Expansion of Antimonato Polyoxovanadates with Transition Metal Complexes: (Co(N3C5H15)2)2[{Co(N3C5H15)2}V15Sb6O42(H2O)].5H2O and (Ni(N3C5H15)2)2[{Ni(N3C5H15)2}V15Sb6O42(H2O)].8H2O
Elena Antonova; Christian Näther; Paul Kögerler; Wolfgang Bensch; Inorganic Chemistry 51 (2012) 2311–2317; doi:10.1021/ic2023117

data_4328373
_publ_section_title
;
 Expansion of Antimonato Polyoxovanadates with Transition Metal Complexes:
 (Co(N3C5H15)2)2[{Co(N3C5H15)2}V15Sb6O42(H2O)].5H2O and
 (Ni(N3C5H15)2)2[{Ni(N3C5H15)2}V15Sb6O42(H2O)].8H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2311
_journal_page_last               2317
_journal_paper_doi               10.1021/ic2023117
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'C10 H30 N6 Ni O42 Sb6 V15,2(C10 H30 N6 Ni), 8(O)'
_chemical_formula_sum            'C30 H90 N18 Ni3 O50 Sb6 V15'
_chemical_formula_weight         3173.9300
_chemical_name_common            (Ni(AEPA)2)2((Ni(AEPA)2)V15Sb6O42(H2O))
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                86.702(11)
_cell_angle_beta                 84.957(11)
_cell_angle_gamma                76.941(11)
_cell_formula_units_Z            2
_cell_length_a                   14.5697(13)
_cell_length_b                   15.8523(16)
_cell_length_c                   20.2411(18)
_cell_measurement_reflns_used    35831
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      2.02
_cell_volume                     4533.0(8)
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_collection       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35831
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.919
_exptl_absorpt_correction_T_max  0.763
_exptl_absorpt_correction_T_min  0.604
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.339
_exptl_crystal_F_000             3098
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
;
_refine_diff_density_max         1.486
_refine_diff_density_min         -1.930
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       0.00045(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1121
_refine_ls_number_reflns         15034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                11716
_reflns_number_total             15034
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2023117_si_002.cif
_cod_data_source_block           ea624
_cod_original_cell_volume        4533.0(7)
_cod_database_code               4328373