#------------------------------------------------------------------------------
#$Date: 2024-07-05 18:36:09 +0300 (Fri, 05 Jul 2024) $
#$Revision: 292983 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/85/7248586.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_7248586
loop_
_publ_author_name
'Shaiwale, Mayuri'
'Som, Narayan N.'
'Jha, Prafulla K.'
'Ballabh, Amar'
_publ_section_title
;
 A simple and efficient synthesis of a series of
 N-(thiazol-2-yl)piperidine-2,6-dione compounds and their interesting NLO
 properties
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              3069
_journal_page_last               3076
_journal_paper_doi               10.1039/D4CE00217B
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C8 H8 N2 O2 S'
_chemical_formula_sum            'C8 H8 N2 O2 S'
_chemical_formula_weight         196.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_Int_Tables_number      43
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-07-04 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   22.635(4)
_cell_length_b                   18.2458(18)
_cell_length_c                   8.4549(12)
_cell_measurement_reflns_used    1255
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7630
_cell_measurement_theta_min      4.2110
_cell_volume                     3491.8(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0851
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.5623
_diffrn_measured_fraction_theta_max 0.5623
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     64.00  90.00   1.00   20.11    --   19.29  77.00 -90.00   26
  2  ω    -10.00  29.00   1.00   20.11    --   19.29  77.00-180.00   39
  3  ω     -2.00  78.00   1.00   20.11    --   19.29  77.00  60.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0156313000
_diffrn_orient_matrix_UB_12      -0.0327741000
_diffrn_orient_matrix_UB_13      -0.0167772000
_diffrn_orient_matrix_UB_21      0.0271284000
_diffrn_orient_matrix_UB_22      -0.0192217000
_diffrn_orient_matrix_UB_23      -0.0063165000
_diffrn_orient_matrix_UB_31      -0.0011343000
_diffrn_orient_matrix_UB_32      -0.0082143000
_diffrn_orient_matrix_UB_33      0.0819852000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2347
_diffrn_reflns_theta_full        28.8341
_diffrn_reflns_theta_max         28.83
_diffrn_reflns_theta_min         3.60
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.4929
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1634.7094
_refine_diff_density_max         0.1026
_refine_diff_density_min         -0.1123
_refine_diff_density_rms         0.0280
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.33(17)
_refine_ls_d_res_high            0.7369
_refine_ls_d_res_low             5.6588
_refine_ls_goodness_of_fit_ref   1.1032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    13
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1032
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0668P)²+0.7915P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.194
_reflns_limit_h_max              28
_reflns_limit_h_min              -28
_reflns_limit_k_max              24
_reflns_limit_k_min              -24
_reflns_limit_l_max              4
_reflns_limit_l_min              -11
_reflns_number_gt                1198
_reflns_number_total             1290
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ce00217b2.cif
_cod_data_source_block           exp_970
_cod_depositor_comments
'Adding full bibliography for 7248586--7248590.cif.'
_cod_original_cell_volume        3491.9(8)
_cod_original_sg_symbol_Hall     ' F 2 -2d'
_cod_database_code               7248586
_reflns_odcompleteness_completeness 98.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C4(H4a,H4b), C3(H3a,H3b)
2.b Aromatic/amide H refined with riding coordinates:
 C(H), C1(H1)
;
_olex2_date_sample_data_collection 2016-12-01
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.205
_oxdiff_exptl_absorpt_empirical_full_min 0.834
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,z
3 -x+1/4,y+1/4,z+1/4
4 x+1/4,-y+1/4,z+1/4
5 x,y+1/2,z+1/2
6 -x,-y+1/2,z+1/2
7 -x+1/4,y+3/4,z+3/4
8 x+1/4,-y+3/4,z+3/4
9 x+1/2,y,z+1/2
10 -x+1/2,-y,z+1/2
11 -x+3/4,y+1/4,z+3/4
12 x+3/4,-y+1/4,z+3/4
13 x+1/2,y+1/2,z
14 -x+1/2,-y+1/2,z
15 -x+3/4,y+3/4,z+1/4
16 x+3/4,-y+3/4,z+1/4
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_refinement_flags_posn
S10 S -0.71024(4) -0.36694(4) -1.41961(10) 0.0607(3) Uani 1.000000 .
N1 N -0.68280(8) -0.50814(9) -1.3591(3) 0.0389(4) Uani 1.000000 .
O12 O -0.60640(8) -0.50589(11) -1.5261(3) 0.0650(6) Uani 1.000000 .
C2 C -0.72889(11) -0.54339(15) -1.2835(4) 0.0537(7) Uani 1.000000 .
O11 O -0.76020(13) -0.50970(13) -1.1959(4) 0.0967(11) Uani 1.000000 .
C5 C -0.65762(13) -0.61789(13) -1.5131(3) 0.0498(6) Uani 1.000000 .
H5a H -0.63091(13) -0.64888(13) -1.4533(3) 0.0597(7) Uiso 1.000000 R
H5b H -0.64889(13) -0.62478(13) -1.6245(3) 0.0597(7) Uiso 1.000000 R
C4 C -0.71909(13) -0.64192(15) -1.4826(4) 0.0549(7) Uani 1.000000 .
H4a H -0.74570(13) -0.61800(15) -1.5563(4) 0.0659(8) Uiso 1.000000 R
H4b H -0.72225(13) -0.69446(15) -1.4980(4) 0.0659(8) Uiso 1.000000 R
C7 C -0.67314(10) -0.43352(12) -1.3225(3) 0.0418(5) Uani 1.000000 .
N8 N -0.63643(12) -0.41133(12) -1.2209(4) 0.0665(8) Uani 1.000000 .
C3 C -0.73588(12) -0.62283(14) -1.3174(5) 0.0572(8) Uani 1.000000 .
H3a H -0.71149(12) -0.65065(14) -1.2446(5) 0.0686(10) Uiso 1.000000 R
H3b H -0.77670(12) -0.63677(14) -1.2996(5) 0.0686(10) Uiso 1.000000 R
C6 C -0.64619(10) -0.54037(12) -1.4709(3) 0.0408(5) Uani 1.000000 .
C C -0.67316(13) -0.30417(14) -1.3130(4) 0.0593(7) Uani 1.000000 .
H H -0.67781(13) -0.25370(14) -1.3220(4) 0.0712(9) Uiso 1.000000 R
C1 C -0.63706(16) -0.33661(16) -1.2160(5) 0.0724(10) Uani 1.000000 .
H1 H -0.61299(16) -0.31033(16) -1.1472(5) 0.0869(12) Uiso 1.000000 R
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
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
C S10 C7 88.91(14) . . ?
C7 N1 C2 117.6(2) . . ?
C6 N1 C2 124.64(19) . . ?
C6 N1 C7 117.72(19) . . ?
O11 C2 N1 119.7(3) . . ?
C3 C2 N1 116.4(2) . . ?
C3 C2 O11 123.9(3) . . ?
C6 C5 C4 113.9(2) . . ?
C3 C4 C5 109.5(2) . . ?
N1 C7 S10 120.6(2) . . ?
N8 C7 S10 115.31(18) . . ?
N8 C7 N1 124.1(2) . . ?
C1 N8 C7 109.5(3) . . ?
C4 C3 C2 112.5(3) . . ?
O12 C6 N1 119.6(2) . . ?
C5 C6 N1 117.7(2) . . ?
C5 C6 O12 122.7(2) . . ?
C1 C S10 110.0(2) . . ?
C C1 N8 116.3(3) . . ?
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
S10 C7 1.690(2) . ?
S10 C 1.682(3) . ?
N1 C2 1.382(3) . ?
N1 C7 1.413(3) . ?
N1 C6 1.388(3) . ?
O12 C6 1.194(3) . ?
C2 O11 1.195(4) . ?
C2 C3 1.486(4) . ?
C5 C4 1.482(4) . ?
C5 C6 1.482(3) . ?
C4 C3 1.489(5) . ?
C7 N8 1.262(4) . ?
N8 C1 1.364(4) . ?
C C1 1.300(5) . ?
