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_4321444
_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     '[Eu(TMSA)~4~][ClO~4~]~3~'
_chemical_formula_sum            'C32 H64 Cl3 Eu N8 O20'
_chemical_formula_weight         1139.22
_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                106.594(1)
_cell_angle_beta                 91.538(1)
_cell_angle_gamma                90.311(1)
_cell_formula_units_Z            2
_cell_length_a                   10.9611(2)
_cell_length_b                   14.6144(3)
_cell_length_c                   15.7992(2)
_cell_measurement_reflns_used    6145
_cell_measurement_temperature    173(2)
_cell_volume                     2424.37(7)
_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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15331
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    1.538
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.56
_refine_diff_density_max         1.332
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.0008(2)
_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   0.992
_refine_ls_goodness_of_fit_obs   1.036
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         10711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_restrained_S_obs      1.036
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_obs          0.0450
_refine_ls_shift/esd_max         0.614
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      '0.0500, 0.0000'
_refine_ls_wR_factor_all         0.1137
_refine_ls_wR_factor_obs         0.0935
_reflns_number_observed          8102
_reflns_number_total             10718
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000244k_4.cif
_cod_data_source_block           compound4
_cod_database_code               4321444