[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_7119520
_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), H2 O'
_chemical_formula_sum            'C74 H92 Mo3 N12 O15 V4'
_chemical_formula_weight         1881.17
_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   mixed
_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                104.468(2)
_cell_angle_beta                 96.532(2)
_cell_angle_gamma                104.992(3)
_cell_formula_units_Z            2
_cell_length_a                   12.4632(4)
_cell_length_b                   14.0872(4)
_cell_length_c                   26.2550(8)
_cell_measurement_reflns_used    17814
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.590
_cell_measurement_theta_min      4.300
_cell_volume                     4232.4(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_temperature      173.00(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1566
_diffrn_reflns_av_unetI/netI     0.1433
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            30037
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.590
_diffrn_reflns_theta_min         3.542
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.615
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44300
_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    1.476
_exptl_crystal_description       rod
_exptl_crystal_F_000             1916
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.572
_refine_diff_density_min         -3.009
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         17221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0918
_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^)+(0.1710P)^2^+1.9106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2376
_refine_ls_wR_factor_ref         0.2609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13598
_reflns_number_total             17221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc00166e2.cif
_cod_data_source_block           mo3v4-G-H2O
_cod_depositor_comments
'Adding full bibliography for 7119518--7119521.cif.'
_cod_database_code               7119520
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O12) = Uanis(O1)
Uanis(O12) = Uanis(O15)
Uanis(N1) = Uanis(N2)
Uanis(C15) = Uanis(C16) = Uanis(C17)
Uanis(C14) = Uanis(C18)
Uanis(C12) = Uanis(C8)
Uanis(C11) = Uanis(C9)
Uanis(C18) = Uanis(C17) = Uanis(C16) = Uanis(C15)
3.a Free rotating group:
 O15(H15A,H15B)
3.b Ternary CH refined with riding coordinates:
 C43(H43), C67(H67), C49(H49), C61(H61)
3.c Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C62(H62A,H62B), C44(H44A,H44B), C45(H45A,H45B), C63(H63A,
 H63B), C47(H47A,H47B), C64(H64A,H64B), C66(H66A,H66B), C65(H65A,H65B),
 C46(H46A,H46B), C68(H68A,H68B), C72(H72A,H72B), C50(H50A,H50B), C54(H54A,H54B),
  C69(H69A,H69B), C71(H71A,H71B), C70(H70A,H70B), C53(H53A,H53B), C52(H52A,
 H52B), C51(H51A,H51B)
3.d Aromatic/amide H refined with riding coordinates:
 N9(H9A), N7(H7), N8(H8A), N11(H11A), N10(H10A), N12(H12A), C20(H20), C42(H42),
  C24(H24), C41(H41), C6(H6), C30(H30), C2(H2), C38(H38), C23(H23), C36(H36),
 C40(H40), C4(H4), C26(H26), C12(H12), C21(H21), C27(H27), C39(H39), C14(H14),
 C29(H29), C22(H22), C28(H28), C35(H35), C5(H5), C8(H8), C32(H32), C34(H34),
 C60(H60), C56(H56), C11(H11), C58(H58), C3(H3), C33(H33), C59(H59), C10(H10),
 C57(H57), C9(H9), C18(H18), C15(H15), C16(H16), C17(H17)
;
_shelx_res_checksum              55015
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'