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_7110425
_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            'C27 H27 F15 N3 Si3 Sm'
_chemical_formula_weight         913.14
_chemical_name_systematic
; 
 ? 
;
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                94.96(1)
_cell_angle_beta                 107.33(1)
_cell_angle_gamma                95.26(1)
_cell_formula_units_Z            2
_cell_length_a                   10.196(4)
_cell_length_b                   10.868(4)
_cell_length_c                   16.461(7)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    198
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      11.5
_cell_volume                     1721.4(12)
_computing_cell_refinement       'XSCANS 2.10b (Siemens)'
_computing_data_collection       'XSCANS 2.10b (Siemens)'
_computing_data_reduction        'XSCANS 2.10b (Siemens)'
_computing_molecular_graphics    'SHELXTL PC 4.2/360 (Siemens)'
_computing_publication_material  'SHELXTL PC 4.2/360 (Siemens)'
_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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5381
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.916
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'irregular plate'
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.378
_refine_diff_density_min         -2.026
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.067
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         4476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_obs          0.0564
_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^)+(0.0911P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1528
_refine_ls_wR_factor_obs         0.1359
_reflns_number_observed          3514
_reflns_number_total             4479
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809275csup1.cif
_cod_data_source_block           xr181
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0911P)^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^)+(0.0911P)^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_database_code               7110425