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_4321446
_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(CF3SO3)3(TMSA)3(OH2)]'
_chemical_formula_sum            'C27 H50 F9 N6 O16 S3 Yb'
_chemical_formula_weight         1154.95
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.2640(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9443(3)
_cell_length_b                   11.1924(4)
_cell_length_c                   44.2517(13)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_volume                     4422.8(3)
_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_device       'SIEMENS SMART CDD / area detector '
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            27229
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    2.364
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       frag
_exptl_crystal_F_000             2324
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.882
_refine_diff_density_min         -2.636
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.00040(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_all   1.178
_refine_ls_goodness_of_fit_obs   1.204
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     571
_refine_ls_number_reflns         10292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_restrained_S_obs      1.204
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_obs          0.0514
_refine_ls_shift/esd_max         3.411
_refine_ls_shift/esd_mean        0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1157
_refine_ls_wR_factor_obs         0.1093
_reflns_number_observed          9078
_reflns_number_total             10297
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000244k_6.cif
_cod_data_source_block           compound6
_cod_database_code               4321446