Hydrothermal Assembly of a Novel Three-Dimensional Framework Formed by [GdMo12O42]9- Anions and Nine Coordinated GdIII Cations
Chuan-De Wu; Can-Zhong Lu; Hong-Hui Zhuang; Jin-Shun Huang; Journal of the American Chemical Society 124 (2002) 3836–3837; doi:10.1021/ja017782w

data_4114734
_publ_contact_author_address
; 
  The State Key Laboratory of Structural Chemistry,
  Fujian Institute of Research on the Structure of Matter,
  the Chinese Academy of Sciences, 
  Fuzhou, Fujian 350002, 
  P. R. China
;
_publ_contact_author_email       czlu@ms.fjirsm.ac.cn
_publ_contact_author_fax         86-591-3714946
_publ_contact_author_name        'Can-Zhong Lu'
_publ_contact_author_phone       86-591-3792865
_publ_section_title
;
 Hydrothermal Assembly of a Novel Three-Dimensional Framework Formed by
 [GdMo12O42]9- Anions and Nine Coordinated GdIII Cations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3836
_journal_page_last               3837
_journal_paper_doi               10.1021/ja017782w
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'Gd4 H24 Mo12 O60'
_chemical_formula_weight         2764.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   17.2627(5)
_cell_length_b                   17.2627(5)
_cell_length_c                   25.6138(8)
_cell_measurement_reflns_used    3761
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.09
_cell_volume                     6610.3(3)
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SMART & SAINT'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       'phi and omega 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  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6613
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    9.364
_exptl_absorpt_correction_T_max  0.6639
_exptl_absorpt_correction_T_min  0.5106
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    4.167
_exptl_crystal_description       Prism
_exptl_crystal_F_000             7584
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.970
_refine_diff_density_min         -3.144
_refine_diff_density_rms         0.345
_refine_ls_extinction_coef       0.000036(11)
_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   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0500P)^2^+808.1702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1209
_reflns_number_gt                1131
_reflns_number_total             1311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja017782w_s3.cif
_cod_data_source_block           JA017782w
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'H24 Gd4 Mo12 O60'
_cod_database_code               4114734
_refine_ls_r_factor_ref          0.0582