Synthesis of highly hindered oxepins and an azepine from bis-trityl carbenium ions: structural characterisation by NMR and X-ray crystallography
Carey, Kieran A.; Clegg, William; Elsegood, Mark R. J.; Golding, Bernard T.; Stuart Hill, M. N.; Maskill, Howard; Journal of the Chemical Society, Perkin Transactions 1  (2002) 2673–; doi:10.1039/b207108h

data_7204498
_publ_section_title
;
 Synthesis of highly hindered oxepins and an azepine from bis-trityl
 carbenium ions: structural characterisation by NMR and X-ray
 crystallography
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2673
_journal_paper_doi               10.1039/b207108h
_journal_year                    2002
_chemical_formula_sum            'C42 H38 O6'
_chemical_formula_weight         638.72
_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   'all non-H atoms found by direct methods'
_audit_creation_method           SHELXL
_cell_angle_alpha                74.83(3)
_cell_angle_beta                 71.95(2)
_cell_angle_gamma                85.00(2)
_cell_formula_units_Z            2
_cell_length_a                   10.162(4)
_cell_length_b                   12.856(5)
_cell_length_c                   13.729(5)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      12.48
_cell_measurement_theta_min      10.11
_cell_volume                     1645.9(11)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Stoe-Siemens diffractometer'
_diffrn_measurement_method       '\w/\q scans with on-line profile fitting'
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7044
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        -1
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0046(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.016
_refine_ls_goodness_of_fit_obs   1.029
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         5799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_restrained_S_obs      1.029
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_obs          0.0455
_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^)+(0.0319P)^2^+1.0784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1184
_refine_ls_wR_factor_obs         0.1057
_reflns_number_observed          4597
_reflns_number_total             5799
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b207108h.txt
_cod_data_source_block           hm5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+1.0784P] 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^)+(0.0319P)^2^+1.0784P] 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-1
_cod_database_code               7204498