#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/52/4115275.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_4115275
loop_
_publ_author_name
'Makoto Yasuda'
'Kay Hirata'
'Mitsuyoshi Nishino'
'Akihiro Yamamoto'
'Akio Baba'
_publ_contact_author_address
;
    Department of Molecular Chemistry
    Graduate School of Engineering
    Osaka University
    2-1 Yamadaoka
    Suita Osaka 565-0871
    Japan
;
_publ_contact_author_email       ' baba@ap.chem.eng.osaka-u.ac.jp'
_publ_contact_author_fax         ' 81(6)68797387 '
_publ_contact_author_name        ' Dr Akio Baba'
_publ_contact_author_phone       ' 81(6)68797386 '
_publ_section_title
;
 Diastereoselective Addition of γ-Substituted Allylic Nucleophiles to
 Ketones: Highly Stereoselective Synthesis of Tertiary Homoallylic
 Alcohols Using an Allylic Tributylstannane/Stannous Chloride System
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13442
_journal_page_last               13447
_journal_paper_doi               10.1021/ja0274047
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'C26 H22 N2 O8 '
_chemical_formula_sum            'C26 H22 N2 O8'
_chemical_formula_weight         490.47
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                91.75(1)
_cell_angle_beta                 110.754(9)
_cell_angle_gamma                106.06(1)
_cell_formula_units_Z            2
_cell_length_a                   10.421(2)
_cell_length_b                   12.772(2)
_cell_length_c                   10.248(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.2
_cell_volume                     1213.1(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 1.0011
_diffrn_measured_fraction_theta_max 1.0011
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5835
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_decay_%        1.44
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     414
_refine_ls_number_reflns         5587
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.0334
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.05000(Max(Fo²,0) + 2Fc²)/3)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1562
_reflns_number_gt                1716
_reflns_number_total             5587
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ja0274047-4_s2_5.cif
_cod_data_source_block           17dE
_cod_original_cell_volume        1213.2(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C26 H22 N2 O8 '
_cod_database_code               4115275
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_adp_type
_atom_site_occupancy
_atom_site_calc_flag
O(1) O 0.6704(2) 0.2924(2) 0.3152(2) 0.0596(7) Uani 1.00 d
O(2) O 0.8746(2) 0.1376(2) 0.5527(2) 0.0696(8) Uani 1.00 d
O(4) O 1.0191(5) -0.2247(3) 1.0215(4) 0.144(2) Uani 1.00 d
O(5) O 0.6869(3) 0.1966(2) 0.1362(3) 0.110(1) Uani 1.00 d
O(6) O 0.6349(3) 0.6366(3) -0.2287(3) 0.114(1) Uani 1.00 d
O(9) O 1.2385(4) -0.1187(3) 1.1178(3) 0.122(1) Uani 1.00 d
O(10) O 0.6802(4) 0.7373(3) -0.0394(4) 0.130(1) Uani 1.00 d
O(11) O 1.1072(3) 0.2047(2) 0.5898(3) 0.107(1) Uani 1.00 d
N(3) N 0.6636(4) 0.6502(3) -0.1042(4) 0.083(1) Uani 1.00 d
N(4) N 1.1178(6) -0.1450(4) 1.0268(4) 0.098(2) Uani 1.00 d
C(1) C 0.6462(4) 0.4562(4) -0.0995(4) 0.070(1) Uani 1.00 d
C(2) C 0.9223(5) -0.0185(3) 0.7287(4) 0.070(1) Uani 1.00 d
C(3) C 1.0872(6) -0.0755(3) 0.9133(4) 0.072(1) Uani 1.00 d
C(5) C 1.0115(4) 0.1412(3) 0.6133(4) 0.069(1) Uani 1.00 d
C(6) C 0.6481(4) 0.3666(3) -0.0277(4) 0.069(1) Uani 1.00 d
C(7) C 0.6913(4) 0.2105(3) 0.4138(3) 0.058(1) Uani 1.00 d
C(8) C 0.6990(4) 0.5702(3) 0.1158(4) 0.065(1) Uani 1.00 d
C(9) C 0.6727(3) 0.3774(3) 0.1152(3) 0.055(1) Uani 1.00 d
C(12) C 0.8475(4) 0.2153(3) 0.4529(4) 0.067(1) Uani 1.00 d
C(13) C 0.7195(5) 0.4615(4) 0.5456(4) 0.069(1) Uani 1.00 d
C(14) C 1.0342(4) 0.0612(3) 0.7149(3) 0.061(1) Uani 1.00 d
C(15) C 0.6996(4) 0.4793(3) 0.1862(4) 0.060(1) Uani 1.00 d
C(17) C 0.5858(5) 0.0976(3) 0.3468(5) 0.078(2) Uani 1.00 d
C(18) C 0.5071(4) 0.2405(3) 0.5096(4) 0.069(1) Uani 1.00 d
C(19) C 0.4393(5) 0.1946(4) 0.5884(5) 0.081(2) Uani 1.00 d
C(20) C 1.1749(5) 0.0700(3) 0.7997(4) 0.079(2) Uani 1.00 d
C(21) C 0.8045(7) 0.5672(4) 0.6065(6) 0.093(2) Uani 1.00 d
C(22) C 1.2021(6) 0.0016(4) 0.9026(4) 0.082(2) Uani 1.00 d
C(23) C 0.9481(5) -0.0889(3) 0.8286(4) 0.076(1) Uani 1.00 d
C(24) C 0.8754(5) 0.3936(4) 0.7297(4) 0.074(2) Uani 1.00 d
C(25) C 0.9566(5) 0.5017(6) 0.7922(5) 0.100(2) Uani 1.00 d
C(26) C 0.9224(7) 0.5865(5) 0.7277(7) 0.106(2) Uani 1.00 d
C(27) C 0.6705(3) 0.5553(3) -0.0262(4) 0.062(1) Uani 1.00 d
C(28) C 0.7555(4) 0.3725(3) 0.6053(4) 0.056(1) Uani 1.00 d
C(29) C 0.6759(4) 0.2779(3) 0.1873(4) 0.071(1) Uani 1.00 d
C(30) C 0.6637(4) 0.2559(3) 0.5401(3) 0.057(1) Uani 1.00 d
H(1) H 0.631(3) 0.453(2) -0.199(3) 0.076(8) Uiso 1.00 calc
H(2) H 0.824(3) -0.028(3) 0.671(3) 0.074(9) Uiso 1.00 calc
H(3) H 0.632(3) 0.294(3) -0.074(3) 0.077(9) Uiso 1.00 calc
H(4) H 0.713(4) 0.641(3) 0.161(3) 0.087(9) Uiso 1.00 calc
H(5) H 0.632(3) 0.451(2) 0.465(3) 0.053(8) Uiso 1.00 calc
H(6) H 0.722(3) 0.490(2) 0.287(3) 0.054(8) Uiso 1.00 calc
H(7) H 0.457(4) 0.268(3) 0.426(4) 0.091(9) Uiso 1.00 calc
H(8) H 1.251(4) 0.133(3) 0.798(3) 0.078(9) Uiso 1.00 calc
H(9) H 0.784(4) 0.622(3) 0.560(4) 0.081(9) Uiso 1.00 calc
H(10) H 1.299(4) 0.013(3) 0.961(4) 0.097(9) Uiso 1.00 calc
H(11) H 0.873(4) -0.146(3) 0.841(4) 0.101(9) Uiso 1.00 calc
H(12) H 0.894(4) 0.332(3) 0.763(4) 0.093(9) Uiso 1.00 calc
H(13) H 1.041(4) 0.510(3) 0.880(4) 0.116(8) Uiso 1.00 calc
H(14) H 0.981(5) 0.660(4) 0.772(5) 0.141(7) Uiso 1.00 calc
H(15) H 0.686(3) 0.206(2) 0.602(3) 0.059(8) Uiso 1.00 calc
H(16) H 0.915(3) 0.291(3) 0.502(3) 0.077(9) Uiso 1.00 calc
H(17) H 0.870(3) 0.193(2) 0.373(3) 0.069(8) Uiso 1.00 calc
H(18) H 0.485(4) 0.102(3) 0.308(4) 0.116(8) Uiso 1.00 calc
H(19) H 0.609(4) 0.059(3) 0.282(4) 0.098(9) Uiso 1.00 calc
H(20) H 0.592(5) 0.056(3) 0.426(4) 0.131(8) Uiso 1.00 calc
H(21) H 0.492(4) 0.166(3) 0.669(4) 0.088(9) Uiso 1.00 calc
H(22) H 0.339(4) 0.188(3) 0.566(3) 0.093(9) Uiso 1.00 calc
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C(7) O(1) C(29) 121.7(2) 1_555 1_555 yes
C(5) O(2) C(12) 115.1(3) 1_555 1_555 yes
O(6) N(3) O(10) 123.2(4) 1_555 1_555 yes
O(6) N(3) C(27) 118.8(4) 1_555 1_555 yes
O(10) N(3) C(27) 117.9(4) 1_555 1_555 yes
O(4) N(4) O(9) 124.7(4) 1_555 1_555 yes
O(4) N(4) C(3) 116.9(5) 1_555 1_555 yes
O(9) N(4) C(3) 118.4(5) 1_555 1_555 yes
C(6) C(1) C(27) 118.3(3) 1_555 1_555 yes
C(6) C(1) H(1) 123(1) 1_555 1_555 no
C(27) C(1) H(1) 117(1) 1_555 1_555 no
C(14) C(2) C(23) 120.9(4) 1_555 1_555 yes
C(14) C(2) H(2) 121(1) 1_555 1_555 no
C(23) C(2) H(2) 117(1) 1_555 1_555 no
N(4) C(3) C(22) 117.4(4) 1_555 1_555 yes
N(4) C(3) C(23) 119.2(4) 1_555 1_555 yes
C(22) C(3) C(23) 123.3(4) 1_555 1_555 yes
O(2) C(5) O(11) 122.9(3) 1_555 1_555 yes
O(2) C(5) C(14) 113.2(3) 1_555 1_555 yes
O(11) C(5) C(14) 123.8(4) 1_555 1_555 yes
C(1) C(6) C(9) 120.6(4) 1_555 1_555 yes
C(1) C(6) H(3) 121(1) 1_555 1_555 no
C(9) C(6) H(3) 117(1) 1_555 1_555 no
O(1) C(7) C(12) 104.5(2) 1_555 1_555 yes
O(1) C(7) C(17) 111.3(3) 1_555 1_555 yes
O(1) C(7) C(30) 103.8(2) 1_555 1_555 yes
C(12) C(7) C(17) 113.5(3) 1_555 1_555 yes
C(12) C(7) C(30) 112.1(3) 1_555 1_555 yes
C(17) C(7) C(30) 111.1(3) 1_555 1_555 yes
C(15) C(8) C(27) 118.0(4) 1_555 1_555 yes
C(15) C(8) H(4) 122(2) 1_555 1_555 no
C(27) C(8) H(4) 119(2) 1_555 1_555 no
C(6) C(9) C(15) 119.4(3) 1_555 1_555 yes
C(6) C(9) C(29) 118.0(3) 1_555 1_555 yes
C(15) C(9) C(29) 122.5(3) 1_555 1_555 yes
O(2) C(12) C(7) 106.6(3) 1_555 1_555 yes
O(2) C(12) H(16) 107(1) 1_555 1_555 no
O(2) C(12) H(17) 106(1) 1_555 1_555 no
C(7) C(12) H(16) 111(1) 1_555 1_555 no
C(7) C(12) H(17) 114(1) 1_555 1_555 no
H(16) C(12) H(17) 109(2) 1_555 1_555 no
C(21) C(13) C(28) 120.2(4) 1_555 1_555 yes
C(21) C(13) H(5) 118(1) 1_555 1_555 no
C(28) C(13) H(5) 120(1) 1_555 1_555 no
C(2) C(14) C(5) 122.7(3) 1_555 1_555 yes
C(2) C(14) C(20) 119.7(3) 1_555 1_555 yes
C(5) C(14) C(20) 117.6(4) 1_555 1_555 yes
C(8) C(15) C(9) 120.6(3) 1_555 1_555 yes
C(8) C(15) H(6) 118(1) 1_555 1_555 no
C(9) C(15) H(6) 121(1) 1_555 1_555 no
C(7) C(17) H(18) 110(2) 1_555 1_555 no
C(7) C(17) H(19) 114(2) 1_555 1_555 no
C(7) C(17) H(20) 103(2) 1_555 1_555 no
H(18) C(17) H(19) 113(3) 1_555 1_555 no
H(18) C(17) H(20) 106(3) 1_555 1_555 no
H(19) C(17) H(20) 107(3) 1_555 1_555 no
C(19) C(18) C(30) 124.2(4) 1_555 1_555 yes
C(19) C(18) H(7) 120(2) 1_555 1_555 no
C(30) C(18) H(7) 115(2) 1_555 1_555 no
C(18) C(19) H(21) 117(2) 1_555 1_555 no
C(18) C(19) H(22) 121(2) 1_555 1_555 no
H(21) C(19) H(22) 120(2) 1_555 1_555 no
C(14) C(20) C(22) 120.0(4) 1_555 1_555 yes
C(14) C(20) H(8) 118(2) 1_555 1_555 no
C(22) C(20) H(8) 120(2) 1_555 1_555 no
C(13) C(21) C(26) 120.9(5) 1_555 1_555 yes
C(13) C(21) H(9) 117(2) 1_555 1_555 no
C(26) C(21) H(9) 121(2) 1_555 1_555 no
C(3) C(22) C(20) 118.2(4) 1_555 1_555 yes
C(3) C(22) H(10) 124(2) 1_555 1_555 no
C(20) C(22) H(10) 117(2) 1_555 1_555 no
C(2) C(23) C(3) 117.9(4) 1_555 1_555 yes
C(2) C(23) H(11) 123(2) 1_555 1_555 no
C(3) C(23) H(11) 118(2) 1_555 1_555 no
C(25) C(24) C(28) 120.4(4) 1_555 1_555 yes
C(25) C(24) H(12) 125(2) 1_555 1_555 no
C(28) C(24) H(12) 114(2) 1_555 1_555 no
C(24) C(25) C(26) 119.9(5) 1_555 1_555 yes
C(24) C(25) H(13) 115(2) 1_555 1_555 no
C(26) C(25) H(13) 124(2) 1_555 1_555 no
C(21) C(26) C(25) 120.3(5) 1_555 1_555 yes
C(21) C(26) H(14) 121(2) 1_555 1_555 no
C(25) C(26) H(14) 118(2) 1_555 1_555 no
N(3) C(27) C(1) 118.2(3) 1_555 1_555 yes
N(3) C(27) C(8) 118.8(4) 1_555 1_555 yes
C(1) C(27) C(8) 123.0(3) 1_555 1_555 yes
C(13) C(28) C(24) 118.1(4) 1_555 1_555 yes
C(13) C(28) C(30) 121.1(4) 1_555 1_555 yes
C(24) C(28) C(30) 120.8(3) 1_555 1_555 yes
O(1) C(29) O(5) 125.1(3) 1_555 1_555 yes
O(1) C(29) C(9) 112.2(3) 1_555 1_555 yes
O(5) C(29) C(9) 122.6(3) 1_555 1_555 yes
C(7) C(30) C(18) 113.5(3) 1_555 1_555 yes
C(7) C(30) C(28) 114.7(3) 1_555 1_555 yes
C(7) C(30) H(15) 100(1) 1_555 1_555 no
C(18) C(30) C(28) 111.4(3) 1_555 1_555 yes
C(18) C(30) H(15) 104(1) 1_555 1_555 no
C(28) C(30) H(15) 111(1) 1_555 1_555 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
O(1) C(7) 1.482(3) yes
O(1) C(29) 1.342(4) yes
O(2) C(5) 1.326(4) yes
O(2) C(12) 1.456(4) yes
O(4) N(4) 1.214(5) yes
O(5) C(29) 1.200(4) yes
O(6) N(3) 1.198(4) yes
O(9) N(4) 1.217(5) yes
O(10) N(3) 1.214(4) yes
O(11) C(5) 1.202(4) yes
N(3) C(27) 1.477(4) yes
N(4) C(3) 1.482(5) yes
C(1) C(6) 1.380(5) yes
C(1) C(27) 1.364(5) yes
C(1) H(1) 0.97(3) no
C(2) C(14) 1.372(5) yes
C(2) C(23) 1.387(5) yes
C(2) H(2) 0.96(3) no
C(3) C(22) 1.365(5) yes
C(3) C(23) 1.359(5) yes
C(5) C(14) 1.487(4) yes
C(6) C(9) 1.390(4) yes
C(6) H(3) 0.97(3) no
C(7) C(12) 1.514(4) yes
C(7) C(17) 1.512(5) yes
C(7) C(30) 1.551(4) yes
C(8) C(15) 1.386(4) yes
C(8) C(27) 1.374(4) yes
C(8) H(4) 0.95(3) no
C(9) C(15) 1.378(4) yes
C(9) C(29) 1.491(4) yes
C(12) H(16) 1.02(3) no
C(12) H(17) 0.98(3) no
C(13) C(21) 1.376(6) yes
C(13) C(28) 1.387(4) yes
C(13) H(5) 0.96(3) no
C(14) C(20) 1.384(5) yes
C(15) H(6) 0.97(3) no
C(17) H(18) 1.00(4) no
C(17) H(19) 0.95(4) no
C(17) H(20) 0.97(4) no
C(18) C(19) 1.303(5) yes
C(18) C(30) 1.503(4) yes
C(18) H(7) 0.97(3) no
C(19) H(21) 0.96(3) no
C(19) H(22) 0.97(3) no
C(20) C(22) 1.391(5) yes
C(20) H(8) 0.97(3) no
C(21) C(26) 1.358(7) yes
C(21) H(9) 0.89(3) no
C(22) H(10) 0.94(3) no
C(23) H(11) 0.96(4) no
C(24) C(25) 1.396(6) yes
C(24) C(28) 1.387(5) yes
C(24) H(12) 0.91(3) no
C(25) C(26) 1.351(7) yes
C(25) H(13) 0.99(4) no
C(26) H(14) 0.96(5) no
C(28) C(30) 1.509(4) yes
C(30) H(15) 0.93(3) no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
O(1) O(6) 3.373(3) 2_665
O(4) H(12) 2.65(4) 2_757
O(4) H(14) 2.76(5) 1_545
O(4) O(10) 3.251(6) 1_546
O(4) N(3) 3.340(6) 1_546
O(4) C(26) 3.458(7) 1_545
O(4) C(24) 3.468(5) 2_757
O(5) H(10) 2.89(4) 2_756
O(5) C(22) 3.129(4) 2_756
O(5) O(9) 3.174(4) 2_756
O(5) H(14) 3.21(5) 2_766
O(5) N(4) 3.232(5) 2_756
O(5) C(3) 3.317(5) 2_756
O(6) H(5) 2.86(3) 2_665
O(6) H(11) 3.03(4) 1_564
O(6) C(21) 3.106(5) 1_554
O(6) H(9) 3.11(3) 1_554
O(6) C(18) 3.389(5) 2_665
O(6) C(26) 3.403(6) 1_554
O(6) H(6) 3.44(3) 2_665
O(6) H(14) 3.53(5) 1_554
O(6) C(15) 3.577(4) 2_665
O(9) H(3) 3.01(3) 2_756
O(9) H(15) 3.04(3) 2_757
O(9) H(21) 3.11(3) 2_757
O(9) H(2) 3.17(3) 2_757
O(9) H(12) 3.18(4) 2_757
O(9) H(18) 3.23(4) 1_656
O(9) C(2) 3.417(5) 2_757
O(10) H(8) 2.68(3) 2_766
O(10) H(11) 2.82(4) 1_564
O(10) C(20) 3.053(6) 2_766
O(10) H(10) 3.19(4) 2_766
O(10) C(22) 3.290(6) 2_766
O(10) C(9) 3.347(5) 2_665
O(10) C(29) 3.421(5) 2_665
O(11) H(22) 2.57(4) 1_655
O(11) H(4) 2.86(3) 2_766
O(11) H(9) 2.93(4) 2_766
O(11) C(19) 3.504(5) 1_655
N(3) H(11) 3.11(4) 1_564
N(3) C(9) 3.385(4) 2_665
N(3) H(7) 3.40(3) 2_665
N(3) C(15) 3.460(5) 2_665
N(4) H(14) 3.17(5) 1_545
N(4) H(12) 3.27(4) 2_757
N(4) C(2) 3.423(5) 2_757
N(4) H(2) 3.52(3) 2_757
N(4) H(3) 3.54(3) 2_756
C(1) H(13) 3.14(4) 2_766
C(1) H(4) 3.42(3) 2_665
C(1) C(8) 3.462(5) 2_665
C(2) H(22) 3.43(3) 2_656
C(3) H(14) 3.35(5) 1_545
C(3) H(17) 3.48(3) 2_756
C(3) C(23) 3.509(5) 2_757
C(3) H(11) 3.56(4) 2_757
C(5) H(4) 3.44(3) 2_766
C(5) H(22) 3.50(4) 1_655
C(6) H(13) 2.97(4) 2_766
C(6) H(4) 3.49(3) 2_665
C(6) H(21) 3.54(3) 1_554
C(8) H(13) 3.14(4) 2_766
C(8) C(27) 3.498(5) 2_665
C(9) H(13) 2.92(4) 2_766
C(9) C(25) 3.496(6) 2_766
C(9) H(14) 3.55(5) 2_766
C(12) H(14) 3.55(5) 2_766
C(13) H(1) 3.06(3) 1_556
C(15) H(13) 2.99(4) 2_766
C(15) C(25) 3.449(6) 2_766
C(15) C(27) 3.507(4) 2_665
C(17) H(21) 3.22(4) 2_656
C(18) H(2) 3.56(3) 2_656
C(18) H(1) 3.58(3) 1_556
C(19) H(20) 3.12(4) 2_656
C(19) H(2) 3.22(3) 2_656
C(19) H(3) 3.32(3) 1_556
C(19) H(8) 3.37(3) 1_455
C(19) H(19) 3.52(3) 2_656
C(19) H(1) 3.53(3) 1_556
C(20) H(19) 3.44(4) 2_756
C(20) H(4) 3.51(3) 2_766
C(20) H(22) 3.55(3) 1_655
C(20) H(17) 3.58(3) 2_756
C(21) H(1) 3.26(3) 1_556
C(21) H(16) 3.54(3) 2_766
C(22) H(19) 3.38(4) 2_756
C(22) H(17) 3.43(3) 2_756
C(22) H(11) 3.58(4) 2_757
C(23) H(14) 3.37(5) 1_545
C(24) H(1) 3.16(3) 1_556
C(25) H(1) 3.31(3) 1_556
C(25) H(13) 3.35(4) 2_767
C(26) H(1) 3.39(3) 1_556
C(26) H(17) 3.48(3) 2_766
C(26) H(16) 3.53(3) 2_766
C(27) H(13) 3.20(4) 2_766
C(28) H(1) 3.04(3) 1_556
C(29) H(14) 3.31(5) 2_766
H(1) H(5) 3.45(4) 1_554
H(1) H(21) 3.58(5) 1_554
H(2) H(22) 2.80(5) 2_656
H(2) H(18) 3.19(5) 2_656
H(2) H(7) 3.43(5) 2_656
H(3) H(21) 2.73(5) 1_554
H(3) H(13) 3.46(5) 2_766
H(4) H(8) 2.80(5) 2_766
H(5) H(5) 3.59(5) 2_666
H(6) H(13) 3.47(5) 2_766
H(7) H(9) 3.24(5) 2_666
H(7) H(11) 3.44(5) 2_656
H(8) H(22) 2.87(5) 1_655
H(8) H(21) 3.17(5) 1_655
H(8) H(19) 3.40(5) 2_756
H(9) H(22) 3.15(5) 2_666
H(9) H(16) 3.32(4) 2_766
H(9) H(17) 3.54(4) 2_766
H(10) H(19) 3.17(5) 2_756
H(10) H(18) 3.37(5) 1_656
H(10) H(19) 3.59(5) 1_656
H(11) H(14) 3.15(6) 1_545
H(13) H(13) 2.86(8) 2_767
H(14) H(17) 2.89(5) 2_766
H(14) H(16) 3.37(5) 2_766
H(18) H(21) 3.50(5) 2_656
H(19) H(21) 2.90(5) 2_656
H(20) H(21) 2.76(6) 2_656
H(20) H(20) 2.95(8) 2_656
H(20) H(22) 3.39(5) 2_656
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O(1) C(7) C(12) O(2) 178.8(3) 1_555 1_555 1_555 1_555 yes
O(1) C(7) C(30) C(18) 74.4(3) 1_555 1_555 1_555 1_555 yes
O(1) C(7) C(30) C(28) -55.2(3) 1_555 1_555 1_555 1_555 yes
O(1) C(29) C(9) C(6) -167.0(3) 1_555 1_555 1_555 1_555 yes
O(1) C(29) C(9) C(15) 16.0(5) 1_555 1_555 1_555 1_555 yes
O(2) C(5) C(14) C(2) 8.7(5) 1_555 1_555 1_555 1_555 yes
O(2) C(5) C(14) C(20) -170.2(3) 1_555 1_555 1_555 1_555 yes
O(2) C(12) C(7) C(17) -59.8(4) 1_555 1_555 1_555 1_555 yes
O(2) C(12) C(7) C(30) 67.0(4) 1_555 1_555 1_555 1_555 yes
O(4) N(4) C(3) C(22) -168.2(4) 1_555 1_555 1_555 1_555 yes
O(4) N(4) C(3) C(23) 13.7(5) 1_555 1_555 1_555 1_555 yes
O(5) C(29) O(1) C(7) 5.8(6) 1_555 1_555 1_555 1_555 yes
O(5) C(29) C(9) C(6) 15.2(6) 1_555 1_555 1_555 1_555 yes
O(5) C(29) C(9) C(15) -161.8(4) 1_555 1_555 1_555 1_555 yes
O(6) N(3) C(27) C(1) 1.1(5) 1_555 1_555 1_555 1_555 yes
O(6) N(3) C(27) C(8) -178.0(3) 1_555 1_555 1_555 1_555 yes
O(9) N(4) C(3) C(22) 11.9(5) 1_555 1_555 1_555 1_555 yes
O(9) N(4) C(3) C(23) -166.2(4) 1_555 1_555 1_555 1_555 yes
O(10) N(3) C(27) C(1) 177.4(4) 1_555 1_555 1_555 1_555 yes
O(10) N(3) C(27) C(8) -1.7(5) 1_555 1_555 1_555 1_555 yes
O(11) C(5) O(2) C(12) 1.0(5) 1_555 1_555 1_555 1_555 yes
O(11) C(5) C(14) C(2) -172.7(4) 1_555 1_555 1_555 1_555 yes
O(11) C(5) C(14) C(20) 8.5(5) 1_555 1_555 1_555 1_555 yes
N(3) C(27) C(1) C(6) -177.9(3) 1_555 1_555 1_555 1_555 yes
N(3) C(27) C(8) C(15) 177.6(3) 1_555 1_555 1_555 1_555 yes
N(4) C(3) C(22) C(20) -177.9(3) 1_555 1_555 1_555 1_555 yes
N(4) C(3) C(23) C(2) 176.4(3) 1_555 1_555 1_555 1_555 yes
C(1) C(6) C(9) C(15) -1.9(5) 1_555 1_555 1_555 1_555 yes
C(1) C(6) C(9) C(29) -179.0(3) 1_555 1_555 1_555 1_555 yes
C(1) C(27) C(8) C(15) -1.5(5) 1_555 1_555 1_555 1_555 yes
C(2) C(14) C(20) C(22) -2.9(5) 1_555 1_555 1_555 1_555 yes
C(2) C(23) C(3) C(22) -1.6(6) 1_555 1_555 1_555 1_555 yes
C(3) C(22) C(20) C(14) 2.2(6) 1_555 1_555 1_555 1_555 yes
C(3) C(23) C(2) C(14) 0.9(5) 1_555 1_555 1_555 1_555 yes
C(5) O(2) C(12) C(7) -171.4(3) 1_555 1_555 1_555 1_555 yes
C(5) C(14) C(2) C(23) -177.5(3) 1_555 1_555 1_555 1_555 yes
C(5) C(14) C(20) C(22) 176.0(3) 1_555 1_555 1_555 1_555 yes
C(6) C(1) C(27) C(8) 1.1(5) 1_555 1_555 1_555 1_555 yes
C(6) C(9) C(15) C(8) 1.5(5) 1_555 1_555 1_555 1_555 yes
C(7) O(1) C(29) C(9) -171.9(3) 1_555 1_555 1_555 1_555 yes
C(7) C(30) C(18) C(19) 127.8(4) 1_555 1_555 1_555 1_555 yes
C(7) C(30) C(28) C(13) 81.0(3) 1_555 1_555 1_555 1_555 yes
C(7) C(30) C(28) C(24) -101.4(3) 1_555 1_555 1_555 1_555 yes
C(8) C(15) C(9) C(29) 178.4(3) 1_555 1_555 1_555 1_555 yes
C(9) C(6) C(1) C(27) 0.6(5) 1_555 1_555 1_555 1_555 yes
C(9) C(15) C(8) C(27) 0.2(5) 1_555 1_555 1_555 1_555 yes
C(12) O(2) C(5) C(14) 179.6(3) 1_555 1_555 1_555 1_555 yes
C(12) C(7) O(1) C(29) 66.8(4) 1_555 1_555 1_555 1_555 yes
C(12) C(7) C(30) C(18) -173.4(3) 1_555 1_555 1_555 1_555 yes
C(12) C(7) C(30) C(28) 57.0(3) 1_555 1_555 1_555 1_555 yes
C(13) C(21) C(26) C(25) -1.3(7) 1_555 1_555 1_555 1_555 yes
C(13) C(28) C(24) C(25) 0.1(5) 1_555 1_555 1_555 1_555 yes
C(13) C(28) C(30) C(18) -49.6(4) 1_555 1_555 1_555 1_555 yes
C(17) C(7) O(1) C(29) -56.0(4) 1_555 1_555 1_555 1_555 yes
C(17) C(7) C(30) C(18) -45.2(4) 1_555 1_555 1_555 1_555 yes
C(17) C(7) C(30) C(28) -174.8(3) 1_555 1_555 1_555 1_555 yes
C(18) C(30) C(28) C(24) 128.0(3) 1_555 1_555 1_555 1_555 yes
C(19) C(18) C(30) C(28) -101.0(4) 1_555 1_555 1_555 1_555 yes
C(20) C(14) C(2) C(23) 1.4(5) 1_555 1_555 1_555 1_555 yes
C(20) C(22) C(3) C(23) 0.1(6) 1_555 1_555 1_555 1_555 yes
C(21) C(13) C(28) C(24) 2.4(5) 1_555 1_555 1_555 1_555 yes
C(21) C(13) C(28) C(30) -180.0(3) 1_555 1_555 1_555 1_555 yes
C(21) C(26) C(25) C(24) 3.9(7) 1_555 1_555 1_555 1_555 yes
C(25) C(24) C(28) C(30) -177.5(3) 1_555 1_555 1_555 1_555 yes
C(26) C(21) C(13) C(28) -1.9(6) 1_555 1_555 1_555 1_555 yes
C(26) C(25) C(24) C(28) -3.3(6) 1_555 1_555 1_555 1_555 yes
C(29) O(1) C(7) C(30) -175.5(3) 1_555 1_555 1_555 1_555 yes
