The first ε-Keggin core of molybdogermanate in extended architectures of nickel(II) with N-donor ligands: syntheses, crystal structures and magnetic properties
Wang, Wenju; Xu, Lin; Gao, Guanggang; Liu, Li; Liu, Xizheng; CrystEngComm 11 (2009) 2488–; doi:10.1039/b903793d

data_7201041
_publ_section_title
;
 The first \e-Keggin core of molybdogermanate in extended architectures
 of nickel(II) with N-donor ligands: syntheses, crystal structures and
 magnetic properties
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              2488
_journal_paper_doi               10.1039/b903793d
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C30 H66 Ge Mo12 N11 Ni4 O42'
_chemical_formula_weight         2711.59
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.472(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.910(6)
_cell_length_b                   15.219(3)
_cell_length_c                   26.760(5)
_cell_measurement_reflns_used    8776
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.8
_cell_volume                     13430(4)
_computing_cell_refinement       'SMART (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 'not measured'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART CCD APEX II'
_diffrn_measurement_method       '\w and \f'
_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  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            36144
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    3.790
_exptl_absorpt_correction_T_max  0.640
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    2.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10032
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.038
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         12742
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+163.7583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1319
_reflns_number_gt                9326
_reflns_number_total             12742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903793d.txt
_cod_data_source_block           123
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C30 H66 Ge Mo12 N11 Ni4 O42 '
_cod_database_code               7201041