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_4336194
_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 Dy N2 O11.25 P3 S6'
_chemical_formula_weight         1353.96
_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                 105.086(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9211(15)
_cell_length_b                   19.9947(14)
_cell_length_c                   19.9744(14)
_cell_measurement_reflns_used    4279
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      20.30
_cell_measurement_theta_min      2.22
_cell_volume                     5753.8(8)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0824
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34714
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    2.024
_exptl_absorpt_correction_T_max  0.6644
_exptl_absorpt_correction_T_min  0.6010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       block
_exptl_crystal_F_000             2726
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.624
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         11327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0700P)^2^+1.9900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1506
_reflns_number_gt                7348
_reflns_number_total             11327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401421h_si_002_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C43 H51.50 Cl2 Co Dy N2 O11.25 P3 S6'
_cod_database_code               4336194