Novel configurational structures of sodium tetrakis(3-heptafluorobutylryl-(+)-camphorato) Ln(III) complexes with a trapped Na+ by Na+...FC interactions in the solid state and in solution.
Shirotani, Dai; Suzuki, Takayoshi; Kaizaki, Sumio; Inorganic chemistry 45 (2006) 6111–6113; doi:10.1021/ic0606633

data_4350339
_publ_section_title
;
 Novel configurational structures of sodium
 tetrakis(3-heptafluorobutylryl-(+)-camphorato) Ln(III) complexes with a
 trapped Na+ by Na+...FC interactions in the solid state and in solution.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6111
_journal_page_last               6113
_journal_paper_doi               10.1021/ic0606633
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C58 H59 F28 La N Na O8'
_chemical_formula_sum            'C58 H59 F28 La N Na O8'
_chemical_formula_weight         1591.96
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.187(6)
_cell_length_b                   24.286(5)
_cell_length_c                   13.220(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14.7
_cell_measurement_theta_min      13.3
_cell_volume                     6802(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    CrystalStructure
_computing_publication_material  ORTEP-3
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.4440
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8503
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.55
_diffrn_standards_interval_time  150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.9278
_exptl_absorpt_correction_T_min  0.8039
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   Coppens_numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.676
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         8503
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.3307
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1596
_reflns_number_gt                2488
_reflns_number_total             8503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic0606633si20060419_060155.cif
_cod_data_source_block           Lahfbc4
_cod_original_cell_volume        6803(3)
_cod_database_code               4350339