Seven-Coordinate Lanthanide Sandwich-Type Complexes with a Tetrathiafulvalene-Fused Schiff Base Ligand
Feng Gao; Long Cui; Wei Liu; Liang Hu; Yu-Wu Zhong; Yi-Zhi Li; Jing-Lin Zuo; Inorganic Chemistry 52 (2013) 11164–11172; doi:10.1021/ic401421h

data_4336195
_publ_section_title
;
 Seven-Coordinate Lanthanide Sandwich-Type Complexes with a
 Tetrathiafulvalene-Fused Schiff Base Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11164
_journal_page_last               11172
_journal_paper_doi               10.1021/ic401421h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C43 H51.5 Cl2 Co N2 O11.25 P3 S6 Tb'
_chemical_formula_weight         1350.38
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.300(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8268(17)
_cell_length_b                   19.9048(16)
_cell_length_c                   20.3778(17)
_cell_measurement_reflns_used    6782
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      21.24
_cell_measurement_theta_min      2.22
_cell_volume                     5800.8(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0124
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37116
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    1.939
_exptl_absorpt_correction_T_max  0.6862
_exptl_absorpt_correction_T_min  0.6226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       block
_exptl_crystal_F_000             2722
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.670
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         11272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0550P)^2^+1.2200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                8297
_reflns_number_total             11272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401421h_si_002_2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C43 H51.50 Cl2 Co N2 O11.25 P3 S6 Tb'
_cod_database_code               4336195