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_4321448
_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)2(H2O)3][CF3SO3]3'
_chemical_formula_sum            'C19 H38 F9 N4 O16 S3 Yb'
_chemical_formula_weight         1018.75
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                75.8150(1)
_cell_angle_beta                 86.805(1)
_cell_angle_gamma                72.6070(1)
_cell_formula_units_Z            2
_cell_length_a                   8.67190(1)
_cell_length_b                   12.2683(2)
_cell_length_c                   19.8094(3)
_cell_measurement_reflns_used    7693
_cell_measurement_temperature    173(2)
_cell_volume                     1949.48(4)
_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  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8898
_diffrn_reflns_theta_max         23.40
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    2.667
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_description       needle
_exptl_crystal_F_000             1014
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.30
_refine_diff_density_max         4.001
_refine_diff_density_min         -3.078
_refine_diff_density_rms         0.252
_refine_ls_extinction_coef       0.0054(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_goodness_of_fit_obs   1.175
_refine_ls_matrix_type           full
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_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_obs          0.0843
_refine_ls_shift/esd_max         0.064
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      '0.0793, 62.2301'
_refine_ls_wR_factor_all         0.2237
_refine_ls_wR_factor_obs         0.2142
_reflns_number_observed          5371
_reflns_number_total             5609
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000244k_8.cif
_cod_data_source_block           compound8
_cod_original_cell_volume        1949.48(5)
_cod_database_code               4321448