3-D Germanate Constructed with Ge7 Cluster Layers and Nickel-Ethanolamine Linkage
Wen Luo; Wen-Qin Mu; Xu Zhang; Xiang Zhang; Ya-Yang Pu; Qin-Yu Zhu; Jie Dai; Inorganic Chemistry 51 (2012) 1489–1494; doi:10.1021/ic201754z

data_4328148
_publ_section_title
;
 3-D Germanate Constructed with Ge7 Cluster Layers and Nickel-Ethanolamine
 Linkage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1489
_journal_page_last               1494
_journal_paper_doi               10.1021/ic201754z
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C8 H27 Ge7 N3 Ni O19'
_chemical_formula_weight         1036.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5087(15)
_cell_length_b                   9.8707(11)
_cell_length_c                   16.4722(14)
_cell_measurement_reflns_used    7662
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     2684.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18274
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    8.081
_exptl_absorpt_correction_T_max  0.4988
_exptl_absorpt_correction_T_min  0.2948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication '
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    2.562
_exptl_crystal_description       Block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.788
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.198
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         4946
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+5.3782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1158
_reflns_number_gt                4671
_reflns_number_total             4946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201754z_si_002.cif
_cod_data_source_block           l
_cod_original_sg_symbol_Hall     'P 2c -2ac  '
_cod_original_sg_symbol_H-M      'P c a 21 '
_cod_database_code               4328148