#------------------------------------------------------------------------------
#$Date: 2016-03-26 15:08:31 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180289 $
#$URL: svn://www.crystallography.net/cod/cif/7/15/03/7150307.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_7150307
loop_
_publ_author_name
'Mitchell, Judith M.'
'Finney, Nathaniel S.'
_publ_section_title
;
 Synthetic studies of pseurotin A: preparation of an advanced lactam
 aldehyde intermediate.
;
_journal_issue                   23
_journal_name_full               'Organic & biomolecular chemistry'
_journal_page_first              4274
_journal_page_last               4281
_journal_paper_doi               10.1039/b512701g
_journal_volume                  3
_journal_year                    2005
_chemical_formula_sum            'C24 H27 N O7 S'
_chemical_formula_weight         473.53
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.4720(10)
_cell_angle_beta                 83.1290(10)
_cell_angle_gamma                69.3510(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9592(7)
_cell_length_b                   9.2569(6)
_cell_length_c                   15.3512(11)
_cell_measurement_reflns_used    4557
_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.38
_cell_volume                     1169.19(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      218(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0366
_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       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7140
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_T_max  0.9819
_exptl_absorpt_correction_T_min  0.9303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0772P)²+1.0148P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1614
_reflns_number_gt                3434
_reflns_number_total             4097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b512701g.txt
_cod_data_source_block           jmich01
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' 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_sg_symbol_H-M      P-1
_cod_database_code               7150307
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N -0.0628(3) 0.9094(3) 0.10731(15) 0.0333(6) Uani 1 1 d . . .
S1 S 0.52235(10) 0.52304(10) 0.22728(6) 0.0516(3) Uani 1 1 d . . .
O1 O -0.1913(3) 1.0899(2) 0.22976(14) 0.0432(5) Uani 1 1 d . . .
O2 O -0.2796(2) 0.8156(2) 0.14434(13) 0.0358(5) Uani 1 1 d . . .
O3 O 0.0109(2) 0.72829(19) 0.29644(11) 0.0286(4) Uani 1 1 d . . .
O4 O 0.0584(3) 0.3994(2) 0.15292(15) 0.0467(6) Uani 1 1 d . . .
O5 O 0.2591(5) 0.2674(4) 0.0694(2) 0.1124(15) Uani 1 1 d . . .
O6 O 0.1642(3) 0.8141(2) 0.02128(14) 0.0513(6) Uani 1 1 d . . .
O7 O 0.2402(2) 0.5671(2) 0.17795(13) 0.0329(4) Uani 1 1 d . . .
C1 C -0.1613(3) 0.8560(3) 0.17716(17) 0.0290(6) Uani 1 1 d . . .
C2 C -0.0451(3) 0.7007(3) 0.22177(16) 0.0276(6) Uani 1 1 d . . .
H2A H -0.0999 0.6229 0.2395 0.033 Uiso 1 1 calc R . .
C3 C 0.0864(3) 0.6489(3) 0.14783(17) 0.0307(6) Uani 1 1 d . . .
C4 C 0.0705(3) 0.8002(3) 0.08400(18) 0.0359(7) Uani 1 1 d . . .
C5 C -0.2376(3) 0.9809(3) 0.23856(18) 0.0296(6) Uani 1 1 d . . .
C6 C -0.3707(3) 0.9686(3) 0.30330(17) 0.0302(6) Uani 1 1 d . . .
C7 C -0.4671(4) 1.1029(3) 0.3362(2) 0.0411(7) Uani 1 1 d . . .
H7A H -0.4463 1.1968 0.3176 0.049 Uiso 1 1 calc R . .
C8 C -0.5931(4) 1.0993(4) 0.3961(2) 0.0504(8) Uani 1 1 d . . .
H8A H -0.6585 1.1911 0.4179 0.061 Uiso 1 1 calc R . .
C9 C -0.6240(4) 0.9629(4) 0.4242(2) 0.0479(8) Uani 1 1 d . . .
H9A H -0.7091 0.9605 0.4661 0.058 Uiso 1 1 calc R . .
C10 C -0.5311(4) 0.8310(4) 0.3913(2) 0.0476(8) Uani 1 1 d . . .
H10A H -0.5529 0.7376 0.4102 0.057 Uiso 1 1 calc R . .
C11 C -0.4054(4) 0.8327(3) 0.3305(2) 0.0417(7) Uani 1 1 d . . .
H11A H -0.3430 0.7412 0.3076 0.050 Uiso 1 1 calc R . .
C12 C -0.3892(4) 0.9397(4) 0.0908(2) 0.0494(8) Uani 1 1 d . . .
H12A H -0.4663 0.9024 0.0713 0.074 Uiso 1 1 calc R . .
H12B H -0.3317 0.9779 0.0394 0.074 Uiso 1 1 calc R . .
H12C H -0.4445 1.0237 0.1249 0.074 Uiso 1 1 calc R . .
C13 C 0.0601(4) 0.5924(3) 0.36191(18) 0.0355(6) Uani 1 1 d . . .
H13A H 0.1522 0.5121 0.3381 0.043 Uiso 1 1 calc R . .
H13B H -0.0270 0.5499 0.3781 0.043 Uiso 1 1 calc R . .
C14 C 0.1040(3) 0.6359(3) 0.44180(17) 0.0311(6) Uani 1 1 d . . .
C15 C 0.2448(3) 0.5474(3) 0.48129(19) 0.0368(7) Uani 1 1 d . . .
H15A H 0.3161 0.4616 0.4561 0.044 Uiso 1 1 calc R . .
C16 C 0.2818(4) 0.5839(3) 0.5574(2) 0.0401(7) Uani 1 1 d . . .
H16A H 0.3778 0.5224 0.5839 0.048 Uiso 1 1 calc R . .
C17 C 0.1802(4) 0.7080(4) 0.59443(19) 0.0415(7) Uani 1 1 d . . .
H17A H 0.2053 0.7322 0.6465 0.050 Uiso 1 1 calc R . .
C18 C 0.0404(4) 0.7978(4) 0.5550(2) 0.0492(8) Uani 1 1 d . . .
H18A H -0.0300 0.8841 0.5800 0.059 Uiso 1 1 calc R . .
C19 C 0.0032(4) 0.7623(4) 0.4797(2) 0.0448(8) Uani 1 1 d . . .
H19A H -0.0926 0.8249 0.4533 0.054 Uiso 1 1 calc R . .
C20 C 0.0503(4) 0.5413(4) 0.0961(2) 0.0426(7) Uani 1 1 d . . .
H20A H -0.0566 0.5915 0.0735 0.051 Uiso 1 1 calc R . .
H20B H 0.1280 0.5197 0.0454 0.051 Uiso 1 1 calc R . .
C21 C 0.1669(4) 0.2690(4) 0.1328(2) 0.0557(9) Uani 1 1 d . . .
C22 C 0.1689(5) 0.1322(4) 0.2014(3) 0.0641(10) Uani 1 1 d . . .
H22A H 0.2509 0.0392 0.1844 0.096 Uiso 1 1 calc R . .
H22B H 0.0656 0.1184 0.2066 0.096 Uiso 1 1 calc R . .
H22C H 0.1913 0.1499 0.2581 0.096 Uiso 1 1 calc R . .
C23 C 0.3322(4) 0.6553(3) 0.1955(2) 0.0423(7) Uani 1 1 d . . .
H23A H 0.2786 0.7159 0.2433 0.051 Uiso 1 1 calc R . .
H23B H 0.3443 0.7279 0.1424 0.051 Uiso 1 1 calc R . .
C24 C 0.6098(5) 0.4628(5) 0.1236(3) 0.0806(13) Uani 1 1 d . . .
H24A H 0.7169 0.3884 0.1316 0.121 Uiso 1 1 calc R . .
H24B H 0.6149 0.5530 0.0814 0.121 Uiso 1 1 calc R . .
H24C H 0.5453 0.4142 0.1013 0.121 Uiso 1 1 calc R . .
H1A H -0.099(4) 0.994(4) 0.079(2) 0.034(8) Uiso 1 1 d . . .
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'
S S 0.1246 0.1234 '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
C4 N1 C1 115.1(2) . . ?
C23 S1 C24 100.88(19) . . ?
C1 O2 C12 114.7(2) . . ?
C2 O3 C13 112.69(19) . . ?
C21 O4 C20 118.2(3) . . ?
C3 O7 C23 118.1(2) . . ?
O2 C1 N1 112.3(2) . . ?
O2 C1 C2 105.3(2) . . ?
N1 C1 C2 103.3(2) . . ?
O2 C1 C5 110.8(2) . . ?
N1 C1 C5 110.0(2) . . ?
C2 C1 C5 114.9(2) . . ?
O3 C2 C1 108.7(2) . . ?
O3 C2 C3 113.7(2) . . ?
C1 C2 C3 103.6(2) . . ?
O7 C3 C20 105.8(2) . . ?
O7 C3 C4 115.0(2) . . ?
C20 C3 C4 106.4(2) . . ?
O7 C3 C2 114.7(2) . . ?
C20 C3 C2 111.2(2) . . ?
C4 C3 C2 103.6(2) . . ?
O6 C4 N1 126.8(3) . . ?
O6 C4 C3 124.7(3) . . ?
N1 C4 C3 108.4(2) . . ?
O1 C5 C6 121.6(2) . . ?
O1 C5 C1 118.5(2) . . ?
C6 C5 C1 119.8(2) . . ?
C11 C6 C7 118.8(3) . . ?
C11 C6 C5 123.8(2) . . ?
C7 C6 C5 117.4(2) . . ?
C8 C7 C6 120.2(3) . . ?
C9 C8 C7 120.5(3) . . ?
C10 C9 C8 119.6(3) . . ?
C9 C10 C11 120.7(3) . . ?
C10 C11 C6 120.2(3) . . ?
O3 C13 C14 108.9(2) . . ?
C15 C14 C19 118.2(3) . . ?
C15 C14 C13 120.6(3) . . ?
C19 C14 C13 121.1(3) . . ?
C14 C15 C16 120.5(3) . . ?
C17 C16 C15 120.5(3) . . ?
C16 C17 C18 119.4(3) . . ?
C19 C18 C17 120.4(3) . . ?
C18 C19 C14 121.0(3) . . ?
O4 C20 C3 109.1(2) . . ?
O5 C21 O4 122.1(4) . . ?
O5 C21 C22 125.6(3) . . ?
O4 C21 C22 112.1(3) . . ?
O7 C23 S1 108.14(18) . . ?
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 C4 1.325(4) . ?
N1 C1 1.435(3) . ?
S1 C23 1.774(3) . ?
S1 C24 1.782(4) . ?
O1 C5 1.200(3) . ?
O2 C1 1.412(3) . ?
O2 C12 1.419(4) . ?
O3 C2 1.402(3) . ?
O3 C13 1.428(3) . ?
O4 C21 1.317(4) . ?
O4 C20 1.421(4) . ?
O5 C21 1.197(5) . ?
O6 C4 1.219(3) . ?
O7 C3 1.405(3) . ?
O7 C23 1.424(3) . ?
C1 C2 1.541(4) . ?
C1 C5 1.542(4) . ?
C2 C3 1.545(4) . ?
C3 C20 1.519(4) . ?
C3 C4 1.527(4) . ?
C5 C6 1.481(4) . ?
C6 C11 1.380(4) . ?
C6 C7 1.384(4) . ?
C7 C8 1.373(4) . ?
C8 C9 1.370(5) . ?
C9 C10 1.359(5) . ?
C10 C11 1.376(4) . ?
C13 C14 1.493(4) . ?
C14 C15 1.379(4) . ?
C14 C19 1.378(4) . ?
C15 C16 1.380(4) . ?
C16 C17 1.360(4) . ?
C17 C18 1.374(5) . ?
C18 C19 1.365(4) . ?
C21 C22 1.488(5) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O6 0.80(3) 2.08(3) 2.867(3) 166(3) 2_575
N1 H1A N1 0.80(3) 3.17(3) 3.655(5) 122(2) 2_575
