#------------------------------------------------------------------------------
#$Date: 2017-10-13 09:09:21 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/20/01/2200153.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_2200153
loop_
_publ_author_name
'Scammells, Peter J.'
'Tranberg, C. Elisabet'
'Tiekink, Edward R. T. '
_publ_section_title
6,7-Dimethyl-5-phenyl-1H-thieno[2,3-e][1,4]diazepin-2(3H)-one
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o344
_journal_page_last               o345
_journal_paper_doi               10.1107/S1600536801004585
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'C15 H14 N2 O S'
_chemical_formula_moiety         'C15 H14 N2 O S'
_chemical_formula_sum            'C15 H14 N2 O S'
_chemical_formula_weight         270.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.115(6)
_cell_length_b                   10.4377(17)
_cell_length_c                   7.484(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10.3
_cell_measurement_theta_min      7.4
_cell_volume                     2664.9(12)
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1996)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Rigaku AFC-7R'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .7107
_diffrn_reflns_av_R_equivalents  .030
_diffrn_reflns_av_sigmaI/netI    .044
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5860
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        .64
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .236
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .31
_exptl_crystal_size_min          .18
_refine_diff_density_max         .40
_refine_diff_density_min         -.25
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          .080
_refine_ls_R_factor_gt           .045
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.1000P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .152
_reflns_number_gt                2084
_reflns_number_total             3057
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ci6018.cif
_cod_data_source_block           I
_cod_original_cell_volume        2664.7(13)
_cod_database_code               2200153
_cod_database_fobs_code          2200153
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'x-1/2, y, -z-1/2'
loop_
_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
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
S8 .955883(15) -.08457(5) .50528(7) .02942(18) Uani d . 1 . . S
O2 .98056(5) .15129(16) -.0480(2) .0359(4) Uani d . 1 . . O
N1 .96128(5) .01871(17) .1742(2) .0279(4) Uani d . 1 . . N
H1 .9790 -.0383 .1423 .084(3) Uiso calc R 1 . . H
N4 .88856(5) .16611(18) .0892(2) .0290(4) Uani d . 1 . . N
C2 .95891(6) .1303(2) .0795(3) .0280(5) Uani d . 1 . . C
C3 .92695(6) .2212(2) .1387(3) .0293(5) Uani d . 1 . . C
H3a .9283 .2338 .2697 .084(3) Uiso calc R 1 . . H
H3b .9304 .3054 .0801 .084(3) Uiso calc R 1 . . H
C8a .93706(6) -.0093(2) .3191(3) .0254(4) Uani d . 1 . . C
C5a .89758(6) .01687(19) .3362(3) .0260(4) Uani d . 1 . . C
C5 .87560(6) .0755(2) .1876(3) .0279(5) Uani d . 1 . . C
C6' .84207(7) .0070(3) .5753(4) .0418(6) Uani d . 1 . . C
H6a .8269 .0477 .4795 .084(3) Uiso calc R 1 . . H
H6b .8437 .0653 .6777 .084(3) Uiso calc R 1 . . H
H6c .8291 -.0725 .6119 .084(3) Uiso calc R 1 . . H
C6 .88275(6) -.0227(2) .5089(3) .0284(5) Uani d . 1 . . C
C7 .91090(7) -.0793(2) .6114(3) .0293(5) Uani d . 1 . . C
C7' .90801(8) -.1298(3) .7991(3) .0422(6) Uani d . 1 . . C
H7a .9334 -.1654 .8353 .084(3) Uiso calc R 1 . . H
H7b .8880 -.1970 .8042 .084(3) Uiso calc R 1 . . H
H7c .9008 -.0599 .8801 .084(3) Uiso calc R 1 . . H
C51 .83687(6) .0197(2) .1352(3) .0313(5) Uani d . 1 . . C
C52 .82830(7) -.1093(2) .1632(4) .0411(6) Uani d . 1 . . C
H52 .8464 -.1618 .2256 .084(3) Uiso calc R 1 . . H
C53 .79324(7) -.1622(3) .1004(4) .0499(7) Uani d . 1 . . C
H53 .7877 -.2503 .1198 .084(3) Uiso calc R 1 . . H
C54 .76674(7) -.0859(3) .0099(4) .0521(8) Uani d . 1 . . C
H54 .7430 -.1218 -.0338 .084(3) Uiso calc R 1 . . H
C55 .77466(7) .0421(3) -.0170(4) .0497(7) Uani d . 1 . . C
H55 .7562 .0943 -.0784 .084(3) Uiso calc R 1 . . H
C56 .80937(7) .0953(3) .0451(3) .0403(6) Uani d . 1 . . C
H56 .8145 .1837 .0264 .084(3) Uiso calc R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-2 -7 -2
-3 -4 -2
-2 -9 -2
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C8a S8 C7 91.50(11)
C2 N1 C8a 123.19(18)
C5 N4 C3 116.76(17)
O2 C2 N1 121.4(2)
O2 C2 C3 123.4(2)
N1 C2 C3 115.20(18)
N4 C3 C2 108.75(17)
C5a C8a N1 127.48(19)
C5a C8a S8 112.28(16)
N1 C8a S8 120.23(15)
C8a C5a C6 111.51(19)
C8a C5a C5 120.59(19)
C6 C5a C5 127.88(19)
N4 C5 C5a 124.46(19)
N4 C5 C51 116.26(19)
C5a C5 C51 119.06(18)
C7 C6 C5a 112.32(19)
C7 C6 C6' 123.6(2)
C5a C6 C6' 123.9(2)
C6 C7 C7' 129.1(2)
C6 C7 S8 112.36(17)
C7' C7 S8 118.45(18)
C52 C51 C56 118.4(2)
C52 C51 C5 121.44(19)
C56 C51 C5 120.0(2)
C51 C52 C53 120.7(2)
C54 C53 C52 119.8(3)
C55 C54 C53 120.1(2)
C54 C55 C56 120.4(3)
C51 C56 C55 120.6(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S8 C8a . 1.723(2) ?
S8 C7 . 1.729(2) ?
O2 C2 . 1.227(3) ?
N1 C2 . 1.365(3) ?
N1 C8a . 1.394(3) ?
N4 C5 . 1.278(3) ?
N4 C3 . 1.477(3) ?
C2 C3 . 1.512(3) ?
C8a C5a . 1.380(3) ?
C5a C6 . 1.448(3) ?
C5a C5 . 1.474(3) ?
C5 C51 . 1.496(3) ?
C6' C6 . 1.506(3) ?
C6 C7 . 1.364(3) ?
C7 C7' . 1.503(3) ?
C51 C52 . 1.394(3) ?
C51 C56 . 1.398(3) ?
C52 C53 . 1.399(3) ?
C53 C54 . 1.382(4) ?
C54 C55 . 1.378(5) ?
C55 C56 . 1.388(4) ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21132947
