#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/41/7204199.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_7204199
loop_
_publ_author_name
'Abdullah G. Al-Sehemi'
'Robert S. Atkinson'
'John Fawcett'
_publ_section_title
;
 Kinetic resolution of amines with enantiopure
 3-N,N-diacylaminoquinazolin-4(3H)-ones
;
_journal_issue                   2
_journal_name_full               'J. Chem. Soc., Perkin Trans. 1'
_journal_page_first              257
_journal_page_last               274
_journal_paper_doi               10.1039/b105917n
_journal_year                    2002
_chemical_formula_sum            'C31 H29 N3 O7'
_chemical_formula_weight         555.57
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.315(3)
_cell_length_b                   14.210(2)
_cell_length_c                   17.368(5)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      12.45
_cell_measurement_theta_min      5.40
_cell_volume                     2792.5(12)
_computing_cell_refinement       'XSCANS (Fait, 1991)'
_computing_data_collection       'XSCANS (Fait, 1991)'
_computing_data_reduction        'XSCANS (Fait, 1991)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4 diffractometer'
_diffrn_measurement_method       'omega scan'
_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  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3891
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.9(19)
_refine_ls_extinction_coef       0.0128(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         3692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0537
_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)+(0.0676P)²+1.9182P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                2817
_reflns_number_total             3692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105917n.txt
_cod_data_source_block           10a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2792.4(11)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7204199
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.1243(2) 0.2368(2) 0.67648(17) 0.0449(7) Uani 1 1 d . . .
O2 O 0.1359(2) 0.3472(2) 0.86275(15) 0.0404(7) Uani 1 1 d . . .
O3 O 0.3192(3) 0.2525(2) 0.92988(15) 0.0416(7) Uani 1 1 d . . .
O4 O 0.4009(3) 0.3934(2) 0.90802(18) 0.0539(8) Uani 1 1 d . . .
O5 O 0.1690(3) 0.4473(2) 0.64789(16) 0.0435(7) Uani 1 1 d . . .
O6 O 0.1942(2) 0.53588(19) 0.82809(15) 0.0376(7) Uani 1 1 d . . .
O7 O 0.0452(3) 0.5552(3) 0.91170(17) 0.0533(9) Uani 1 1 d . . .
N1 N 0.4672(3) 0.2870(2) 0.6183(2) 0.0380(8) Uani 1 1 d . . .
N2 N 0.2414(3) 0.3663(2) 0.75061(17) 0.0320(7) Uani 1 1 d . . .
N3 N 0.3002(3) 0.3104(2) 0.69665(17) 0.0304(7) Uani 1 1 d . . .
C1 C 0.4787(3) 0.4103(3) 0.7160(2) 0.0339(9) Uani 1 1 d . . .
H1B H 0.4391 0.4163 0.7660 0.041 Uiso 1 1 calc R . .
C2 C 0.4167(3) 0.3313(3) 0.6739(2) 0.0319(9) Uani 1 1 d . . .
C4 C 0.2271(3) 0.2454(3) 0.6573(2) 0.0336(9) Uani 1 1 d . . .
C5 C 0.2878(4) 0.1930(3) 0.5975(2) 0.0337(9) Uani 1 1 d . . .
C6 C 0.2294(4) 0.1212(3) 0.5578(2) 0.0456(11) Uani 1 1 d . . .
H6A H 0.1515 0.1063 0.5695 0.055 Uiso 1 1 calc R . .
C7 C 0.2892(4) 0.0728(3) 0.5007(3) 0.0510(12) Uani 1 1 d . . .
H7A H 0.2524 0.0234 0.4750 0.061 Uiso 1 1 calc R . .
C8 C 0.4043(5) 0.0980(3) 0.4818(3) 0.0527(12) Uani 1 1 d . . .
H8A H 0.4434 0.0654 0.4429 0.063 Uiso 1 1 calc R . .
C9 C 0.4615(4) 0.1698(3) 0.5191(3) 0.0470(11) Uani 1 1 d . . .
H9A H 0.5375 0.1872 0.5044 0.056 Uiso 1 1 calc R . .
C10 C 0.4044(4) 0.2168(3) 0.5795(2) 0.0352(9) Uani 1 1 d . . .
C11 C 0.61154(18) 0.3936(2) 0.73370(15) 0.0366(9) Uani 1 1 d G . .
C12 C 0.6491(2) 0.4148(2) 0.80793(14) 0.0470(11) Uani 1 1 d G . .
H12A H 0.5965 0.4409 0.8431 0.056 Uiso 1 1 calc R . .
C13 C 0.7652(2) 0.3968(2) 0.82960(13) 0.0559(13) Uani 1 1 d G . .
H13A H 0.7902 0.4110 0.8793 0.067 Uiso 1 1 calc R . .
C14 C 0.84374(19) 0.3577(2) 0.77704(18) 0.0558(13) Uani 1 1 d G . .
H14A H 0.9214 0.3457 0.7915 0.067 Uiso 1 1 calc R . .
C15 C 0.8062(2) 0.3366(2) 0.70282(16) 0.0559(13) Uani 1 1 d G . .
H15A H 0.8588 0.3105 0.6677 0.067 Uiso 1 1 calc R . .
C16 C 0.6901(2) 0.3546(2) 0.68115(12) 0.0475(11) Uani 1 1 d G . .
H16A H 0.6650 0.3404 0.6315 0.057 Uiso 1 1 calc R . .
C17 C 0.4575(2) 0.50339(14) 0.67335(14) 0.0344(9) Uani 1 1 d G . .
C18 C 0.4187(3) 0.58065(18) 0.71547(12) 0.0442(11) Uani 1 1 d G . .
H18A H 0.4090 0.5758 0.7685 0.053 Uiso 1 1 calc R . .
C19 C 0.3947(3) 0.66516(15) 0.67834(18) 0.0555(13) Uani 1 1 d G . .
H19A H 0.3688 0.7168 0.7065 0.067 Uiso 1 1 calc R . .
C20 C 0.4093(3) 0.67241(14) 0.59910(18) 0.0532(12) Uani 1 1 d G . .
H20A H 0.3932 0.7290 0.5743 0.064 Uiso 1 1 calc R . .
C21 C 0.4480(3) 0.59515(19) 0.55698(12) 0.0490(11) Uani 1 1 d G . .
H21A H 0.4578 0.6000 0.5040 0.059 Uiso 1 1 calc R . .
C22 C 0.4721(2) 0.51064(15) 0.59411(14) 0.0390(10) Uani 1 1 d G . .
H22A H 0.4980 0.4590 0.5659 0.047 Uiso 1 1 calc R . .
C23 C 0.2180(3) 0.3226(3) 0.8227(2) 0.0329(9) Uani 1 1 d . . .
C24 C 0.3013(4) 0.2442(3) 0.8473(2) 0.0352(9) Uani 1 1 d . . .
H24A H 0.3770 0.2504 0.8203 0.042 Uiso 1 1 calc R . .
C25 C 0.2513(4) 0.1471(3) 0.8351(3) 0.0508(12) Uani 1 1 d . . .
H25A H 0.3086 0.1010 0.8506 0.076 Uiso 1 1 calc R . .
H25B H 0.2327 0.1387 0.7816 0.076 Uiso 1 1 calc R . .
H25C H 0.1809 0.1399 0.8653 0.076 Uiso 1 1 calc R . .
C26 C 0.3750(4) 0.3315(4) 0.9515(3) 0.0472(11) Uani 1 1 d . . .
C27 C 0.3995(5) 0.3319(4) 1.0361(2) 0.0651(15) Uani 1 1 d . . .
H27A H 0.4389 0.3894 1.0497 0.098 Uiso 1 1 calc R . .
H27B H 0.4489 0.2793 1.0489 0.098 Uiso 1 1 calc R . .
H27C H 0.3263 0.3274 1.0638 0.098 Uiso 1 1 calc R . .
C28 C 0.1724(3) 0.4391(3) 0.7173(2) 0.0347(9) Uani 1 1 d . . .
C29 C 0.1088(4) 0.5073(3) 0.7703(2) 0.0354(9) Uani 1 1 d . . .
H29A H 0.0425 0.4752 0.7953 0.043 Uiso 1 1 calc R . .
C31 C 0.1487(4) 0.5606(3) 0.8973(3) 0.0425(10) Uani 1 1 d . . .
C32 C 0.2425(5) 0.5954(4) 0.9497(3) 0.0620(14) Uani 1 1 d . . .
H32A H 0.2081 0.6125 0.9982 0.093 Uiso 1 1 calc R . .
H32B H 0.2800 0.6494 0.9272 0.093 Uiso 1 1 calc R . .
H32C H 0.3001 0.5467 0.9575 0.093 Uiso 1 1 calc R . .
C30 C 0.0642(4) 0.5925(3) 0.7281(3) 0.0520(12) Uiso 1 1 d . . .
H30A H 0.0247 0.6336 0.7636 0.078 Uiso 1 1 calc R . .
H30B H 0.0098 0.5732 0.6887 0.078 Uiso 1 1 calc R . .
H30C H 0.1295 0.6250 0.7050 0.078 Uiso 1 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 0.0033 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C26 O3 C24 114.2(3) . . ?
C31 O6 C29 115.7(3) . . ?
C2 N1 C10 119.0(3) . . ?
N3 N2 C28 113.8(3) . . ?
N3 N2 C23 115.6(3) . . ?
C28 N2 C23 125.0(3) . . ?
N2 N3 C2 121.0(3) . . ?
N2 N3 C4 114.6(3) . . ?
C2 N3 C4 123.3(3) . . ?
C2 C1 C17 109.4(3) . . ?
C2 C1 C11 115.6(3) . . ?
C17 C1 C11 112.2(3) . . ?
N1 C2 N3 121.6(4) . . ?
N1 C2 C1 121.3(3) . . ?
N3 C2 C1 117.0(3) . . ?
O1 C4 N3 119.5(4) . . ?
O1 C4 C5 126.7(4) . . ?
N3 C4 C5 113.8(3) . . ?
C10 C5 C6 120.8(4) . . ?
C10 C5 C4 118.9(4) . . ?
C6 C5 C4 120.3(4) . . ?
C7 C6 C5 119.1(4) . . ?
C6 C7 C8 119.9(5) . . ?
C9 C8 C7 121.5(5) . . ?
C8 C9 C10 119.4(4) . . ?
C5 C10 N1 123.0(4) . . ?
C5 C10 C9 119.2(4) . . ?
N1 C10 C9 117.8(4) . . ?
C12 C11 C16 120.0 . . ?
C12 C11 C1 116.5(2) . . ?
C16 C11 C1 123.4(2) . . ?
C11 C12 C13 120.0 . . ?
C14 C13 C12 120.0 . . ?
C13 C14 C15 120.0 . . ?
C14 C15 C16 120.0 . . ?
C15 C16 C11 120.0 . . ?
C18 C17 C22 120.0 . . ?
C18 C17 C1 118.4(2) . . ?
C22 C17 C1 121.6(2) . . ?
C17 C18 C19 120.0 . . ?
C18 C19 C20 120.0 . . ?
C21 C20 C19 120.0 . . ?
C20 C21 C22 120.0 . . ?
C21 C22 C17 120.0 . . ?
O2 C23 N2 121.5(4) . . ?
O2 C23 C24 121.7(4) . . ?
N2 C23 C24 116.8(3) . . ?
O3 C24 C25 105.4(3) . . ?
O3 C24 C23 107.7(3) . . ?
C25 C24 C23 113.5(3) . . ?
O4 C26 O3 123.6(4) . . ?
O4 C26 C27 124.9(5) . . ?
O3 C26 C27 111.5(4) . . ?
O5 C28 N2 119.4(4) . . ?
O5 C28 C29 121.9(4) . . ?
N2 C28 C29 118.6(3) . . ?
O6 C29 C30 109.6(3) . . ?
O6 C29 C28 106.4(3) . . ?
C30 C29 C28 112.2(3) . . ?
O7 C31 O6 122.7(4) . . ?
O7 C31 C32 126.3(4) . . ?
O6 C31 C32 111.0(4) . . ?
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
O1 C4 1.216(5) . ?
O2 C23 1.211(5) . ?
O3 C26 1.341(6) . ?
O3 C24 1.454(5) . ?
O4 C26 1.196(5) . ?
O5 C28 1.212(5) . ?
O6 C31 1.354(5) . ?
O6 C29 1.451(5) . ?
O7 C31 1.199(5) . ?
N1 C2 1.286(5) . ?
N1 C10 1.398(5) . ?
N2 N3 1.397(4) . ?
N2 C28 1.420(5) . ?
N2 C23 1.423(5) . ?
N3 C2 1.407(5) . ?
N3 C4 1.416(5) . ?
C1 C2 1.513(6) . ?
C1 C17 1.536(4) . ?
C1 C11 1.552(4) . ?
C4 C5 1.451(6) . ?
C5 C10 1.397(6) . ?
C5 C6 1.398(6) . ?
C6 C7 1.384(6) . ?
C7 C8 1.390(7) . ?
C8 C9 1.371(6) . ?
C9 C10 1.403(6) . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
C17 C18 1.3900 . ?
C17 C22 1.3900 . ?
C18 C19 1.3900 . ?
C19 C20 1.3900 . ?
C20 C21 1.3900 . ?
C21 C22 1.3900 . ?
C23 C24 1.521(5) . ?
C24 C25 1.506(6) . ?
C26 C27 1.494(6) . ?
C28 C29 1.517(6) . ?
C29 C30 1.503(6) . ?
C31 C32 1.482(7) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21189928
