Lanthanide-Transition Heterometallic Extended Structures with Novel Orthogonal Metalloligand as Building Block
Zheng He; Cheng He; En-Qing Gao; Zhe-Ming Wang; Xiao-Fan Yang; Chun-Sheng Liao; Chun-Hua Yan; Inorganic Chemistry 42 (2003) 2206–2208; doi:10.1021/ic026271n

data_4313439
_publ_contact_author_address
;
State Key Lab of Rare Earth Materials Chemistry and Applications & 
PKU-HKU Joint Lab on Rare Earth Materials and Bioinorganic Chemistry, 
College of Chemistry and Molecular Engineering, 
Peking University, 
Beijing 100871, 
China
;
_publ_contact_author_email       chyan@chem.pku.edu.cn
_publ_contact_author_fax         86-(10)-62754179
_publ_contact_author_name        'Prof. Chun-Hua Yan'
_publ_contact_author_phone       86-(10)-62754179
_publ_section_title
;
 Lanthanide-Transition Heterometallic Extended Structures with Novel
 Orthogonal Metalloligand as Building Block
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2206
_journal_page_last               2208
_journal_paper_doi               10.1021/ic026271n
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C35 H40.5 Cl2 Gd0.5 N12 Ni O15'
_chemical_formula_weight         1077.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 92.781(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7063(4)
_cell_length_b                   12.4103(4)
_cell_length_c                   30.2541(8)
_cell_measurement_reflns_used    46208
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      3.40
_cell_volume                     5140.1(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'NONIUS KappaCCD Diffractometer'
_diffrn_measurement_method       CCD
_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  0.0708
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            44981
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    1.185
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            'brownish red'
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2194
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.244
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.0036(7)
_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   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         11631
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0814
_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^)+(0.1227P)^2^+14.3446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2173
_refine_ls_wR_factor_ref         0.2470
_reflns_number_gt                8145
_reflns_number_total             11631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026271nsi20021215_043713_3.cif
_cod_data_source_block           GdNi
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_original_formula_sum        'C35 H40.50 Cl2 Gd0.50 N12 Ni O15'
_cod_database_code               4313439