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_7110423
_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            'C32 H35 F15 N3 O3.5 Sm'
_chemical_formula_weight         952.98
_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   mixed
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                98.42(1)
_cell_angle_beta                 95.81(1)
_cell_angle_gamma                114.02(1)
_cell_formula_units_Z            2
_cell_length_a                   10.745(1)
_cell_length_b                   10.773(1)
_cell_length_c                   18.216(2)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    203
_cell_measurement_theta_max      13
_cell_measurement_theta_min      12
_cell_volume                     1874.8(4)
_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_publication_material  'SHELXTL PC 4.2/360 (Siemens, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7673
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.679
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             946
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.492
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.109
_refine_ls_goodness_of_fit_obs   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         6535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_restrained_S_obs      1.131
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_obs          0.0404
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+3.1239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1218
_refine_ls_wR_factor_obs         0.1165
_reflns_number_observed          5796
_reflns_number_total             6535
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809275csup1.cif
_cod_data_source_block           xr120
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+3.1239P] 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^)+(0.0664P)^2^+3.1239P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1874.8(3)
_cod_original_formula_sum        'C32 H35 F15 N3 O3.50 Sm'
_cod_database_code               7110423