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_4321442
_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     '[Nd(TMSA)4][CF3SO3]3'
_chemical_formula_sum            'C35 H64 F9 N8 Nd O17 S3'
_chemical_formula_weight         1280.36
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 90.45
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.6586(10)
_cell_length_b                   19.3078(7)
_cell_length_c                   11.1429(4)
_cell_measurement_reflns_used    4483
_cell_measurement_temperature    173(2)
_cell_volume                     5305.0(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\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  0.0709
_diffrn_reflns_av_sigmaI/netI    0.1109
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16832
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    1.200
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2620
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.234
_refine_diff_density_min         -2.335
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.00014(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   0.938
_refine_ls_goodness_of_fit_obs   0.970
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_restrained_S_obs      0.970
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_obs          0.0591
_refine_ls_shift/esd_max         0.375
_refine_ls_shift/esd_mean        0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      '0.0870, 0.0000'
_refine_ls_wR_factor_all         0.1643
_refine_ls_wR_factor_obs         0.1236
_reflns_number_observed          3763
_reflns_number_total             6195
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000244k_2.cif
_cod_data_source_block           compound2
_cod_database_code               4321442