#------------------------------------------------------------------------------
#$Date: 2025-08-19 13:52:15 +0200 (Tue 19 de Aug de 2025) $
#$Revision: 301804 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/47/2214717.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2214717
loop_
_publ_author_name
'Guo, Hao'
'Zabawa, Mark'
'Woo, Joyce'
'Zheng, Chong'
'Yao, Qingwei'
_publ_section_title
(Z)-N-tert-Butyl-C-(2,3,4-trimethoxyphenyl)nitrone
_journal_coeditor_code           HJ3042
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3552
_journal_page_last               o3552
_journal_paper_doi               10.1107/S1600536807031674
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C14 H21 N O4'
_chemical_formula_moiety         'C14 H21 N O4'
_chemical_formula_sum            'C14 H21 N O4'
_chemical_formula_weight         267.32
_chemical_melting_point          .395E-305
_chemical_name_systematic
;
(Z)-N-tert-Butyl-C-(2,3,4-trimethoxyphenyl)nitrone
;
_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
_cell_angle_alpha                74.055(3)
_cell_angle_beta                 68.612(3)
_cell_angle_gamma                82.108(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7424(15)
_cell_length_b                   9.5039(17)
_cell_length_c                   9.8424(17)
_cell_measurement_reflns_used    427
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      -14
_cell_volume                     731.5(2)
_computing_cell_refinement       'SMART and SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Siemens SMART CCD PLATFORM'
_diffrn_measurement_method       ω
_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  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5580
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.9653
_exptl_absorpt_correction_T_min  0.8566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.172
_refine_ls_extinction_coef       0.024(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0678P)²+0.113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1236
_reflns_number_gt                2189
_reflns_number_total             2563
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hj3042.cif
_cod_data_source_block           I
_cod_database_code               2214717
_cod_database_fobs_code          2214717
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
O O1 0.75304(15) 1.17217(13) 0.34565(15) 0.0717(4) Uani d . 1
O O2 1.29356(14) 0.62646(12) 0.30972(13) 0.0647(3) Uani d . 1
O O3 1.09014(13) 0.54726(11) 0.20004(11) 0.0584(3) Uani d . 1
O O4 0.82513(12) 0.72922(12) 0.16273(12) 0.0610(3) Uani d . 1
N N1 0.70119(15) 1.11834(13) 0.26398(14) 0.0523(3) Uani d . 1
C C1 1.00430(18) 0.94615(16) 0.31636(17) 0.0518(4) Uani d . 1
H H1 0.9838 1.0337 0.3462 0.062 Uiso calc R 1
C C2 1.13649(18) 0.85577(16) 0.33577(17) 0.0532(4) Uani d . 1
H H2 1.2046 0.8837 0.3767 0.064 Uiso calc R 1
C C3 1.16811(17) 0.72379(16) 0.29453(16) 0.0496(4) Uani d . 1
C C4 1.06241(17) 0.68092(15) 0.23628(15) 0.0481(3) Uani d . 1
C C5 0.93260(17) 0.77314(16) 0.21437(15) 0.0481(3) Uani d . 1
C C6 0.90073(17) 0.90925(16) 0.25308(16) 0.0484(3) Uani d . 1
C C7 0.76466(18) 0.99913(17) 0.22132(17) 0.0526(4) Uani d . 1
H H7 0.7175 0.9683 0.1642 0.063 Uiso calc R 1
C C8 0.55423(19) 1.20292(18) 0.22727(18) 0.0600(4) Uani d . 1
C C9 0.5125(3) 1.1466(3) 0.1152(3) 0.0883(6) Uani d . 1
H H93 0.4750 1.0486 0.1604 0.132 Uiso calc R 1
H H92 0.6087 1.1466 0.0275 0.132 Uiso calc R 1
H H91 0.4275 1.2089 0.0867 0.132 Uiso calc R 1
C C10 0.4129(2) 1.1846(3) 0.3765(2) 0.0886(6) Uani d . 1
H H103 0.3178 1.2403 0.3611 0.133 Uiso calc R 1
H H102 0.4435 1.2190 0.4457 0.133 Uiso calc R 1
H H101 0.3880 1.0830 0.4170 0.133 Uiso calc R 1
C C11 0.6005(3) 1.3618(2) 0.1600(2) 0.0835(6) Uani d . 1
H H113 0.5067 1.4208 0.1458 0.125 Uiso calc R 1
H H112 0.6879 1.3701 0.0647 0.125 Uiso calc R 1
H H111 0.6363 1.3949 0.2268 0.125 Uiso calc R 1
C C12 1.4108(2) 0.6695(2) 0.3579(3) 0.0795(6) Uani d . 1
H H123 1.4613 0.7567 0.2879 0.119 Uiso calc R 1
H H122 1.4935 0.5924 0.3627 0.119 Uiso calc R 1
H H121 1.3569 0.6883 0.4557 0.119 Uiso calc R 1
C C13 1.0042(3) 0.43237(19) 0.3183(2) 0.0809(6) Uani d . 1
H H133 1.0439 0.4156 0.4007 0.121 Uiso calc R 1
H H132 1.0216 0.3447 0.2832 0.121 Uiso calc R 1
H H131 0.8889 0.4588 0.3514 0.121 Uiso calc R 1
C C14 0.8909(2) 0.7105(2) 0.0131(2) 0.0747(5) Uani d . 1
H H143 0.9072 0.8047 -0.0570 0.112 Uiso calc R 1
H H142 0.8155 0.6581 -0.0035 0.112 Uiso calc R 1
H H141 0.9942 0.6561 -0.0011 0.112 Uiso calc R 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
C3 O2 C12 117.46(13)
C4 O3 C13 113.76(12)
C5 O4 C14 116.22(12)
O1 N1 C7 122.97(12)
O1 N1 C8 114.34(12)
C7 N1 C8 122.64(13)
C2 C1 C6 121.58(13)
C2 C1 H1 119.2
C6 C1 H1 119.2
C1 C2 C3 120.34(13)
C1 C2 H2 119.8
C3 C2 H2 119.8
O2 C3 C2 125.16(13)
O2 C3 C4 115.39(13)
C2 C3 C4 119.42(13)
O3 C4 C5 120.53(13)
O3 C4 C3 119.60(13)
C5 C4 C3 119.87(13)
O4 C5 C4 120.03(12)
O4 C5 C6 118.53(13)
C4 C5 C6 121.32(13)
C1 C6 C5 117.41(13)
C1 C6 C7 125.82(13)
C5 C6 C7 116.77(13)
N1 C7 C6 126.98(14)
N1 C7 H7 116.5
C6 C7 H7 116.5
C11 C8 C9 109.38(16)
C11 C8 C10 111.50(16)
C9 C8 C10 111.30(17)
C11 C8 N1 106.89(14)
C9 C8 N1 111.94(14)
C10 C8 N1 105.73(13)
C8 C9 H93 109.5
C8 C9 H92 109.5
H93 C9 H92 109.5
C8 C9 H91 109.5
H93 C9 H91 109.5
H92 C9 H91 109.5
C8 C10 H103 109.5
C8 C10 H102 109.5
H103 C10 H102 109.5
C8 C10 H101 109.5
H103 C10 H101 109.5
H102 C10 H101 109.5
C8 C11 H113 109.5
C8 C11 H112 109.5
H113 C11 H112 109.5
C8 C11 H111 109.5
H113 C11 H111 109.5
H112 C11 H111 109.5
O2 C12 H123 109.5
O2 C12 H122 109.5
H123 C12 H122 109.5
O2 C12 H121 109.5
H123 C12 H121 109.5
H122 C12 H121 109.5
O3 C13 H133 109.5
O3 C13 H132 109.5
H133 C13 H132 109.5
O3 C13 H131 109.5
H133 C13 H131 109.5
H132 C13 H131 109.5
O4 C14 H143 109.5
O4 C14 H142 109.5
H143 C14 H142 109.5
O4 C14 H141 109.5
H143 C14 H141 109.5
H142 C14 H141 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 N1 1.2918(16)
O2 C3 1.3586(18)
O2 C12 1.421(2)
O3 C4 1.3788(17)
O3 C13 1.414(2)
O4 C5 1.3739(16)
O4 C14 1.425(2)
N1 C7 1.299(2)
N1 C8 1.5240(19)
C1 C2 1.381(2)
C1 C6 1.396(2)
C1 H1 0.9300
C2 C3 1.385(2)
C2 H2 0.9300
C3 C4 1.402(2)
C4 C5 1.380(2)
C5 C6 1.411(2)
C6 C7 1.445(2)
C7 H7 0.9300
C8 C11 1.518(3)
C8 C9 1.520(3)
C8 C10 1.520(2)
C9 H93 0.9600
C9 H92 0.9600
C9 H91 0.9600
C10 H103 0.9600
C10 H102 0.9600
C10 H101 0.9600
C11 H113 0.9600
C11 H112 0.9600
C11 H111 0.9600
C12 H123 0.9600
C12 H122 0.9600
C12 H121 0.9600
C13 H133 0.9600
C13 H132 0.9600
C13 H131 0.9600
C14 H143 0.9600
C14 H142 0.9600
C14 H141 0.9600
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21123868
2 PubChem 139072715
