#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:04:46 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180372 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/41/7204157.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7204157
loop_
_publ_author_name
'Moisés Canle L.'
'William Clegg'
'Ibrahim Demirtas'
'Mark R. J. Elsegood'
'Johanna Haider'
'Howard Maskill'
'Peter C. Miatt'
_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
_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 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       'ω/θ 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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0257P)²+0.2022P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
N1_a N 0.41604(13) 0.41996(13) 0.47468(12) 0.0300(3) Uani 0.50 d PD 1
H1_a H 0.344(4) 0.455(5) 0.516(4) 0.045 Uiso 0.50 d PD 1
O1_b O 0.41604(13) 0.41996(13) 0.47468(12) 0.0300(3) Uani 0.50 d P 2
C1 C 0.34475(16) 0.37154(17) 0.33209(14) 0.0224(3) Uani 1 d . .
C2 C 0.17401(16) 0.19470(17) 0.29424(14) 0.0228(3) Uani 1 d . .
C3 C 0.0709(2) 0.1759(2) 0.39102(17) 0.0357(4) Uani 1 d . .
H3 H 0.1063 0.2728 0.4813 0.043 Uiso 1 calc R .
C4 C -0.0832(2) 0.0168(2) 0.35717(18) 0.0394(4) Uani 1 d . .
H4 H -0.1521 0.0058 0.4245 0.047 Uiso 1 calc R .
C5 C -0.13663(18) -0.1247(2) 0.22664(18) 0.0354(4) Uani 1 d . .
H5 H -0.2417 -0.2335 0.2038 0.043 Uiso 1 calc R .
C6 C -0.03688(18) -0.10755(19) 0.12961(17) 0.0327(4) Uani 1 d . .
H6 H -0.0735 -0.2046 0.0393 0.039 Uiso 1 calc R .
C7 C 0.11785(17) 0.05155(18) 0.16302(15) 0.0266(3) Uani 1 d . .
H7 H 0.1856 0.0620 0.0950 0.032 Uiso 1 calc R .
C8 C 0.46990(16) 0.33176(16) 0.24073(15) 0.0253(3) Uani 1 d . .
C9 C 0.48733(18) 0.36352(18) 0.12418(16) 0.0304(3) Uani 1 d . .
H9 H 0.4249 0.4178 0.1027 0.036 Uiso 1 calc R .
C10 C 0.5949(2) 0.3170(2) 0.03863(19) 0.0408(4) Uani 1 d . .
H10 H 0.6060 0.3403 -0.0404 0.049 Uiso 1 calc R .
C11 C 0.6853(2) 0.2373(2) 0.0680(2) 0.0473(5) Uani 1 d . .
H11 H 0.7595 0.2064 0.0099 0.057 Uiso 1 calc R .
C12 C 0.66759(19) 0.2025(2) 0.1823(2) 0.0464(5) Uani 1 d . .
H12 H 0.7287 0.1461 0.2022 0.056 Uiso 1 calc R .
C13 C 0.56093(18) 0.24942(19) 0.26841(19) 0.0353(4) Uani 1 d . .
H13 H 0.5499 0.2252 0.3470 0.042 Uiso 1 calc R .
C14 C 0.30965(16) 0.52119(17) 0.32392(14) 0.0224(3) Uani 1 d . .
C15 C 0.14238(18) 0.49515(19) 0.29152(17) 0.0325(4) Uani 1 d . .
H15 H 0.0457 0.3821 0.2744 0.039 Uiso 1 calc R .
C16 C 0.1135(2) 0.6315(2) 0.28366(19) 0.0404(4) Uani 1 d . .
H16 H -0.0021 0.6108 0.2614 0.048 Uiso 1 calc R .
C17 C 0.2524(2) 0.7970(2) 0.30804(17) 0.0353(4) Uani 1 d . .
H17 H 0.2330 0.8903 0.3028 0.042 Uiso 1 calc R .
C18 C 0.41921(19) 0.82461(19) 0.34008(16) 0.0309(3) Uani 1 d . .
H18 H 0.5152 0.9382 0.3574 0.037 Uiso 1 calc R .
C19 C 0.44895(18) 0.68933(18) 0.34738(15) 0.0275(3) Uani 1 d . .
H19 H 0.5651 0.7106 0.3685 0.033 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1_a N1_a C1 110.25(13) 2_666 . ?
N1_a C1 C8 108.67(12) . . ?
N1_a C1 C14 111.61(11) . . ?
C8 C1 C14 112.19(11) . . ?
N1_a C1 C2 102.55(11) . . ?
C8 C1 C2 109.94(12) . . ?
C14 C1 C2 111.43(11) . . ?
C7 C2 C3 118.17(13) . . ?
C7 C2 C1 121.21(13) . . ?
C3 C2 C1 120.61(13) . . ?
C2 C3 C4 120.77(15) . . ?
C5 C4 C3 120.35(16) . . ?
C6 C5 C4 119.54(14) . . ?
C5 C6 C7 120.35(15) . . ?
C2 C7 C6 120.81(14) . . ?
C9 C8 C13 118.26(14) . . ?
C9 C8 C1 122.00(12) . . ?
C13 C8 C1 119.59(14) . . ?
C8 C9 C10 120.89(14) . . ?
C11 C10 C9 120.22(17) . . ?
C10 C11 C12 119.63(16) . . ?
C11 C12 C13 120.36(15) . . ?
C12 C13 C8 120.64(16) . . ?
C15 C14 C19 117.68(13) . . ?
C15 C14 C1 122.14(12) . . ?
C19 C14 C1 120.17(12) . . ?
C14 C15 C16 121.24(13) . . ?
C17 C16 C15 120.32(15) . . ?
C18 C17 C16 119.07(14) . . ?
C17 C18 C19 120.94(13) . . ?
C18 C19 C14 120.74(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1_a N1_a 1.445(2) 2_666 ?
N1_a C1 1.470(2) . ?
C1 C8 1.529(2) . ?
C1 C14 1.5416(19) . ?
C1 C2 1.543(2) . ?
C2 C7 1.386(2) . ?
C2 C3 1.390(2) . ?
C3 C4 1.391(2) . ?
C4 C5 1.377(3) . ?
C5 C6 1.373(2) . ?
C6 C7 1.394(2) . ?
C8 C9 1.389(2) . ?
C8 C13 1.393(2) . ?
C9 C10 1.390(2) . ?
C10 C11 1.377(3) . ?
C11 C12 1.380(3) . ?
C12 C13 1.388(2) . ?
C14 C15 1.387(2) . ?
C14 C19 1.402(2) . ?
C15 C16 1.391(2) . ?
C16 C17 1.382(2) . ?
C17 C18 1.377(2) . ?
C18 C19 1.383(2) . ?
