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_7201040
_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            'C27 H70 Ge Mo12 N11 Ni4 O47'
_chemical_formula_weight         2759.58
_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                112.528(3)
_cell_angle_beta                 106.237(3)
_cell_angle_gamma                97.703(2)
_cell_formula_units_Z            2
_cell_length_a                   14.544(2)
_cell_length_b                   15.039(3)
_cell_length_c                   18.655(3)
_cell_measurement_reflns_used    5466
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.80
_cell_volume                     3482.3(10)
_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      273(2)
_diffrn_detector_area_resol_mean 'not measured'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0697
_diffrn_reflns_av_sigmaI/netI    0.1094
_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       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30123
_diffrn_reflns_theta_full        26.09
_diffrn_reflns_theta_max         26.09
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    3.658
_exptl_absorpt_correction_T_max  0.608
_exptl_absorpt_correction_T_min  0.567
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    2.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2618
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.746
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         13645
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1551
_reflns_number_gt                8561
_reflns_number_total             13645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903793d.txt
_cod_data_source_block           1
_cod_original_cell_volume        3482.2(16)
_cod_database_code               7201040