Coordination of Lanthanide Triflates and Perchlorates with N,N,N',N'-Tetramethylsuccinamide
Brian M. Rapko; Bruce K. McNamara; Robin D. Rogers; Grant A. Broker; Gregg J. Lumetta; Benjamin P. Hay; Inorganic Chemistry 39 (2000) 4858–4867; doi:10.1021/ic000244k

data_4321447
_publ_section_title
;
 Coordination of Lanthanide Triflates and Perchlorates with
 N,N,N',N'-Tetramethylsuccinamide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4858
_journal_page_last               4867
_journal_paper_doi               10.1021/ic000244k
_journal_volume                  39
_journal_year                    2000
_chemical_formula_structural     '[Yb(TMSA)3(H2O)][ClO4]3'
_chemical_formula_sum            'C24 H50 Cl3 N6 O19 Yb'
_chemical_formula_weight         1006.09
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 111.4260(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.2312(6)
_cell_length_b                   11.1552(3)
_cell_length_c                   19.8016(4)
_cell_measurement_reflns_used    3931
_cell_measurement_temperature    173(2)
_cell_volume                     3954.42(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4072
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    2.648
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.50
_refine_diff_density_max         2.642
_refine_diff_density_min         -1.786
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_coef       0.00000(9)
_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_all   1.122
_refine_ls_goodness_of_fit_obs   1.123
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
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_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.149
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_obs          0.0393
_refine_ls_shift/esd_max         -1.323
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      '0.0625, 48.6402'
_refine_ls_wR_factor_all         0.1067
_refine_ls_wR_factor_obs         0.1036
_reflns_number_observed          2642
_reflns_number_total             2668
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000244k_7.cif
_cod_data_source_block           compound7
_cod_original_cell_volume        3954.4(2)
_cod_database_code               4321447