N-Tritylhydroxylamines: preparations, structures, base strengths, and reactions with nitrous acid and perchloric acid
Moisés Canle L.; William Clegg; Ibrahim Demirtas; Mark R. J. Elsegood; Johanna Haider; Howard Maskill; Peter C. Miatt; J. Chem. Soc., Perkin Trans. 2  (2001) 1742–1747; doi:10.1039/b103569j

data_7204157
_publ_section_title
;
 N-Tritylhydroxylamines: preparations, structures, base strengths, and
 reactions with nitrous acid and perchloric acid
;
_journal_issue                   9
_journal_name_full               'J. Chem. Soc., Perkin Trans. 2'
_journal_page_first              1742
_journal_page_last               1747
_journal_paper_doi               10.1039/b103569j
_journal_year                    2001
_chemical_formula_sum            'C38 H31 N O'
_chemical_formula_weight         517.64
_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 except H1 coords freely refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                113.29(4)
_cell_angle_beta                 90.24(4)
_cell_angle_gamma                115.20(3)
_cell_formula_units_Z            1
_cell_length_a                   8.677(6)
_cell_length_b                   9.042(6)
_cell_length_c                   10.769(7)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      24.60
_cell_measurement_theta_min      20.06
_cell_volume                     686.9(9)
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4757
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         4.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       'triangular prism'
_exptl_crystal_F_000             274
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.154
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.0145(9)
_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   1.070
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2409
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_obs          0.0370
_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^)+(0.0257P)^2^+0.2022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0947
_refine_ls_wR_factor_obs         0.0885
_reflns_number_observed          2074
_reflns_number_total             2409
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b103569j.txt
_cod_data_source_block           hm8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.2022P] 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^)+(0.0257P)^2^+0.2022P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        686.9(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204157