#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/54/1505442.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_1505442
loop_
_publ_author_name
'Wang, Qi-Qiang'
'Wang, De-Xian'
'Zheng, Qi-Yu'
'Wang, Mei-Xiang'
_publ_section_title
;
 Formation and conformational conversion of flattened partial cone oxygen
 bridged calix[2]arene[2]triazines.
;
_journal_issue                   15
_journal_name_full               'Organic letters'
_journal_page_first              2847
_journal_page_last               2850
_journal_paper_doi               10.1021/ol0710008
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C50 H38 N6 O10'
_chemical_formula_weight         882.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 102.76(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3404(19)
_cell_length_b                   27.574(6)
_cell_length_c                   17.783(4)
_cell_measurement_reflns_used    20336
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.48
_cell_volume                     4466.9(17)
_computing_cell_refinement       'Rapid Auto(Rigaku 2001)'
_computing_data_collection       'Rapid Auto(Rigaku 2001)'
_computing_data_reduction        'Rapid Auto(Rigaku 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku raxis Rapid IP Area Detector'
_diffrn_measurement_method       'ω oscillation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20336
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9980
_exptl_absorpt_correction_T_min  0.9318
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   abscor
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin platelet'
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1272
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0835P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1741
_reflns_number_gt                2607
_reflns_number_total             5050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0710008si20070429_041047.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4466.9(16)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1505442
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
O1 O 1.33522(17) 0.29003(7) 0.21916(10) 0.0464(5) Uani 1 1 d .
O2 O 1.12237(17) 0.28810(7) 0.43967(9) 0.0453(4) Uani 1 1 d .
O3 O 1.3669(4) 0.46355(9) 0.31470(17) 0.1043(10) Uani 1 1 d .
O4 O 1.2677(3) 0.45962(8) 0.41612(16) 0.0934(9) Uani 1 1 d .
O5 O 1.18489(18) 0.24197(6) 0.31399(10) 0.0471(5) Uani 1 1 d .
N1 N 1.1003(2) 0.29044(8) 0.14532(11) 0.0404(5) Uani 1 1 d .
N2 N 1.0451(2) 0.23374(7) 0.04188(11) 0.0405(5) Uani 1 1 d .
N3 N 1.2818(2) 0.23395(8) 0.12591(12) 0.0414(5) Uani 1 1 d .
C1 C 1.0144(2) 0.26985(9) 0.08485(13) 0.0378(6) Uani 1 1 d .
C2 C 1.1816(3) 0.21627(9) 0.06632(14) 0.0384(5) Uani 1 1 d .
C3 C 1.2329(3) 0.27039(9) 0.16145(14) 0.0403(6) Uani 1 1 d .
C4 C 1.2168(2) 0.28997(9) 0.32548(14) 0.0391(6) Uani 1 1 d .
C5 C 1.2848(2) 0.31590(10) 0.27612(13) 0.0392(6) Uani 1 1 d .
C6 C 1.3132(3) 0.36447(10) 0.28589(14) 0.0429(6) Uani 1 1 d .
H6A H 1.3580 0.3812 0.2519 0.051 Uiso 1 1 calc R
C7 C 1.2745(3) 0.38852(9) 0.34676(15) 0.0437(6) Uani 1 1 d .
C8 C 1.2066(3) 0.36336(10) 0.39752(14) 0.0418(6) Uani 1 1 d .
H8A H 1.1803 0.3793 0.4385 0.050 Uiso 1 1 calc R
C9 C 1.1792(2) 0.31488(9) 0.38595(13) 0.0387(6) Uani 1 1 d .
C10 C 1.3082(3) 0.44079(11) 0.35604(19) 0.0604(8) Uani 1 1 d .
C11 C 1.2926(7) 0.51083(14) 0.4297(3) 0.149(2) Uani 1 1 d .
H11A H 1.2585 0.5202 0.4747 0.223 Uiso 1 1 calc R
H11B H 1.2402 0.5288 0.3860 0.223 Uiso 1 1 calc R
H11C H 1.3957 0.5176 0.4376 0.223 Uiso 1 1 calc R
C12 C 1.3052(3) 0.21096(11) 0.3492(2) 0.0717(10) Uani 1 1 d .
H12A H 1.3376 0.2189 0.4034 0.086 Uiso 1 1 calc R
H12B H 1.3870 0.2157 0.3246 0.086 Uiso 1 1 calc R
C13 C 1.2555(3) 0.15975(11) 0.34045(18) 0.0583(8) Uani 1 1 d .
C14 C 1.1723(4) 0.14199(16) 0.3883(3) 0.0940(13) Uani 1 1 d .
H14A H 1.1485 0.1623 0.4255 0.113 Uiso 1 1 calc R
C15 C 1.1232(6) 0.0955(2) 0.3833(4) 0.152(3) Uani 1 1 d .
H15A H 1.0655 0.0838 0.4157 0.182 Uiso 1 1 calc R
C16 C 1.1605(10) 0.0676(2) 0.3307(6) 0.175(4) Uani 1 1 d .
H16A H 1.1261 0.0358 0.3282 0.210 Uiso 1 1 calc R
C17 C 1.2434(10) 0.0796(3) 0.2796(5) 0.181(4) Uani 1 1 d .
H17A H 1.2670 0.0579 0.2441 0.217 Uiso 1 1 calc R
C18 C 1.2918(5) 0.13037(19) 0.2863(3) 0.1149(16) Uani 1 1 d .
H18A H 1.3476 0.1425 0.2532 0.138 Uiso 1 1 calc R
C19 C 1.2254(3) 0.17438(9) 0.02472(14) 0.0400(6) Uani 1 1 d .
C20 C 1.3622(3) 0.15314(10) 0.04973(16) 0.0476(7) Uani 1 1 d .
H20A H 1.4256 0.1649 0.0938 0.057 Uiso 1 1 calc R
C21 C 1.4055(3) 0.11483(10) 0.01015(18) 0.0542(7) Uani 1 1 d .
H21A H 1.4980 0.1013 0.0278 0.065 Uiso 1 1 calc R
C22 C 1.3134(3) 0.09617(10) -0.05554(17) 0.0512(7) Uani 1 1 d .
C23 C 1.1750(3) 0.11642(10) -0.07859(16) 0.0519(7) Uani 1 1 d .
H23A H 1.1097 0.1036 -0.1211 0.062 Uiso 1 1 calc R
C24 C 1.1317(3) 0.15527(9) -0.03984(15) 0.0465(6) Uani 1 1 d .
H24A H 1.0389 0.1687 -0.0572 0.056 Uiso 1 1 calc R
C25 C 1.3618(4) 0.05518(12) -0.1008(2) 0.0817(11) Uani 1 1 d .
H25A H 1.4605 0.0459 -0.0768 0.123 Uiso 1 1 calc R
H25B H 1.3582 0.0657 -0.1526 0.123 Uiso 1 1 calc R
H25C H 1.2976 0.0279 -0.1015 0.123 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
C3 O1 C5 117.27(18) . .
C1 O2 C9 116.70(18) 2_755 .
C10 O4 C11 117.2(3) . .
C4 O5 C12 112.81(19) . .
C1 N1 C3 111.5(2) . .
C1 N2 C2 113.2(2) . .
C3 N3 C2 113.6(2) . .
N1 C1 N2 128.6(2) . .
N1 C1 O2 117.6(2) . 2_755
N2 C1 O2 113.8(2) . 2_755
N3 C2 N2 124.9(2) . .
N3 C2 C19 117.3(2) . .
N2 C2 C19 117.8(2) . .
N3 C3 N1 128.1(2) . .
N3 C3 O1 114.0(2) . .
N1 C3 O1 117.8(2) . .
O5 C4 C9 120.9(2) . .
O5 C4 C5 121.4(2) . .
C9 C4 C5 117.7(2) . .
C6 C5 C4 121.7(2) . .
C6 C5 O1 120.2(2) . .
C4 C5 O1 117.9(2) . .
C5 C6 C7 119.4(2) . .
C6 C7 C8 120.1(2) . .
C6 C7 C10 118.0(2) . .
C8 C7 C10 121.9(3) . .
C9 C8 C7 119.0(2) . .
C8 C9 C4 122.0(2) . .
C8 C9 O2 119.9(2) . .
C4 C9 O2 117.9(2) . .
O3 C10 O4 123.3(3) . .
O3 C10 C7 124.2(3) . .
O4 C10 C7 112.5(3) . .
O5 C12 C13 108.9(2) . .
C18 C13 C14 119.6(4) . .
C18 C13 C12 121.4(4) . .
C14 C13 C12 119.0(3) . .
C15 C14 C13 121.9(5) . .
C16 C15 C14 117.4(7) . .
C15 C16 C17 127.7(8) . .
C16 C17 C18 112.9(6) . .
C13 C18 C17 120.4(6) . .
C24 C19 C20 118.3(2) . .
C24 C19 C2 121.2(2) . .
C20 C19 C2 120.5(2) . .
C21 C20 C19 120.9(3) . .
C20 C21 C22 121.1(3) . .
C23 C22 C21 117.7(3) . .
C23 C22 C25 120.9(3) . .
C21 C22 C25 121.4(3) . .
C24 C23 C22 121.5(3) . .
C23 C24 C19 120.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C3 1.352(3) .
O1 C5 1.403(3) .
O2 C1 1.353(3) 2_755
O2 C9 1.401(3) .
O3 C10 1.188(4) .
O4 C10 1.316(4) .
O4 C11 1.443(4) .
O5 C4 1.362(3) .
O5 C12 1.440(3) .
N1 C1 1.320(3) .
N1 C3 1.329(3) .
N2 C1 1.324(3) .
N2 C2 1.343(3) .
N3 C3 1.321(3) .
N3 C2 1.341(3) .
C1 O2 1.353(3) 2_755
C2 C19 1.477(3) .
C4 C9 1.385(3) .
C4 C5 1.390(3) .
C5 C6 1.369(4) .
C6 C7 1.384(3) .
C7 C8 1.397(3) .
C7 C10 1.477(4) .
C8 C9 1.368(4) .
C12 C13 1.484(4) .
C13 C18 1.357(5) .
C13 C14 1.364(5) .
C14 C15 1.358(6) .
C15 C16 1.316(9) .
C16 C17 1.359(11) .
C17 C18 1.468(9) .
C19 C24 1.385(4) .
C19 C20 1.387(3) .
C20 C21 1.379(4) .
C21 C22 1.388(4) .
C22 C23 1.385(4) .
C22 C25 1.513(4) .
C23 C24 1.382(4) .
