    1.00    --   40.81-125.00 -30.00   32
 12  \w     38.00 140.00   1.00    2.58    --  112.00 -30.00  30.00  102
 13  \w     48.00  94.00   1.00    2.58    --  112.00 -30.00 -60.00   46
 14  \w     40.00 138.00   1.00    2.58    --  112.00 -45.00-180.00   98
 15  \w     30.00 105.00   1.00    2.58    --  112.00 -95.00-150.00   75
 16  \w    -73.00  -8.00   1.00    1.00    --  -40.81 125.00 -60.00   65
 17  \w   -115.00 -21.00   1.00    1.00    --  -40.81 -38.00 150.00   94
 18  \w   -102.00 -25.00   1.00    1.00    --  -40.81 -38.00-120.00   77
 19  \w   -108.00 -18.00   1.00    1.00    --  -40.81 -57.00  60.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0202918000
_diffrn_orient_matrix_UB_12      -0.0900779000
_diffrn_orient_matrix_UB_13      0.0167246000
_diffrn_orient_matrix_UB_21      0.0976323000
_diffrn_orient_matrix_UB_22      0.0712479000
_diffrn_orient_matrix_UB_23      0.0454551000
_diffrn_orient_matrix_UB_31      -0.0829603000
_diffrn_orient_matrix_UB_32      0.0066087000
_diffrn_orient_matrix_UB_33      0.0391123000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32458
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.880
_diffrn_reflns_theta_min         3.572
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.493
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       plate
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.172
_refine_diff_density_min         -1.231
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1100
_refine_ls_number_reflns         17728
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0613P)^2^+2.0454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16178
_reflns_number_total             17728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc00166e2.cif
_cod_data_source_block           exp_347
_cod_depositor_comments
'Adding full bibliography for 7119518--7119521.cif.'
_cod_original_cell_volume        4333.34(19)
_cod_database_code               7119521
_chemical_oxdiff_formula         Mo3V4O14C28H36N10
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C79A-N14A
 1.45 with sigma of 0.02
 C78A-N14A
 1.45 with sigma of 0.02
 N14A-C80A
 1.3 with sigma of 0.02
 C80A-O16A
 1.2 with sigma of 0.02
 C78B-N14B
 1.45 with sigma of 0.02
 C79B-N14B
 1.45 with sigma of 0.02
 N14B-C80B
 1.3 with sigma of 0.02
 C80B-O16B
 1.2 with sigma of 0.02
 C79B-C78B
 2.5 with sigma of 0.04
3. Restrained planarity
 O16A, C79A, C78A, C80A, N14A
 with sigma of 0.1
 C79B, C80B, C78B, N14B, O16B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C79B) = Uanis(C78B)
5. Others
 Sof(C79B)=Sof(H79D)=Sof(H79E)=Sof(H79F)=Sof(C80B)=Sof(H80B)=Sof(C78B)=
 Sof(H78D)=Sof(H78E)=Sof(H78F)=Sof(N14B)=Sof(O16B)=1-FVAR(1)
 Sof(O16A)=Sof(C79A)=Sof(H79A)=Sof(H79B)=Sof(H79C)=Sof(C78A)=Sof(H78A)=
 Sof(H78B)=Sof(H78C)=Sof(C80A)=Sof(H80A)=Sof(N14A)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C49(H49), C67(H67), C61(H61), C43(H43)
6.b Secondary CH2 refined with riding coordinates:
 C72(H72A,H72B), C53(H53A,H53B), C54(H54A,H54B), C69(H69A,H69B), C68(H68A,
 H68B), C52(H52A,H52B), C71(H71A,H71B), C66(H66A,H66B), C70(H70A,H70B),
 C47(H47A,H47B), C48(H48A,H48B), C44(H44A,H44B), C62(H62A,H62B), C65(H65A,H65B),
  C51(H51A,H51B), C46(H46A,H46B), C50(H50A,H50B), C45(H45A,H45B), C64(H64A,
 H64B), C63(H63A,H63B)
6.c Aromatic/amide H refined with riding coordinates:
 N9(H9A), N12(H12A), N11(H11A), C24(H24), C57(H57), C32(H32), N10(H10A),
 C77(H77), C58(H58), C2(H2), N7(H7), C20(H20), C33(H33), C30(H30), C6(H6),
 C23(H23), C56(H56), C17(H17), C35(H35), C36(H36), C16(H16), C60(H60), C12(H12),
  C26(H26), C22(H22), C59(H59), C18(H18), C21(H21), C28(H28), C15(H15), N8(H8A),
  C3(H3), C29(H29), C27(H27), C11(H11), C4(H4), C34(H34), C9(H9), C14(H14),
 C5(H5), C8(H8), C38(H38), C42(H42), C10(H10), C40(H40), C39(H39), C41(H41),
 C80A(H80A), C80B(H80B)
6.d Idealised Me refined as rotating group:
 C76(H76A,H76B,H76C), C75(H75A,H75B,H75C), C79A(H79A,H79B,H79C), C78A(H78A,
 H78B,H78C), C79B(H79D,H79E,H79F), C78B(H78D,H78E,H78F)
;
_shelx_res_checksum              18621
_shelx_shelxl_version_number     2014/7
_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 1.652
_oxdiff_exptl_absorpt_empirical_full_min 0.676