#------------------------------------------------------------------------------
#$Date: 2021-12-15 05:06:27 +0200 (Wed, 15 Dec 2021) $
#$Revision: 271434 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243944.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_2243944
loop_
_publ_author_name
'Belov, Feodor'
'Villinger, Alexander'
'von Langermann, Jan'
_publ_section_title
;
(R)-Baclofen [(R)-4-amino-3-(4-chlorophenyl)butanoic acid]
;
_journal_coeditor_code YZ2013
_journal_issue 1
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989021012809
_journal_volume 78
_journal_year 2022
_chemical_absolute_configuration syn
_chemical_formula_iupac 'C10 H12 Cl N O2'
_chemical_formula_moiety 'C10 H12 Cl N O2'
_chemical_formula_sum 'C10 H12 Cl N O2'
_chemical_formula_weight 213.66
_chemical_name_common
;
(R)-Baclofen
;
_chemical_name_systematic
;
(R)-4-amino-3-(4-chlorophenyl)butanoic acid
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method SHELXL-2014/7
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 6.8913(5)
_cell_length_b 7.6898(5)
_cell_length_c 19.7527(14)
_cell_measurement_reflns_used 9871
_cell_measurement_temperature 123(2)
_cell_measurement_theta_max 32.97
_cell_measurement_theta_min 2.84
_cell_volume 1046.75(13)
_computing_cell_refinement
;
APEX2 (Bruker, 2003)
;
_computing_data_collection
;
APEX2 (Bruker, 2003)
;
_computing_data_reduction
;
SAINT (Bruker, 2003)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2014/7 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 123(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Bruker D8 QUEST diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0415
_diffrn_reflns_av_unetI/netI 0.0309
_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 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 23624
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 32.492
_diffrn_reflns_theta_min 2.062
_diffrn_source 'microfocus sealed tube'
_exptl_absorpt_coefficient_mu 0.338
_exptl_absorpt_correction_T_max 0.7465
_exptl_absorpt_correction_T_min 0.6617
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS2016/2; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.356
_exptl_crystal_description block
_exptl_crystal_F_000 448
_exptl_crystal_size_max 0.270
_exptl_crystal_size_mid 0.190
_exptl_crystal_size_min 0.160
_refine_diff_density_max 0.362
_refine_diff_density_min -0.302
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack 0.04(6)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.072
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 140
_refine_ls_number_reflns 3796
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.072
_refine_ls_R_factor_all 0.0405
_refine_ls_R_factor_gt 0.0334
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+0.2629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0787
_refine_ls_wR_factor_ref 0.0817
_reflns_number_gt 3447
_reflns_number_total 3796
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2013sup1.cif
_cod_data_source_block I
_cod_database_code 2243944
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.914
_shelx_estimated_absorpt_t_max 0.948
_shelx_hkl_file
;
-1 0 0 1.20 1.20
-1 0 0 3.50 1.00
-1 0 0 1.70 0.60
-1 0 0 2.30 0.80
1 0 0 1.60 1.20
1 0 0 2.40 1.00
1 0 0 0.60 0.60
-2 0 0 2839.92 84.69
-2 0 0 2954.40 85.19
2 0 0 2977.00 86.69
2 0 0 2842.92 86.19
2 0 0 2822.12 85.09
-2 0 0 2932.11 86.79
-2 0 0 2865.61 86.19
3 0 0 -0.10 3.20
3 0 0 0.60 2.40
3 0 0 6.20 2.20
-3 0 0 4.40 1.70
-3 0 0 -1.20 2.30
-3 0 0 -1.30 2.90
4 0 0 1199.88 40.20
4 0 0 1171.68 40.80
4 0 0 1155.98 37.80
-4 0 0 1218.68 38.00
-4 0 0 1171.68 39.90
-4 0 0 1218.18 41.30
-4 0 0 1175.88 37.20
-5 0 0 8.60 5.30
-5 0 0 7.20 5.10
-5 0 0 6.10 3.40
5 0 0 11.10 4.30
5 0 0 -0.10 7.30
5 0 0 3.90 3.20
6 0 0 1725.53 59.09
6 0 0 1726.83 55.09
-6 0 0 1646.94 60.19
-6 0 0 1758.12 54.19
7 0 0 -2.40 7.00
7 0 0 -1.10 5.40
-7 0 0 4.10 8.80
-7 0 0 10.40 7.30
-8 0 0 58.49 13.20
8 0 0 30.30 8.00
8 0 0 15.80 9.70
9 0 0 -9.10 10.10
9 0 0 -1.20 13.00
-9 0 0 6.30 16.00
-10 0 0 147.69 24.40
-10 0 0 105.09 21.80
10 0 0 84.99 19.30
0 1 0 1.50 0.70
0 -1 0 2.50 0.80
0 -1 0 3.90 0.90
0 -1 0 0.90 0.50
0 -1 0 2.30 0.70
-1 1 0 4.50 1.70
-1 1 0 1.50 1.60
1 -1 0 1.50 1.30
1 -1 0 3.30 1.60
-1 -1 0 7.00 1.30
-1 1 0 3.70 1.30
-1 1 0 4.90 1.50
1 1 0 4.60 1.30
1 -1 0 1.90 1.60
-1 -1 0 7.50 1.40
1 -1 0 5.10 1.50
-2 -1 0 2598.64 74.99
-2 1 0 2521.75 75.19
2 1 0 2577.04 74.89
2 -1 0 2425.76 74.79
2 1 0 2608.04 75.09
-2 -1 0 2585.74 75.49
-2 1 0 2484.15 74.89
2 1 0 2358.36 74.29
-2 1 0 2501.15 75.49
2 -1 0 2378.96 75.19
-2 -1 0 2507.55 74.39
-3 -1 0 404.36 14.50
-3 -1 0 411.26 15.60
-3 1 0 394.66 15.60
-3 1 0 381.36 15.10
3 1 0 404.76 16.10
3 1 0 394.06 15.60
3 -1 0 385.36 16.50
3 -1 0 383.36 16.00
-3 -1 0 430.96 16.90
3 -1 0 381.26 15.00
-3 1 0 399.66 16.70
4 -1 0 1957.90 63.49
4 1 0 2040.30 62.99
4 -1 0 2004.90 61.79
-4 -1 0 1981.00 60.99
-4 -1 0 2028.90 64.19
-4 1 0 1929.91 62.69
4 1 0 1975.60 63.29
-4 -1 0 2013.80 62.99
4 -1 0 1932.31 63.89
-4 1 0 1950.50 63.89
-4 1 0 2003.50 61.79
-5 -1 0 200.58 13.60
5 -1 0 201.08 12.50
5 -1 0 188.68 10.60
5 -1 0 208.48 15.60
-5 -1 0 205.88 10.80
5 1 0 222.08 14.70
-5 1 0 198.88 13.10
-5 -1 0 196.28 12.70
-5 1 0 184.28 13.20
5 1 0 208.18 12.20
6 -1 0 192.68 12.00
6 1 0 215.28 13.90
-6 1 0 210.88 15.70
6 -1 0 187.48 14.10
-6 -1 0 214.98 12.30
-6 -1 0 208.68 16.20
7 -1 0 256.97 18.50
-7 -1 0 213.78 20.50
-7 1 0 247.18 19.50
7 1 0 230.88 16.80
7 -1 0 253.47 15.10
8 -1 0 350.36 20.00
8 -1 0 346.57 23.50
-8 1 0 385.86 24.40
-8 -1 0 321.87 28.80
-8 1 0 359.36 27.00
8 1 0 382.26 23.50
-9 -1 0 4.20 17.60
9 -1 0 0.70 13.30
-9 1 0 1.90 16.10
-9 1 0 8.70 14.30
9 -1 0 5.90 11.00
9 1 0 7.60 13.10
-10 -1 0 62.39 25.30
10 -1 0 42.00 18.90
-10 1 0 78.99 22.00
-10 1 0 99.29 21.50
10 1 0 60.39 19.40
0 2 0 1840.22 55.79
0 -2 0 1834.82 55.19
0 -2 0 1854.41 55.19
0 2 0 1813.92 55.19
0 -2 0 1886.21 55.79
0 -2 0 1882.21 55.19
1 -2 0 7073.49 203.48
-1 -2 0 6800.92 203.08
-2 -2 0 12.00 2.30
-2 2 0 7.70 2.90
2 -2 0 13.60 3.20
-2 -2 0 12.90 2.70
2 -2 0 14.60 2.70
-2 2 0 20.80 3.40
2 -2 0 12.30 3.10
2 2 0 12.30 2.30
-2 2 0 15.40 2.60
-2 -2 0 10.70 2.10
-3 2 0 1080.09 34.80
-3 -2 0 1027.70 34.60
3 2 0 993.30 33.10
-3 2 0 1056.79 34.10
-3 2 0 1037.50 33.80
3 2 0 1005.30 31.70
-3 2 0 1032.60 36.70
-3 -2 0 1026.80 33.60
-3 -2 0 1015.00 33.40
3 -2 0 979.90 34.50
3 -2 0 1073.79 35.20
3 -2 0 999.40 34.90
-4 -2 0 428.46 17.00
4 -2 0 397.06 19.30
-4 2 0 440.26 18.40
4 -2 0 418.76 18.30
-4 -2 0 463.05 19.10
4 -2 0 412.96 17.40
-4 2 0 419.56 18.60
-4 -2 0 446.16 18.00
4 2 0 453.65 17.30
4 2 0 448.36 17.90
-4 2 0 407.76 17.70
-5 -2 0 154.38 12.70
5 2 0 148.09 10.40
-5 2 0 167.68 11.30
5 2 0 146.59 12.90
5 -2 0 152.28 10.00
-5 2 0 134.39 12.30
-5 2 0 181.08 12.70
-5 -2 0 149.59 10.30
5 -2 0 156.08 11.30
-5 -2 0 133.09 12.00
-6 2 0 396.46 20.50
-6 2 0 416.56 22.30
-6 -2 0 388.26 22.40
6 2 0 412.36 19.50
6 2 0 368.26 21.30
6 -2 0 413.76 21.20
6 -2 0 428.86 19.00
-7 2 0 25.30 8.10
-7 -2 0 31.60 10.70
7 -2 0 25.20 7.20
-7 2 0 31.60 9.80
7 -2 0 30.10 8.50
7 2 0 20.30 7.70
-8 -2 0 13.30 13.40
-8 2 0 -10.00 11.80
8 -2 0 12.00 10.80
8 -2 0 -0.60 8.60
-8 2 0 11.10 11.10
8 2 0 4.50 9.70
9 -2 0 7.70 11.70
9 2 0 -0.50 8.80
9 2 0 -3.70 13.10
-9 2 0 8.80 15.60
-9 2 0 1.10 15.20
-9 -2 0 23.50 17.40
9 -2 0 -4.10 14.70
10 -2 0 53.89 22.40
-10 2 0 63.59 22.00
10 -2 0 47.40 16.60
-10 -2 0 45.70 24.00
-10 2 0 58.09 23.60
10 2 0 10.40 19.10
0 3 0 2.40 2.00
0 -3 0 -1.20 1.50
0 -3 0 0.90 1.40
0 -3 0 1.00 1.80
0 3 0 0.70 1.50
-1 -3 0 883.21 27.20
1 -3 0 860.51 28.70
-1 -3 0 856.41 28.40
-1 3 0 887.21 29.30
1 -3 0 842.42 27.10
1 -3 0 881.61 29.00
-1 -3 0 902.61 28.90
1 3 0 881.11 28.50
-1 3 0 845.72 27.20
1 3 0 867.61 27.40
2 -3 0 228.98 10.20
-2 -3 0 244.28 10.70
2 3 0 226.38 11.30
2 -3 0 228.68 13.40
2 -3 0 244.78 11.00
2 -3 0 225.58 10.50
-3 -3 0 5031.40 145.49
-3 3 0 4812.82 145.19
3 -3 0 4872.21 147.19
-3 3 0 4862.21 147.89
3 -3 0 4788.52 146.99
-3 3 0 4996.90 147.49
-3 -3 0 4873.01 146.29
3 3 0 4836.32 146.09
-3 -3 0 5078.49 146.39
4 -3 0 65.09 10.80
-4 -3 0 62.49 8.20
-4 -3 0 50.79 7.20
4 -3 0 69.09 7.40
-4 3 0 69.69 7.80
-4 3 0 74.09 7.90
4 3 0 53.19 6.00
-4 3 0 62.39 7.70
-4 -3 0 67.99 7.90
4 -3 0 61.99 6.90
5 3 0 90.09 8.70
5 -3 0 92.69 10.00
-5 -3 0 99.29 11.60
-5 -3 0 124.99 16.70
-5 3 0 98.69 10.40
-5 -3 0 112.59 18.30
5 -3 0 99.49 9.50
-5 3 0 90.79 11.50
-5 3 0 92.79 10.60
5 3 0 83.69 10.30
-6 3 0 5.10 6.60
-6 3 0 -2.40 7.00
6 3 0 2.30 5.60
-6 -3 0 13.30 8.10
6 -3 0 2.00 5.40
6 3 0 -4.90 7.90
6 -3 0 2.50 6.30
-7 -3 0 70.89 13.00
7 -3 0 61.69 9.10
7 -3 0 84.19 14.50
-7 3 0 63.59 11.30
-7 3 0 67.09 11.20
7 3 0 65.69 9.20
8 -3 0 166.58 21.20
8 -3 0 172.38 18.10
8 3 0 186.08 18.40
-8 -3 0 170.28 24.60
-8 3 0 154.78 21.30
-9 3 0 118.39 18.70
-9 3 0 123.99 19.80
-9 -3 0 104.99 21.40
9 3 0 102.79 15.00
9 -3 0 112.19 15.10
9 -3 0 107.19 18.10
10 3 0 -6.10 18.70
-10 -3 0 -2.40 28.20
-10 3 0 18.00 22.50
10 -3 0 -5.00 22.70
-10 3 0 37.10 23.00
10 -3 0 -18.10 17.40
0 4 0 328.97 15.40
0 -4 0 347.27 13.30
0 -4 0 328.97 14.20
0 -4 0 358.26 13.50
0 4 0 351.86 13.50
0 -4 0 342.27 13.40
1 -4 0 3792.32 112.29
-1 -4 0 3647.84 110.09
1 -4 0 3660.63 113.99
-1 4 0 3699.83 112.59
1 -4 0 3655.03 110.09
-1 4 0 3606.54 110.09
-1 -4 0 3796.72 111.59
1 -4 0 3813.52 111.99
1 4 0 3686.63 111.39
-1 -4 0 3815.82 112.19
2 -4 0 355.86 15.60
2 -4 0 365.36 15.70
-2 -4 0 388.16 15.60
2 4 0 382.56 15.40
2 -4 0 366.06 14.50
-2 -4 0 385.76 15.60
2 4 0 372.26 13.60
-2 4 0 371.36 16.40
-3 4 0 2086.29 66.79
-3 -4 0 2132.69 65.79
3 4 0 2128.59 65.59
3 -4 0 1980.60 65.59
3 -4 0 1947.21 65.49
3 -4 0 2147.09 65.69
3 -4 0 2089.19 66.49
4 -4 0 1170.78 40.30
4 4 0 1132.09 39.00
-4 -4 0 1163.48 38.70
4 -4 0 1019.00 40.40
4 -4 0 1115.39 40.10
-4 4 0 1128.39 40.90
-4 4 0 1152.98 38.60
-4 -4 0 1219.78 40.20
-5 4 0 1048.30 39.60
5 -4 0 1101.69 41.20
-5 4 0 1100.69 38.60
-5 4 0 1081.39 41.40
-5 -4 0 1242.98 42.50
5 -4 0 1102.59 40.90
6 -4 0 98.99 11.80
6 -4 0 88.79 12.80
-6 4 0 96.59 13.10
-6 -4 0 87.69 15.30
-6 4 0 93.69 13.60
-7 4 0 265.07 21.20
-7 -4 0 239.08 24.10
7 -4 0 235.78 18.20
7 -4 0 229.48 19.40
-7 4 0 258.47 20.00
-8 -4 0 91.19 18.20
-8 4 0 81.69 15.40
-8 4 0 81.89 17.00
8 -4 0 90.69 14.80
9 -4 0 26.10 13.90
9 -4 0 38.80 16.60
-9 -4 0 17.60 22.90
-9 4 0 37.40 16.80
-9 4 0 49.00 18.40
0 -5 0 1.60 2.80
0 5 0 2.00 3.00
0 -5 0 1.00 2.50
0 -5 0 2.30 2.80
0 -5 0 0.40 3.60
0 5 0 5.10 2.60
1 -5 0 468.35 19.20
-1 -5 0 500.45 18.00
1 -5 0 492.85 19.90
1 -5 0 492.85 18.00
-1 -5 0 527.75 19.50
1 5 0 499.35 19.20
-1 5 0 486.05 20.40
-1 -5 0 501.55 20.00
1 -5 0 494.95 19.50
-2 -5 0 154.68 10.10
-2 5 0 160.28 10.80
2 -5 0 160.88 10.00
-2 5 0 149.88 7.60
-2 -5 0 141.09 7.20
2 5 0 153.58 9.30
2 -5 0 143.59 10.00
2 -5 0 146.99 10.60
-2 -5 0 141.49 9.50
3 -5 0 882.11 30.70
-3 5 0 868.31 32.80
-3 -5 0 840.42 31.40
3 5 0 878.51 31.10
3 -5 0 859.81 31.90
3 -5 0 798.42 31.00
4 5 0 2081.69 65.99
-4 -5 0 2166.28 66.29
-4 5 0 1904.51 67.89
4 -5 0 1986.90 66.39
4 -5 0 1978.10 67.19
-4 -5 0 2042.10 64.09
-5 5 0 148.19 14.00
5 -5 0 139.69 12.60
5 -5 0 151.08 13.20
-5 -5 0 141.39 14.80
6 -5 0 125.79 15.40
6 -5 0 121.59 13.30
-6 5 0 112.29 15.70
-6 5 0 121.79 13.80
-6 -5 0 157.68 18.60
7 -5 0 43.40 10.10
7 -5 0 39.20 11.10
-7 -5 0 60.89 14.60
-7 5 0 32.60 10.30
-8 5 0 65.39 16.10
8 -5 0 83.09 13.60
8 -5 0 72.19 15.10
-8 5 0 86.69 16.80
-9 5 0 53.19 21.20
9 -5 0 26.00 15.90
-9 5 0 -2.80 17.70
9 -5 0 17.50 19.00
-9 -5 0 11.50 25.20
0 -6 0 1143.69 41.40
0 6 0 1243.68 40.20
0 -6 0 1249.18 40.50
0 -6 0 1198.28 40.20
0 -6 0 1189.88 40.00
0 6 0 1160.18 41.60
-1 -6 0 66.99 8.40
1 -6 0 58.29 7.00
-1 6 0 69.69 6.50
1 6 0 61.89 7.00
1 -6 0 71.49 6.80
-1 -6 0 78.49 8.90
-1 6 0 56.59 8.10
1 -6 0 72.39 8.80
-1 -6 0 72.19 6.60
-2 -6 0 316.57 13.10
-2 6 0 322.17 17.40
-2 6 0 330.87 13.40
2 -6 0 324.57 16.10
2 6 0 330.57 15.60
3 -6 0 67.59 8.40
-3 6 0 88.89 11.00
3 -6 0 91.19 9.30
3 6 0 94.19 8.70
4 -6 0 253.27 16.00
4 6 0 277.57 15.00
-4 6 0 243.28 17.00
4 -6 0 275.27 16.00
5 -6 0 260.47 16.70
-5 -6 0 230.08 18.00
-5 6 0 233.58 18.00
5 -6 0 231.88 17.00
6 -6 0 151.68 17.60
6 -6 0 152.98 16.10
-6 6 0 147.99 18.90
-6 -6 0 162.98 21.10
7 -6 0 6.50 11.00
-7 6 0 24.20 14.00
-7 -6 0 8.70 16.60
8 -6 0 -15.70 16.30
-8 6 0 1.80 18.00
-8 -6 0 -17.50 22.50
8 -6 0 -0.40 13.90
9 -6 0 34.80 18.30
-9 6 0 -3.60 24.90
9 -6 0 53.29 21.40
-9 -6 0 50.49 27.90
0 -7 0 -0.40 3.50
0 7 0 -4.60 4.40
0 -7 0 -8.40 5.00
0 7 0 0.80 3.80
1 7 0 35.40 6.10
1 -7 0 32.80 6.00
-1 7 0 38.60 7.50
-1 7 0 35.40 5.30
1 -7 0 25.30 5.20
-1 -7 0 19.50 5.00
2 -7 0 1.60 4.40
-2 7 0 2.80 5.40
-2 7 0 3.80 3.80
-2 -7 0 4.50 3.80
2 7 0 9.00 4.50
-3 7 0 30.60 7.40
3 -7 0 16.90 6.30
3 7 0 21.60 5.30
-4 7 0 128.89 15.30
4 -7 0 135.29 13.40
4 7 0 152.38 12.60
4 -7 0 151.38 13.50
5 -7 0 640.84 30.00
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0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 90077
_shelx_res_file
;
shelx.res created by SHELXL-2014/7
TITL is_rbaclofenkrsitall in P2(1)2(1)2(1)
CELL 0.71073 6.8913 7.6898 19.7527 90.000 90.000 90.000
ZERR 4.00 0.0005 0.0005 0.0014 0.000 0.000 0.000
LATT -1
SYMM 1/2 - X, - Y, 1/2 + Z
SYMM - X, 1/2 + Y, 1/2 - Z
SYMM 1/2 + X, 1/2 - Y, - Z
SFAC C H CL N O
UNIT 40 48 4 4 8
MERG 2
OMIT -3.00 65.00
TWIN
FMAP 2
PLAN 20
SIZE 0.160 0.190 0.270
ACTA
BOND $H
EQIV $1 x-1/2, -y+1/2, -z+1
EQIV $4 x+1/2, -y+1/2, -z+1
EQIV $5 x, y+1, z
EQIV $6 -x+3/2, -y+1, z-1/2
EQIV $7 -x+1, y+1/2, -z+3/2
EQIV $8 -x+2, y+1/2, -z+3/2
EQIV $9 -x+1, y+1/2, -z+3/2
HTAB N1 O2_$4
HTAB N1 O2_$5
HTAB N1 O1_$1
HTAB N1 Cl1_$6
HTAB C4 Cl1_$7
HTAB C4 Cl1_$8
MPLA 6 C5 C6 C7 C8 C9 C10 H9_$8 H6_$9
MPLA 6 C5_$8 C6_$8 C7_$8 C8_$8 C9_$8 C10_$8
MPLA 6 C5_$6 C6_$6 C7_$6 C8_$6 C9_$6 C10_$6
CONF
LIST 4
L.S. 12
TEMP -150.15
WGHT 0.037200 0.262900
BASF 0.04470
FVAR 1.12981
CL1 3 0.908260 0.160659 0.883038 11.00000 0.02181 0.03351 =
0.01578 0.00057 -0.00328 0.00413
N1 4 0.584231 0.602600 0.523524 11.00000 0.01344 0.00943 =
0.01743 0.00001 -0.00125 0.00029
O1 5 0.760644 0.020924 0.544922 11.00000 0.01521 0.01726 =
0.02585 -0.00548 0.00313 0.00164
O2 5 0.453418 -0.066020 0.536360 11.00000 0.01667 0.00957 =
0.02723 -0.00108 -0.00269 -0.00111
C1 1 0.582469 0.046648 0.549373 11.00000 0.01564 0.00969 =
0.01168 0.00090 0.00031 0.00064
C2 1 0.508521 0.225527 0.570658 11.00000 0.01469 0.00913 =
0.02025 -0.00181 -0.00252 0.00056
AFIX 23
H2A 2 0.408068 0.209775 0.605959 11.00000 -1.20000
H2B 2 0.445407 0.280918 0.531134 11.00000 -1.20000
AFIX 0
C3 1 0.664298 0.349664 0.598008 11.00000 0.01303 0.00986 =
0.01441 -0.00099 -0.00126 0.00132
AFIX 13
H3 2 0.781795 0.337840 0.568658 11.00000 -1.20000
AFIX 0
C4 1 0.596574 0.538837 0.594293 11.00000 0.01592 0.01039 =
0.01553 -0.00120 -0.00118 0.00148
AFIX 23
H4A 2 0.467440 0.548976 0.615896 11.00000 -1.20000
H4B 2 0.688167 0.612962 0.619948 11.00000 -1.20000
AFIX 0
C5 1 0.723051 0.303418 0.670123 11.00000 0.01331 0.01002 =
0.01692 -0.00098 -0.00128 0.00062
C6 1 0.614844 0.358158 0.725944 11.00000 0.01463 0.01461 =
0.01865 0.00115 0.00152 0.00279
AFIX 43
H6 2 0.500475 0.424775 0.718984 11.00000 -1.20000
AFIX 0
C7 1 0.671908 0.316619 0.791916 11.00000 0.01863 0.01707 =
0.01629 0.00037 0.00287 0.00100
AFIX 43
H7 2 0.598637 0.355958 0.829667 11.00000 -1.20000
AFIX 0
C8 1 0.837038 0.217177 0.801192 11.00000 0.01885 0.01878 =
0.01511 0.00020 -0.00246 0.00010
C9 1 0.945880 0.158996 0.746842 11.00000 0.01998 0.02761 =
0.01939 0.00015 -0.00341 0.01146
AFIX 43
H9 2 1.058041 0.089552 0.753985 11.00000 -1.20000
AFIX 0
C10 1 0.888640 0.203681 0.681653 11.00000 0.01875 0.02429 =
0.01692 -0.00300 -0.00146 0.00900
AFIX 43
H10 2 0.963900 0.165472 0.644204 11.00000 -1.20000
AFIX 0
H1A 2 0.701177 0.586122 0.503113 11.00000 0.04379
H1B 2 0.554866 0.720539 0.524484 11.00000 0.02174
H1C 2 0.489826 0.557247 0.502105 11.00000 0.02915
HKLF 4
REM is_rbaclofenkrsitall in P2(1)2(1)2(1)
REM R1 = 0.0334 for 3447 Fo > 4sig(Fo) and 0.0405 for all 3796 data
REM 140 parameters refined using 0 restraints
END
WGHT 0.0372 0.2629
REM Highest difference peak 0.362, deepest hole -0.302, 1-sigma level 0.052
Q1 1 0.7009 0.3195 0.6345 11.00000 0.05 0.36
Q2 1 0.9060 0.1682 0.8418 11.00000 0.05 0.36
Q3 1 0.9135 0.1821 0.7140 11.00000 0.05 0.35
Q4 1 0.5861 0.5637 0.5601 11.00000 0.05 0.32
Q5 1 0.6501 0.3326 0.7563 11.00000 0.05 0.30
Q6 1 0.8043 0.2539 0.6755 11.00000 0.05 0.30
Q7 1 0.7554 0.2648 0.7977 11.00000 0.05 0.27
Q8 1 0.5409 0.1291 0.5574 11.00000 0.05 0.24
Q9 1 0.6020 0.2861 0.5923 11.00000 0.05 0.23
Q10 1 0.9009 0.1670 0.7801 11.00000 0.05 0.22
Q11 1 0.6374 0.3452 0.6902 11.00000 0.05 0.22
Q12 1 0.9004 0.1629 0.9198 11.00000 0.05 0.20
Q13 1 0.6825 0.3010 0.7058 11.00000 0.05 0.20
Q14 1 0.6425 0.4533 0.5968 11.00000 0.05 0.20
Q15 1 0.9816 0.2413 0.8780 11.00000 0.05 0.19
Q16 1 0.5191 -0.0215 0.5441 11.00000 0.05 0.19
Q17 1 0.4228 -0.0380 0.5641 11.00000 0.05 0.18
Q18 1 0.7540 0.3310 0.5943 11.00000 0.05 0.18
Q19 1 0.5792 0.5585 0.6326 11.00000 0.05 0.17
Q20 1 0.9958 -0.0720 0.7706 11.00000 0.05 0.16
;
_shelx_res_checksum 7002
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_type_symbol
_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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl Cl1 0.90826(7) 0.16066(7) 0.88304(2) 0.02370(11) Uani d 1 . .
N N1 0.5842(2) 0.60260(18) 0.52352(7) 0.0134(2) Uani d 1 . .
O O1 0.76064(19) 0.02092(17) 0.54492(7) 0.0194(3) Uani d 1 . .
O O2 0.45342(19) -0.06602(16) 0.53636(7) 0.0178(3) Uani d 1 . .
C C1 0.5825(3) 0.0466(2) 0.54937(7) 0.0123(3) Uani d 1 . .
C C2 0.5085(2) 0.2255(2) 0.57066(9) 0.0147(3) Uani d 1 . .
H H2A 0.4081 0.2098 0.6060 0.018 Uiso calc 1 . .
H H2B 0.4454 0.2809 0.5311 0.018 Uiso calc 1 . .
C C3 0.6643(2) 0.3497(2) 0.59801(8) 0.0124(3) Uani d 1 . .
H H3 0.7818 0.3378 0.5687 0.015 Uiso calc 1 . .
C C4 0.5966(3) 0.5388(2) 0.59429(8) 0.0139(3) Uani d 1 . .
H H4A 0.4674 0.5490 0.6159 0.017 Uiso calc 1 . .
H H4B 0.6882 0.6130 0.6199 0.017 Uiso calc 1 . .
C C5 0.7231(2) 0.3034(2) 0.67012(8) 0.0134(3) Uani d 1 . .
C C6 0.6148(2) 0.3582(2) 0.72594(8) 0.0160(3) Uani d 1 . .
H H6 0.5005 0.4248 0.7190 0.019 Uiso calc 1 . .
C C7 0.6719(3) 0.3166(2) 0.79192(8) 0.0173(3) Uani d 1 . .
H H7 0.5986 0.3560 0.8297 0.021 Uiso calc 1 . .
C C8 0.8370(3) 0.2172(2) 0.80119(8) 0.0176(3) Uani d 1 . .
C C9 0.9459(3) 0.1590(3) 0.74684(9) 0.0223(4) Uani d 1 . .
H H9 1.0580 0.0896 0.7540 0.027 Uiso calc 1 . .
C C10 0.8886(3) 0.2037(2) 0.68165(8) 0.0200(3) Uani d 1 . .
H H10 0.9639 0.1655 0.6442 0.024 Uiso calc 1 . .
H H1A 0.701(5) 0.586(4) 0.5031(16) 0.044(8) Uiso d 1 . .
H H1B 0.555(4) 0.721(3) 0.5245(11) 0.022(6) Uiso d 1 . .
H H1C 0.490(4) 0.557(4) 0.5021(14) 0.029(7) Uiso d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cl1 0.02181(19) 0.0335(2) 0.01578(16) 0.0041(2) -0.00328(16) 0.00057(16)
N1 0.0134(6) 0.0094(6) 0.0174(6) 0.0003(5) -0.0012(5) 0.0000(4)
O1 0.0152(6) 0.0173(6) 0.0258(6) 0.0016(5) 0.0031(5) -0.0055(5)
O2 0.0167(6) 0.0096(5) 0.0272(6) -0.0011(4) -0.0027(5) -0.0011(5)
C1 0.0156(7) 0.0097(6) 0.0117(6) 0.0006(6) 0.0003(6) 0.0009(5)
C2 0.0147(7) 0.0091(6) 0.0202(7) 0.0006(6) -0.0025(6) -0.0018(6)
C3 0.0130(6) 0.0099(6) 0.0144(6) 0.0013(6) -0.0013(5) -0.0010(5)
C4 0.0159(7) 0.0104(6) 0.0155(6) 0.0015(6) -0.0012(6) -0.0012(5)
C5 0.0133(7) 0.0100(7) 0.0169(7) 0.0006(5) -0.0013(5) -0.0010(5)
C6 0.0146(7) 0.0146(7) 0.0187(7) 0.0028(6) 0.0015(5) 0.0012(6)
C7 0.0186(7) 0.0171(8) 0.0163(7) 0.0010(7) 0.0029(6) 0.0004(6)
C8 0.0188(8) 0.0188(8) 0.0151(7) 0.0001(6) -0.0025(6) 0.0002(6)
C9 0.0200(9) 0.0276(9) 0.0194(7) 0.0115(8) -0.0034(6) 0.0002(7)
C10 0.0188(8) 0.0243(9) 0.0169(7) 0.0090(7) -0.0015(6) -0.0030(6)
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C4 N1 H1A . . 109(2) ?
C4 N1 H1B . . 108.4(14) ?
H1A N1 H1B . . 110(3) ?
C4 N1 H1C . . 112.1(19) ?
H1A N1 H1C . . 114(2) ?
H1B N1 H1C . . 104(2) ?
O1 C1 O2 . . 124.61(16) ?
O1 C1 C2 . . 119.43(15) ?
O2 C1 C2 . . 115.95(15) ?
C1 C2 C3 . . 115.09(14) ?
C1 C2 H2A . . 108.5 ?
C3 C2 H2A . . 108.5 ?
C1 C2 H2B . . 108.5 ?
C3 C2 H2B . . 108.5 ?
H2A C2 H2B . . 107.5 ?
C5 C3 C4 . . 110.37(13) ?
C5 C3 C2 . . 111.71(14) ?
C4 C3 C2 . . 111.18(13) ?
C5 C3 H3 . . 107.8 ?
C4 C3 H3 . . 107.8 ?
C2 C3 H3 . . 107.8 ?
N1 C4 C3 . . 112.15(12) ?
N1 C4 H4A . . 109.2 ?
C3 C4 H4A . . 109.2 ?
N1 C4 H4B . . 109.2 ?
C3 C4 H4B . . 109.2 ?
H4A C4 H4B . . 107.9 ?
C10 C5 C6 . . 118.31(15) ?
C10 C5 C3 . . 119.94(14) ?
C6 C5 C3 . . 121.76(14) ?
C5 C6 C7 . . 121.13(15) ?
C5 C6 H6 . . 119.4 ?
C7 C6 H6 . . 119.4 ?
C8 C7 C6 . . 118.76(15) ?
C8 C7 H7 . . 120.6 ?
C6 C7 H7 . . 120.6 ?
C7 C8 C9 . . 121.46(16) ?
C7 C8 Cl1 . . 119.47(13) ?
C9 C8 Cl1 . . 119.07(14) ?
C8 C9 C10 . . 119.01(16) ?
C8 C9 H9 . . 120.5 ?
C10 C9 H9 . . 120.5 ?
C9 C10 C5 . . 121.32(16) ?
C9 C10 H10 . . 119.3 ?
C5 C10 H10 . . 119.3 ?
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
Cl1 C8 . 1.7445(17) ?
N1 C4 . 1.484(2) ?
N1 H1A . 0.91(3) ?
N1 H1B . 0.93(3) ?
N1 H1C . 0.85(3) ?
O1 C1 . 1.247(2) ?
O2 C1 . 1.268(2) ?
C1 C2 . 1.526(2) ?
C2 C3 . 1.535(2) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 C5 . 1.523(2) ?
C3 C4 . 1.529(2) ?
C3 H3 . 1.0000 ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 C10 . 1.394(2) ?
C5 C6 . 1.396(2) ?
C6 C7 . 1.398(2) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.383(3) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.384(2) ?
C9 C10 . 1.390(2) ?
C9 H9 . 0.9500 ?
C10 H10 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1A O2 4_556 0.91(3) 1.91(3) 2.820(2) 176(3)
N1 H1B O2 1_565 0.93(3) 1.80(3) 2.7149(19) 168(2)
N1 H1C O1 4_456 0.85(3) 1.93(3) 2.775(2) 174(3)
N1 H1B Cl1 2_664 0.93(3) 2.95(2) 3.3192(14) 105.3(16)
C4 H4A Cl1 3_656 0.99 2.73 3.6306(19) 151.8
C4 H4B Cl1 3_756 0.99 2.81 3.5668(19) 134.1
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1 C1 C2 C3 . . . . -11.2(2) ?
O2 C1 C2 C3 . . . . 169.78(14) ?
C1 C2 C3 C5 . . . . -76.36(17) ?
C1 C2 C3 C4 . . . . 159.86(13) ?
C5 C3 C4 N1 . . . . 165.95(14) ?
C2 C3 C4 N1 . . . . -69.51(18) ?
C4 C3 C5 C10 . . . . -138.39(16) ?
C2 C3 C5 C10 . . . . 97.37(19) ?
C4 C3 C5 C6 . . . . 41.7(2) ?
C2 C3 C5 C6 . . . . -82.53(19) ?
C10 C5 C6 C7 . . . . 0.9(3) ?
C3 C5 C6 C7 . . . . -179.16(16) ?
C5 C6 C7 C8 . . . . -1.0(3) ?
C6 C7 C8 C9 . . . . 0.1(3) ?
C6 C7 C8 Cl1 . . . . -178.86(14) ?
C7 C8 C9 C10 . . . . 0.8(3) ?
Cl1 C8 C9 C10 . . . . 179.81(16) ?
C8 C9 C10 C5 . . . . -0.9(3) ?
C6 C5 C10 C9 . . . . 0.0(3) ?
C3 C5 C10 C9 . . . . -179.86(18) ?
_cod_database_fobs_code 2243944