Trifluoromethyl derivatives of pentacyclo[5.4.0.0^2,6^.0^3,10^.0^5,9^]undecane
Linden, Anthony; Romański, Jarosław; Mlostoń, Grzegorz; Heimgartner, Heinz; Acta Crystallographica Section C 61 (2005) o221–o226; doi:10.1107/S0108270105004701

data_2014885
_publ_section_title
;
 Trifluoromethyl derivatives of
 pentacyclo[5.4.0.0^2,6^.0^3,10^.0^5,9^]undecane
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o221
_journal_page_last               o226
_journal_paper_doi               10.1107/S0108270105004701
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C21 H24 F3 N O Si, C H4 O'
_chemical_formula_moiety         'C21 H24 F3 N O Si, C H4 O'
_chemical_formula_sum            'C22 H28 F3 N O2 Si'
_chemical_formula_weight         423.54
_chemical_melting_point          414
_chemical_name_systematic
;
N-phenyl-[exo-11-(trifluoromethyl)-endo-11-
(trimethylsilyloxy)pentacyclo[5.4.0.0^2,6^.0^3,10^.0^5,9^]undecan-
8-yliden]amine methanol solvate
;
_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-97
_cell_angle_alpha                100.2675(15)
_cell_angle_beta                 91.417(2)
_cell_angle_gamma                94.652(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8352(2)
_cell_length_b                   9.3775(3)
_cell_length_c                   12.6843(5)
_cell_measurement_reflns_used    5859
_cell_measurement_temperature    160.0(10)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.0
_cell_volume                     1029.86(6)
_computing_cell_refinement       'DENZO--SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO--SMN and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      160.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scans with \k offsets'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'Nonius FR590 sealed tube generator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26283
_diffrn_reflns_theta_full        30.11
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         3.32
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.312
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         6017
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.054P)^2^+0.529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                4581
_reflns_number_total             6025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk1816.cif
_cod_data_source_block           VII
_cod_original_sg_symbol_H-M      'P -1         '
_cod_database_code               2014885
_cod_database_fobs_code          2014885