Highly electrophilic lanthanide complexes containing fluorinated amido ligands: multiple Ln···F interactions, agostic interactions and η6-arene coordination
Click, Damon R.; Scott, Brian L.; Watkin, John G.; Chemical Communications  (1999) 633–; doi:10.1039/a809275c

data_7110424
_publ_section_title
;
 Highly electrophilic lanthanide complexes containing fluorinated amido
 ligands: multiple Ln&#x00B7;&#x00B7;&#x00B7;F interactions, agostic
 interactions and \h6-arene coordination
;
_journal_issue                   7
_journal_name_full               'Chemical Communications'
_journal_page_first              633
_journal_paper_doi               10.1039/a809275c
_journal_year                    1999
_chemical_formula_sum            'C50 H16 F30 N3 Nd'
_chemical_formula_weight         1372.90
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.47(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.964(4)
_cell_length_b                   8.712(2)
_cell_length_c                   24.927(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    198
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      11.0
_cell_volume                     4756.9(16)
_computing_cell_refinement       'XSCANS 2.10b (Siemens, 1994)'
_computing_data_collection       'XSCANS 2.10b (Siemens, 1994)'
_computing_data_reduction        'XSCANS 2.10b (Siemens, 1994)'
_computing_molecular_graphics    'SHELXTL PC 4.2/360 (Siemens, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198
_diffrn_measurement_device       'Siemens P4/PC'
_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  0.0626
_diffrn_reflns_av_sigmaI/netI    0.1113
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7834
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             2668
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.062
_refine_ls_goodness_of_fit_obs   1.152
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         6213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_restrained_S_obs      1.152
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_obs          0.0577
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1252
_refine_ls_wR_factor_obs         0.1015
_reflns_number_observed          3827
_reflns_number_total             6217
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809275csup1.cif
_cod_data_source_block           xr130
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7110424