New self-assembly hybrid compounds based on arsenic‒vanadium clusters and transition metal mixed-organic-ligand complexes
Guo, Hai-Yang; Li, Zhi-Fang; Zhang, Xiao; Fu, Li-Wei; Hu, Yang-Yang; Guo, Lan-Lan; Cui, Xiao-Bing; Huo, Qi-Sheng; Xu, Ji-Qing; CrystEngComm 18 (2016) 566–; doi:10.1039/C5CE01983D

data_7223457
_publ_section_title
;
 New self-assembly hybrid compounds based on arsenic--vanadium clusters
 and transition metal mixed-organic-ligand complexes
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              566
_journal_paper_doi               10.1039/C5CE01983D
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C46 H41 As8 N12 Ni2.5 O43 V14'
_chemical_formula_weight         2909.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-16 deposited with the CCDC.
2015-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.80109(15)
_cell_length_b                   23.8678(2)
_cell_length_c                   27.1204(2)
_cell_measurement_reflns_used    13245
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3080
_cell_measurement_theta_min      3.3410
_cell_volume                     8933.50(14)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            29903
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.073
_diffrn_reflns_theta_min         2.955
_exptl_absorpt_coefficient_mu    4.933
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71529
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.163
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             5604
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.751
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
 Flack x determined using 6734 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1162
_refine_ls_number_reflns         19099
_refine_ls_number_restraints     828
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0767P)^2^+14.8542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.708
_reflns_friedel_fraction_full    0.928
_reflns_friedel_fraction_max     0.720
_reflns_number_gt                17390
_reflns_number_total             19099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01983d2.cif
_cod_data_source_block           shelx_1a
_cod_depositor_comments
'Adding full bibliography for 7223456--7223462.cif.'
_cod_original_formula_sum        'C46 H41 As8 N12 Ni2.50 O43 V14'
_cod_database_code               7223457
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.372
_shelx_estimated_absorpt_t_max   0.525
_shelx_res_checksum              39996