#------------------------------------------------------------------------------
#$Date: 2018-03-16 09:07:53 +0200 (Fri, 16 Mar 2018) $
#$Revision: 206982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/24/2242429.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_2242429
loop_
_publ_author_name
'Ou\'edraogo, Mohammad'
'Abou, Akoun'
'Djand\'e, Abdoulaye'
'Ouari, Olivier'
'Zoueu, T. J\'er\'emie'
_publ_section_title
;
2-Oxo-2H-chromen-7-yl 4-tert-butylbenzoate
;
_journal_coeditor_code SJ5549
_journal_issue 4
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 530
_journal_page_last 534
_journal_paper_doi 10.1107/S2056989018004188
_journal_volume 74
_journal_year 2018
_chemical_formula_iupac 'C20 H18 O4'
_chemical_formula_moiety 'C20 H18 O4'
_chemical_formula_sum 'C20 H18 O4'
_chemical_formula_weight 322.34
_chemical_melting_point_gt 406
_chemical_melting_point_lt 408
_chemical_name_common 'Coumarin ester'
_chemical_name_systematic
;
2-Oxo-2H-chromen-7-yl 4-tert-butylbenzoate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2014/7
_cell_angle_alpha 90
_cell_angle_beta 93.627(11)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 18.684(2)
_cell_length_b 6.5431(5)
_cell_length_c 13.6688(14)
_cell_measurement_reflns_used 1499
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 63.4210
_cell_measurement_theta_min 4.7300
_cell_volume 1667.7(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
PLATON (Spek,2009) and Mercury (Macrae et al., 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015), publCIF (Westrip, 2010) and WinGX
(Farrugia,
2012)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2014 (Burla et al., 2015)
;
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 5.3048
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction SuperNova, Dual, Cu at zero, Atlas S2'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0350
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 9647
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 67.722
_diffrn_reflns_theta_min 4.743
_exptl_absorpt_coefficient_mu 0.726
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.71393
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.284
_exptl_crystal_description prism
_exptl_crystal_F_000 680
_exptl_crystal_size_max .40
_exptl_crystal_size_mid .12
_exptl_crystal_size_min .04
_refine_diff_density_max 0.144
_refine_diff_density_min -0.130
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.009
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_constraints 72
_refine_ls_number_parameters 217
_refine_ls_number_reflns 3005
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.009
_refine_ls_R_factor_all 0.0942
_refine_ls_R_factor_gt 0.0569
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0981P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1610
_refine_ls_wR_factor_ref 0.2015
_reflns_number_gt 1710
_reflns_number_total 3005
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file sj5549sup1.cif
_cod_data_source_block I
_cod_database_code 2242429
_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_hkl_file
;
-2 0 0 34421.0 314.657 2
2 0 0 33390.8 449.729 4
-3 0 0 13260.8 227.455 2
3 0 0 13479.6 351.057 4
-4 0 0 6717.05 178.547 2
4 0 0 6799.82 289.223 4
5 0 0 14887.1 485.109 4
-5 0 0 13743.9 271.904 2
6 0 0 24645.6 692.864 4
6 0 0 25153.2 563.026 6
7 0 0 23141.2 579.477 6
8 0 0 53919.5 974.335 6
9 0 0 38957.2 893.607 6
10 0 0 3229.62 281.082 6
11 0 0 2433.27 267.038 6
12 0 0 64.0815 39.7782 6
13 0 0 840.861 187.492 6
-13 0 0 944.884 188.050 5
-14 0 0 87.1761 66.3770 5
14 0 0 245.499 128.079 6
15 0 0 281.959 98.5820 6
-15 0 0 372.412 143.639 5
-16 0 0 58.5229 30.9143 31
-17 0 0 221.500 52.7528 31
-18 0 0 100.786 37.6655 31
-19 0 0 58.2898 33.5353 31
-20 0 0 0.88140 16.0357 31
-21 0 0 16.4267 17.1941 31
-22 0 0 21.0584 11.8355 31
0 1 0-6.64810 24.2632 3
0 -1 0-6.79662 20.4659 1
1 -1 0 392.477 87.6076 1
1 1 0 312.703 74.8195 1
1 -1 0 384.131 67.9893 3
-1 -1 0 365.519 76.0596 1
-1 1 0 417.939 68.9589 3
2 -1 0 2268.67 220.361 1
-2 -1 0 2272.37 179.384 1
-2 1 0 2498.78 175.549 3
2 1 0 2252.03 180.066 1
2 -1 0 2194.74 163.890 3
3 -1 0 44915.5 1037.92 1
3 1 0 44849.6 807.602 1
3 -1 0 43916.4 797.496 3
4 -1 0 374.450 106.855 1
4 1 0 475.088 87.2684 1
4 -1 0 417.940 86.3662 3
-4 1 0 483.215 110.821 2
-5 -1 0 6302.61 313.196 4
5 1 0 6599.48 344.208 1
5 -1 0 6429.12 453.541 1
-5 1 0 6607.83 290.541 5
-5 1 0 6024.77 371.008 2
5 -1 0 6893.03 297.276 6
5 -1 0 6747.29 275.782 11
6 -1 0 2904.12 324.845 1
6 1 0 2735.47 195.765 6
-6 1 0 2686.10 254.825 2
-6 1 0 2884.58 210.243 5
6 -1 0 2841.53 202.659 11
6 -1 0 3001.78 216.333 6
7 1 0 2417.49 198.297 9
7 -1 0 2613.27 217.503 6
7 -1 0 2559.79 210.011 11
-7 1 0 2427.29 213.109 5
7 1 0 2685.92 204.261 6
8 -1 0 51.7292 49.8375 6
8 1 0 4.28220 26.8823 6
-8 1 0 33.5252 42.7074 5
8 -1 0 3.75722 29.1565 11
9 1 0 857.272 136.344 6
9 -1 0 919.284 147.692 6
9 -1 0 841.572 139.298 11
-9 1 0 800.149 142.560 5
10 1 0 38.2435 42.8909 6
10 -1 0 53.0741 55.5292 6
-10 1 0 57.5228 52.9477 5
-11 1 0 122.032 67.4070 5
11 1 0 196.418 86.2923 6
11 -1 0 174.508 61.6100 6
12 1 0 760.897 157.984 6
-12 1 0 754.516 165.335 5
12 -1 0 749.591 174.055 6
-13 1 0 21.2160 51.4087 5
13 1 0 35.7345 31.3575 6
13 -1 0-12.6829 44.6769 6
14 1 0 24.8992 62.5447 6
-14 1 0-31.4203 64.0581 5
14 -1 0 15.9375 57.9699 6
15 -1 0 69.2965 68.3192 6
-15 1 0 49.7772 61.8264 5
-16 -1 0 455.600 72.6534 31
-16 1 0 438.506 71.7870 31
-16 -1 0 618.673 83.2696 24
-17 -1 0 111.058 37.1509 31
-17 -1 0 154.516 40.3380 24
-17 1 0 128.271 38.4391 31
-18 -1 0-6.92561 20.5251 31
-18 -1 0 14.0874 18.2624 24
-18 1 0-12.2170 19.4371 31
-18 1 0 43.5151 27.0927 29
-19 -1 0-6.20643 17.7595 31
-19 1 0-11.0094 19.4345 31
-20 -1 0 11.7001 21.9832 31
-20 1 0 0.22311 13.5611 31
-21 1 0 15.0645 10.6403 31
-21 -1 0-1.37714 10.9766 31
-22 -1 0 20.4811 12.9419 31
-22 1 0-5.16871 10.9268 31
0 2 0 776.010 161.616 1
0 -2 0 765.618 162.744 1
0 2 0 764.439 154.922 3
1 -2 0 436.457 127.053 1
-1 2 0 446.024 119.095 1
1 2 0 368.276 102.040 1
1 2 0 390.693 97.9736 3
-1 -2 0 363.929 109.863 1
-1 2 0 283.538 82.2840 3
-1 -2 0 431.047 82.6739 7
-2 -2 0 814.880 109.548 7
-2 -2 0 938.641 179.908 1
2 2 0 870.325 170.743 1
2 2 0 766.000 110.842 10
-2 2 0 862.787 139.877 3
3 -2 0 5365.69 254.824 11
3 2 0 5589.05 290.058 13
-3 -2 0 5566.61 288.397 7
3 2 0 5441.71 410.667 1
3 2 0 5110.44 278.006 10
-3 2 0 5953.35 378.850 3
-3 2 0 5580.84 276.474 5
3 -2 0 5100.76 366.202 3
-3 -2 0 5438.73 413.399 1
3 -2 0 5837.93 292.590 6
4 2 0 1948.81 186.057 13
4 -2 0 2025.04 165.009 11
4 -2 0 1877.57 227.379 3
-4 -2 0 1850.99 172.406 7
-4 2 0 2018.93 178.110 5
4 2 0 1800.52 236.307 1
4 -2 0 1877.61 176.172 6
4 2 0 1829.39 177.241 10
-5 -2 0 33.7007 27.6668 7
5 -2 0 38.1035 37.3071 11
-5 2 0 14.2304 34.6905 5
5 2 0 41.0243 40.0937 6
5 2 0 36.5258 31.8597 13
5 2 0-11.7870 36.1928 10
5 -2 0 7.73568 20.5855 6
6 2 0 13521.0 544.900 13
6 2 0 13771.7 503.599 10
6 2 0 13502.2 469.094 6
-6 2 0 13795.0 518.500 5
6 -2 0 13549.4 476.795 11
6 -2 0 13245.7 516.208 6
7 -2 0 468.053 102.066 11
-7 2 0 314.210 84.0724 5
7 2 0 322.101 104.764 9
7 2 0 451.626 91.7561 6
7 2 0 424.101 111.750 13
7 -2 0 345.063 93.0273 6
-8 2 0 23.8053 36.3585 5
8 2 0 3.50070 33.0231 6
8 -2 0 14.1329 35.9729 6
8 -2 0-40.5892 50.4146 11
8 2 0 21.1652 34.1679 9
9 -2 0 110.158 60.9534 11
-9 2 0 115.436 69.9611 5
9 -2 0 114.306 47.1162 6
9 2 0 35.7191 25.7160 9
-10 2 0 203.256 93.4835 5
10 -2 0 264.747 95.8345 11
10 -2 0 301.181 103.833 6
-11 2 0 542.182 141.353 5
11 -2 0 709.598 165.861 6
11 -2 0 515.773 138.143 11
12 -2 0 75.0923 57.7074 6
-12 2 0 89.9300 68.5865 5
13 -2 0 337.015 135.504 6
-13 2 0 65.1970 58.4236 5
-14 2 0 1026.98 223.094 5
14 -2 0 1223.20 245.732 6
14 2 0 1200.78 250.868 13
-15 -2 0 1282.68 117.667 31
-15 2 0 1440.97 133.993 23
-15 -2 0 1431.89 128.735 24
-15 2 0 1192.50 96.0782 17
-16 -2 0 75.0406 32.5884 31
-16 -2 0 2.04048 29.2117 24
-17 -2 0 21.6854 21.6835 31
-17 -2 0-18.4591 25.2208 24
-18 2 0 6.91526 21.0940 31
-18 -2 0 10.2338 18.4144 31
-18 -2 0 38.6368 28.2545 24
-19 2 0 10.3739 13.8559 29
-19 2 0 7.96508 13.1636 31
-19 -2 0 29.6590 20.1398 31
-19 -2 0 1.40755 15.7651 24
-20 -2 0 11.9748 18.8579 24
-20 2 0 0.81165 16.6734 29
-20 -2 0-0.77942 16.1491 31
-21 -2 0 6.04098 10.8115 31
-21 -2 0-11.9188 11.2326 24
-21 2 0 25.0223 16.8028 29
0 3 0 32.4471 29.3155 10
0 -3 0-27.1330 44.3622 6
0 -3 0-13.2152 37.1346 7
-1 -3 0 1677.32 178.903 6
1 3 0 1489.86 183.153 10
-1 3 0 1358.38 174.535 10
1 -3 0 1847.83 192.262 6
-1 -3 0 1580.26 196.504 7
2 3 0 5645.97 353.254 10
-2 3 0 5331.88 341.038 10
2 -3 0 5983.41 350.438 6
-2 -3 0 5375.99 354.529 7
3 -3 0 9975.46 464.400 6
3 3 0 9291.94 458.865 10
3 -3 0 9385.06 425.621 11
-3 -3 0 9475.46 467.899 7
-4 -3 0 322.704 87.7824 7
4 -3 0 441.698 96.0199 11
4 -3 0 450.066 108.442 6
4 3 0 353.607 96.6753 10
5 3 0 4176.90 325.745 10
5 3 0 3547.34 336.264 9
-5 -3 0 3603.37 300.186 7
5 -3 0 3686.08 303.415 6
5 -3 0 3648.51 276.633 11
-6 -3 0 164.798 79.6419 7
6 3 0 100.540 67.0893 13
6 3 0 162.758 71.0974 10
6 -3 0 122.664 68.3558 6
6 -3 0 72.1051 47.3269 11
6 3 0 97.3424 80.0474 9
7 -3 0 2847.38 269.195 11
7 3 0 3128.24 298.438 10
-7 3 0 2692.71 278.280 5
7 -3 0 2513.89 273.123 6
7 3 0 2668.49 290.320 13
7 3 0 2751.33 313.622 9
8 -3 0 897.971 172.026 6
-8 3 0 901.656 170.496 5
8 3 0 951.909 202.372 9
8 -3 0 1055.27 175.692 11
8 3 0 874.050 179.190 13
9 3 0 867.196 180.505 13
9 3 0 894.136 189.258 9
9 -3 0 974.627 187.255 6
9 -3 0 829.266 168.466 11
-9 3 0 759.377 164.522 5
10 3 0 30.4818 54.7870 9
10 3 0-58.1639 56.1319 13
10 -3 0-6.06217 41.9130 6
-10 3 0-6.16604 52.3352 5
10 -3 0-26.5407 39.2416 11
-11 3 0 202.744 96.6836 5
11 -3 0 74.7987 67.2324 6
11 -3 0 155.994 80.6113 11
11 3 0 133.497 95.7300 13
12 -3 0 1025.09 219.138 6
12 -3 0 841.384 186.414 11
12 3 0 931.764 217.715 13
-12 3 0 918.577 197.642 5
13 -3 0 153.057 107.395 6
-13 3 0 287.692 110.947 5
13 3 0 199.652 107.175 13
-14 3 0 1449.41 135.864 23
14 3 0 1571.54 104.316 16
-14 3 0 1249.32 100.485 17
-14 -3 0 1579.51 132.445 24
-15 3 0-10.2902 21.8631 23
-15 -3 0 40.6181 33.0907 24
-15 3 0 35.7351 23.3962 17
15 3 0 54.8637 19.6911 16
-16 3 0 32.2083 28.6542 23
-16 3 0-19.1010 21.8847 17
16 3 0 0.63795 14.7684 16
-16 -3 0-19.4299 19.9680 24
17 3 0 6.76898 14.0997 16
-17 3 0 6.03005 20.3988 23
-17 3 0-6.45159 16.3191 17
-17 -3 0 11.0472 19.0190 24
18 3 0-11.2012 13.9050 16
-18 -3 0 6.58157 15.1324 24
-18 3 0-19.6251 18.9239 17
-19 -3 0 8.39699 12.5045 24
-19 3 0 4.35719 12.3144 29
-19 3 0 10.6206 12.4211 17
-20 -3 0-17.6566 17.1410 24
-20 3 0-1.09730 13.7001 29
0 -4 0 872.400 177.018 7
0 4 0 702.779 159.767 9
0 4 0 709.794 146.615 10
1 4 0 473.987 120.479 10
1 4 0 309.707 111.832 9
-1 -4 0 303.459 104.536 7
-1 4 0 516.418 135.123 10
1 -4 0 438.210 126.536 7
2 4 0 54.1854 69.9655 9
-2 4 0 76.7763 64.1290 10
2 4 0-7.15097 43.2537 10
-2 -4 0-1.13022 39.4119 7
3 4 0-3.51806 44.3957 10
-3 -4 0-7.79873 40.7848 7
3 -4 0 15.2153 42.4751 11
3 4 0 12.0402 60.8844 9
-4 -4 0 1112.74 196.231 7
4 -4 0 1144.57 181.324 11
4 4 0 1240.23 203.379 10
4 4 0 991.513 205.897 9
5 4 0 10.0206 46.4004 9
5 4 0 10.0541 55.6644 10
5 -4 0-30.4643 70.5241 6
-5 -4 0 75.1038 56.6369 7
5 -4 0 45.6232 30.1033 11
6 4 0 52.5513 36.1657 9
6 4 0 59.9938 65.5904 10
6 -4 0 162.650 82.6031 11
6 -4 0 25.1874 32.2001 6
-6 -4 0 62.3968 43.8048 7
7 -4 0 38.1503 57.9365 6
7 4 0 30.5172 64.6371 9
7 4 0-7.66795 41.8570 10
7 -4 0 72.7932 72.2454 11
8 -4 0 45.7394 63.5442 6
8 -4 0 57.7625 51.7018 11
8 4 0 106.093 75.2495 9
9 -4 0 843.086 179.615 11
9 4 0 691.837 176.423 9
9 -4 0 485.868 134.625 6
10 -4 0 1418.89 251.769 6
10 4 0 1531.94 276.067 9
10 -4 0 1612.44 256.748 11
11 4 0 25.5765 55.2379 9
11 -4 0 49.4495 69.6109 6
-11 4 0 93.4673 32.9825 17
-11 4 0 60.1141 36.3600 23
11 4 0 109.548 30.2604 16
-11 -4 0 83.6871 36.6820 24
12 4 0 164.151 36.4271 16
-12 4 0 101.331 43.5313 23
-12 4 0 131.120 36.3108 17
-12 -4 0 122.680 43.4715 24
-13 4 0 83.1138 42.1891 23
-13 4 0 71.4634 29.1208 17
-13 -4 0 61.6651 32.5508 24
13 4 0 92.1796 31.8599 16
-14 -4 0 15.6868 15.5101 24
-14 4 0 2.88129 17.7054 17
14 4 0 24.9673 23.5801 16
15 4 0 34.0085 19.8435 16
-15 4 0 57.5004 34.0815 23
-15 4 0 72.6606 29.4026 17
-15 -4 0 48.5103 29.1982 24
16 4 0 33.1939 24.3306 16
-16 -4 0 18.3951 22.8163 24
-16 4 0 6.89331 20.5319 17
-16 4 0 25.0804 24.7995 23
-17 4 0 0.64817 17.8824 23
-17 -4 0 1.94875 19.2644 24
17 4 0 14.1486 15.7273 16
-17 4 0 27.1070 16.0206 17
-18 -4 0-9.51090 14.5829 24
-18 4 0 42.1352 19.0536 17
-18 -4 0 14.9172 12.7363 20
-18 4 0 6.02555 16.5660 29
-19 4 0-1.43649 9.76279 17
-19 -4 0-11.1053 10.9478 24
-19 4 0-1.15788 10.8626 29
0 5 0 67.4441 72.6878 10
0 -5 0 14.6115 48.8242 7
1 -5 0 84.6594 56.2376 11
1 5 0 31.2267 54.5739 10
1 -5 0 87.8861 87.2690 7
-1 -5 0 195.745 108.319 7
2 -5 0 662.494 160.473 11
2 -5 0 442.595 164.383 7
-2 -5 0 456.797 160.063 7
2 5 0 780.349 171.459 10
2 5 0 290.692 122.353 9
3 -5 0 423.382 157.324 7
3 5 0 389.772 128.951 10
3 5 0 347.461 150.041 9
-3 -5 0 464.269 154.410 7
3 -5 0 533.548 141.789 11
-4 -5 0 1084.77 221.801 7
4 5 0 804.043 189.215 10
4 5 0 733.861 195.988 9
4 -5 0 716.738 196.996 7
4 -5 0 1159.79 214.591 11
5 -5 0 115.682 85.1597 7
5 -5 0 110.225 99.6417 11
-5 -5 0 164.302 90.4335 7
5 5 0 69.0852 58.6452 10
5 5 0 58.3056 44.1718 9
-6 -5 0 886.858 208.890 7
6 5 0 858.477 213.655 9
6 -5 0 825.136 185.023 11
7 -5 0 23.5798 20.1580 18
7 -5 0-2.81507 73.6251 11
-7 -5 0 30.5178 17.7760 20
-7 5 0 16.6452 15.8033 30
7 5 0 84.6866 62.4890 9
-8 -5 0-4.11914 15.0242 20
-8 5 0 39.6801 25.7688 30
8 -5 0 16.0854 17.0991 18
8 5 0 62.1058 23.7014 16
-8 5 0 44.8445 22.4245 17
9 -5 0 75.6858 18.6830 18
-9 5 0 63.5787 26.9507 30
-9 5 0 109.758 34.5670 17
9 5 0 112.629 30.8274 16
-10 5 0 518.836 64.8908 30
10 -5 0 741.227 70.6735 18
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1 0 16 34.0624 12.1580 25
1 0 16 55.1319 30.4191 19
2 0 16-4.51343 12.2038 25
3 0 16-3.63563 10.0550 25
-5 1 16-11.8519 19.0107 19
-4 1 16-5.12474 19.8037 19
-3 1 16 17.4158 10.6369 25
-3 1 16-12.6051 24.6500 19
-2 1 16 18.2129 12.0253 25
-2 1 16 12.9400 16.9356 19
-1 1 16 85.6068 22.6983 25
-1 1 16 64.8612 28.0378 19
0 1 16 151.016 29.0424 25
0 1 16 117.442 37.9788 19
1 1 16 68.9787 20.7555 25
1 1 16 174.039 47.8545 19
2 1 16 8.25763 11.5631 25
0 0 0 0.00 0.00 0
TITL cr11 in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184 18.684445 6.543071 13.668776 90.0000 93.6273 90.0000
ZERR 5.00 0.002431 0.000472 0.001443 0.0000 0.0109 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H O
UNIT 60.00 60.00 25.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 99285
_shelx_res_file
;
shelx.res created by SHELXL-2014/7
TITL SIR2014 run in space group P 21/c
CELL 1.54184 18.6844 6.5431 13.6688 90.000 93.627 90.000
ZERR 4.00 0.0024 0.0005 0.0014 0.000 0.011 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H O
UNIT 80 72 16
MERG 2
FMAP 2
PLAN 25
HTAB C8 O4_$1
EQIV $1 x, -1+y,z
HTAB C6 O4
ACTA
BOND $H
CONF
L.S. 10
TEMP 25.00
WGHT 0.098100
FVAR 3.44079
O3 3 0.053382 0.195527 0.657088 11.00000 0.11805 0.07197 =
0.09914 0.00630 -0.00138 0.01063
O1 3 -0.198104 0.343276 0.653692 11.00000 0.11682 0.08750 =
0.09882 -0.01890 -0.00574 0.00736
O4 3 0.041521 0.517703 0.603141 11.00000 0.12890 0.08122 =
0.16018 0.02764 0.01190 0.02139
C7 1 -0.019236 0.145521 0.641396 11.00000 0.11887 0.06838 =
0.07263 0.00372 -0.00130 0.00889
C4 1 -0.157905 0.006792 0.610575 11.00000 0.13212 0.07393 =
0.06472 0.00190 -0.00002 -0.00641
C6 1 -0.074755 0.278344 0.656759 11.00000 0.12781 0.06552 =
0.07643 -0.00883 -0.00468 0.00648
AFIX 43
H6 2 -0.066170 0.411886 0.677641 11.00000 -1.20000
AFIX 0
C11 1 0.158647 0.383830 0.635382 11.00000 0.12006 0.06898 =
0.06811 -0.00292 -0.00170 0.00671
C5 1 -0.143555 0.204425 0.639794 11.00000 0.12060 0.07318 =
0.06603 -0.00421 -0.00208 0.00580
C9 1 -0.100110 -0.123494 0.598170 11.00000 0.14961 0.06419 =
0.07793 0.00101 0.00371 0.00164
AFIX 43
H9 2 -0.108584 -0.258566 0.579690 11.00000 -1.20000
AFIX 0
C10 1 0.078852 0.379852 0.629994 11.00000 0.13337 0.06465 =
0.07301 -0.00306 -0.00115 0.01153
C12 1 0.191963 0.562913 0.610661 11.00000 0.13336 0.06876 =
0.08904 0.00346 -0.00187 0.00915
AFIX 43
H12 2 0.164458 0.677406 0.593533 11.00000 -1.20000
AFIX 0
C14 1 0.308340 0.406401 0.634986 11.00000 0.12441 0.08392 =
0.08135 -0.00006 -0.00556 -0.00178
C8 1 -0.031070 -0.054928 0.612872 11.00000 0.12989 0.06811 =
0.08149 0.00280 0.00453 0.01056
AFIX 43
H8 2 0.007312 -0.141919 0.603804 11.00000 -1.20000
AFIX 0
C3 1 -0.231702 -0.053155 0.595679 11.00000 0.14318 0.08639 =
0.08926 -0.00275 0.00015 -0.01437
AFIX 43
H3 2 -0.243238 -0.186639 0.577400 11.00000 -1.20000
AFIX 0
O2 3 -0.312547 0.420878 0.650863 11.00000 0.12566 0.14950 =
0.14909 -0.04335 -0.00627 0.01826
C13 1 0.265724 0.573816 0.611100 11.00000 0.13238 0.07720 =
0.09656 0.00700 0.00003 -0.00735
AFIX 43
H13 2 0.287202 0.696472 0.594974 11.00000 -1.20000
AFIX 0
C16 1 0.200332 0.216338 0.661382 11.00000 0.12119 0.07400 =
0.09150 0.00982 0.00377 0.00335
AFIX 43
H16 2 0.178773 0.095069 0.679377 11.00000 -1.20000
AFIX 0
C15 1 0.274303 0.228434 0.660738 11.00000 0.12287 0.08174 =
0.10409 0.01283 -0.00403 0.00776
AFIX 43
H15 2 0.301779 0.113996 0.678059 11.00000 -1.20000
AFIX 0
C1 1 -0.269377 0.288140 0.637849 11.00000 0.12695 0.11361 =
0.09535 -0.01829 -0.00285 0.00297
C2 1 -0.283915 0.082580 0.608035 11.00000 0.12287 0.11522 =
0.10230 -0.00860 0.00168 -0.01584
AFIX 43
H2 2 -0.331369 0.041464 0.596789 11.00000 -1.20000
AFIX 0
C17 1 0.390197 0.410155 0.633110 11.00000 0.11486 0.10941 =
0.10800 -0.00047 -0.00272 -0.00682
C18 1 0.418521 0.621412 0.605300 11.00000 0.13654 0.13304 =
0.18549 0.01741 -0.01925 -0.03145
AFIX 33
H18A 2 0.397348 0.660565 0.542255 11.00000 -1.50000
H18B 2 0.406199 0.719970 0.653471 11.00000 -1.50000
H18C 2 0.469713 0.615698 0.602797 11.00000 -1.50000
AFIX 0
C19 1 0.425055 0.355145 0.732885 11.00000 0.11909 0.24612 =
0.14324 0.05025 -0.01232 0.01571
AFIX 33
H19A 2 0.476264 0.358319 0.730245 11.00000 -1.50000
H19B 2 0.410704 0.451822 0.780712 11.00000 -1.50000
H19C 2 0.410256 0.220483 0.750836 11.00000 -1.50000
AFIX 0
C20 1 0.412633 0.257183 0.554558 11.00000 0.13986 0.16572 =
0.19756 -0.04772 0.05178 -0.02648
AFIX 33
H20A 2 0.390140 0.294154 0.491967 11.00000 -1.50000
H20B 2 0.463789 0.260413 0.551234 11.00000 -1.50000
H20C 2 0.397910 0.121937 0.571666 11.00000 -1.50000
AFIX 0
HKLF 4
REM SIR2014 run in space group P 21/c
REM R1 = 0.0569 for 1710 Fo > 4sig(Fo) and 0.0942 for all 3005 data
REM 217 parameters refined using 0 restraints
END
WGHT 0.0981 0.0000
REM Highest difference peak 0.144, deepest hole -0.130, 1-sigma level 0.032
Q1 1 0.4232 0.1618 0.6469 11.00000 0.05 0.14
Q2 1 0.0354 0.6445 0.5800 11.00000 0.05 0.13
Q3 1 -0.0159 0.0217 0.6622 11.00000 0.05 0.12
Q4 1 -0.1894 0.4917 0.6850 11.00000 0.05 0.12
Q5 1 0.0517 0.4559 0.5824 11.00000 0.05 0.12
Q6 1 0.0662 0.0599 0.6799 11.00000 0.05 0.11
Q7 1 -0.2710 0.1381 0.6406 11.00000 0.05 0.11
Q8 1 -0.1009 -0.2836 0.6104 11.00000 0.05 0.10
Q9 1 0.0678 0.2877 0.7795 11.00000 0.05 0.10
Q10 1 -0.3063 0.5794 0.6619 11.00000 0.05 0.10
Q11 1 -0.1546 0.0806 0.6256 11.00000 0.05 0.10
Q12 1 0.1855 0.0715 0.6594 11.00000 0.05 0.10
Q13 1 0.0000 0.5000 0.5000 10.50000 0.05 0.09
Q14 1 0.4126 0.4816 0.5125 11.00000 0.05 0.09
Q15 1 0.4127 0.3644 0.7005 11.00000 0.05 0.09
Q16 1 -0.0450 0.0880 0.5847 11.00000 0.05 0.08
Q17 1 0.2862 0.4677 0.6041 11.00000 0.05 0.08
Q18 1 0.4135 0.5160 0.6718 11.00000 0.05 0.08
Q19 1 0.1661 0.4493 0.5832 11.00000 0.05 0.08
Q20 1 0.3000 0.3555 0.6243 11.00000 0.05 0.08
Q21 1 0.4144 0.5255 0.7651 11.00000 0.05 0.08
Q22 1 0.3932 0.1273 0.5349 11.00000 0.05 0.08
Q23 1 -0.2848 0.4773 0.7262 11.00000 0.05 0.07
Q24 1 0.2936 0.0964 0.7172 11.00000 0.05 0.07
Q25 1 0.1286 0.0514 0.6589 11.00000 0.05 0.07
;
_shelx_res_checksum 53801
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
O O3 0.05338(12) 0.1955(3) 0.65709(16) 0.0967(6) Uani d 1
O O1 -0.19810(13) 0.3433(3) 0.65369(16) 0.1016(7) Uani d 1
O O4 0.04152(14) 0.5177(3) 0.6031(2) 0.1233(9) Uani d 1
C C7 -0.01924(18) 0.1455(4) 0.64140(19) 0.0869(8) Uani d 1
C C4 -0.15790(19) 0.0068(4) 0.61057(19) 0.0905(8) Uani d 1
C C6 -0.07476(18) 0.2783(4) 0.6568(2) 0.0904(8) Uani d 1
H H6 -0.0662 0.4119 0.6776 0.108 Uiso calc 1
C C11 0.15865(18) 0.3838(4) 0.63538(19) 0.0860(8) Uani d 1
C C5 -0.14356(18) 0.2044(4) 0.63979(19) 0.0869(8) Uani d 1
C C9 -0.1001(2) -0.1235(4) 0.5982(2) 0.0974(9) Uani d 1
H H9 -0.1086 -0.2586 0.5797 0.117 Uiso calc 1
C C10 0.0789(2) 0.3799(4) 0.6300(2) 0.0907(8) Uani d 1
C C12 0.1920(2) 0.5629(4) 0.6107(2) 0.0974(9) Uani d 1
H H12 0.1645 0.6774 0.5935 0.117 Uiso calc 1
C C14 0.3083(2) 0.4064(5) 0.6350(2) 0.0971(9) Uani d 1
C C8 -0.0311(2) -0.0549(4) 0.6129(2) 0.0933(8) Uani d 1
H H8 0.0073 -0.1419 0.6038 0.112 Uiso calc 1
C C3 -0.2317(2) -0.0532(5) 0.5957(2) 0.1066(10) Uani d 1
H H3 -0.2432 -0.1866 0.5774 0.128 Uiso calc 1
O O2 -0.31255(16) 0.4209(5) 0.6509(2) 0.1421(11) Uani d 1
C C13 0.2657(2) 0.5738(5) 0.6111(2) 0.1024(10) Uani d 1
H H13 0.2872 0.6965 0.5950 0.123 Uiso calc 1
C C16 0.20033(19) 0.2163(4) 0.6614(2) 0.0957(9) Uani d 1
H H16 0.1788 0.0951 0.6794 0.115 Uiso calc 1
C C15 0.2743(2) 0.2284(5) 0.6607(2) 0.1034(10) Uani d 1
H H15 0.3018 0.1140 0.6781 0.124 Uiso calc 1
C C1 -0.2694(2) 0.2881(6) 0.6378(3) 0.1124(10) Uani d 1
C C2 -0.2839(2) 0.0826(6) 0.6080(3) 0.1137(11) Uani d 1
H H2 -0.3314 0.0415 0.5968 0.136 Uiso calc 1
C C17 0.3902(2) 0.4102(6) 0.6331(3) 0.1112(10) Uani d 1
C C18 0.4185(3) 0.6214(7) 0.6053(4) 0.1529(18) Uani d 1
H H18A 0.3973 0.6606 0.5423 0.229 Uiso calc 1
H H18B 0.4062 0.7200 0.6535 0.229 Uiso calc 1
H H18C 0.4697 0.6157 0.6028 0.229 Uiso calc 1
C C19 0.4251(3) 0.3551(9) 0.7329(4) 0.170(2) Uani d 1
H H19A 0.4763 0.3583 0.7302 0.256 Uiso calc 1
H H19B 0.4107 0.4518 0.7807 0.256 Uiso calc 1
H H19C 0.4103 0.2205 0.7508 0.256 Uiso calc 1
C C20 0.4126(3) 0.2572(8) 0.5546(4) 0.166(2) Uani d 1
H H20A 0.3901 0.2942 0.4920 0.249 Uiso calc 1
H H20B 0.4638 0.2604 0.5512 0.249 Uiso calc 1
H H20C 0.3979 0.1219 0.5717 0.249 Uiso calc 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
O3 0.1181(17) 0.0720(10) 0.0991(14) 0.0106(10) -0.0014(11) 0.0063(9)
O1 0.1168(17) 0.0875(13) 0.0988(14) 0.0074(11) -0.0057(12) -0.0189(10)
O4 0.129(2) 0.0812(13) 0.160(2) 0.0214(13) 0.0119(16) 0.0276(13)
C7 0.119(2) 0.0684(13) 0.0726(15) 0.0089(14) -0.0013(14) 0.0037(10)
C4 0.132(2) 0.0739(14) 0.0647(14) -0.0064(15) 0.0000(14) 0.0019(10)
C6 0.128(2) 0.0655(13) 0.0764(15) 0.0065(14) -0.0047(14) -0.0088(11)
C11 0.120(2) 0.0690(13) 0.0681(14) 0.0067(13) -0.0017(14) -0.0029(10)
C5 0.121(2) 0.0732(13) 0.0660(14) 0.0058(15) -0.0021(13) -0.0042(11)
C9 0.150(3) 0.0642(13) 0.0779(16) 0.0016(16) 0.0037(17) 0.0010(11)
C10 0.133(3) 0.0646(13) 0.0730(15) 0.0115(14) -0.0011(15) -0.0031(11)
C12 0.133(3) 0.0688(14) 0.0890(18) 0.0092(15) -0.0019(17) 0.0035(12)
C14 0.124(3) 0.0839(17) 0.0813(17) -0.0018(16) -0.0056(16) -0.0001(13)
C8 0.130(3) 0.0681(14) 0.0815(16) 0.0106(15) 0.0045(16) 0.0028(12)
C3 0.143(3) 0.0864(18) 0.0893(19) -0.0144(19) 0.0001(19) -0.0027(14)
O2 0.126(2) 0.149(2) 0.149(2) 0.0183(18) -0.0063(17) -0.0434(19)
C13 0.132(3) 0.0772(16) 0.097(2) -0.0074(16) 0.0000(18) 0.0070(14)
C16 0.121(3) 0.0740(15) 0.0915(19) 0.0033(15) 0.0038(16) 0.0098(13)
C15 0.123(3) 0.0817(17) 0.104(2) 0.0078(16) -0.0040(18) 0.0128(15)
C1 0.127(3) 0.114(2) 0.095(2) 0.003(2) -0.0028(19) -0.0183(18)
C2 0.123(3) 0.115(3) 0.102(2) -0.016(2) 0.002(2) -0.0086(19)
C17 0.115(3) 0.109(2) 0.108(2) -0.0068(19) -0.0027(19) -0.0005(18)
C18 0.137(4) 0.133(3) 0.185(5) -0.031(3) -0.019(3) 0.017(3)
C19 0.119(3) 0.246(6) 0.143(4) 0.016(3) -0.012(3) 0.050(4)
C20 0.140(4) 0.166(4) 0.198(5) -0.026(3) 0.052(4) -0.048(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 '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
C10 O3 C7 121.3(2)
C1 O1 C5 121.1(3)
C6 C7 C8 122.2(3)
C6 C7 O3 124.1(3)
C8 C7 O3 113.7(3)
C5 C4 C9 118.2(3)
C5 C4 C3 117.8(3)
C9 C4 C3 124.0(3)
C5 C6 C7 117.1(3)
C5 C6 H6 121.5
C7 C6 H6 121.5
C16 C11 C12 118.8(3)
C16 C11 C10 123.2(3)
C12 C11 C10 118.0(3)
C4 C5 C6 122.8(3)
C4 C5 O1 121.6(3)
C6 C5 O1 115.6(2)
C8 C9 C4 120.8(3)
C8 C9 H9 119.6
C4 C9 H9 119.6
O4 C10 O3 123.5(3)
O4 C10 C11 124.8(3)
O3 C10 C11 111.7(2)
C11 C12 C13 120.6(3)
C11 C12 H12 119.7
C13 C12 H12 119.7
C13 C14 C15 117.4(4)
C13 C14 C17 123.0(3)
C15 C14 C17 119.6(3)
C9 C8 C7 119.0(3)
C9 C8 H8 120.5
C7 C8 H8 120.5
C2 C3 C4 120.1(3)
C2 C3 H3 119.9
C4 C3 H3 119.9
C12 C13 C14 121.4(3)
C12 C13 H13 119.3
C14 C13 H13 119.3
C11 C16 C15 120.1(3)
C11 C16 H16 120.0
C15 C16 H16 120.0
C14 C15 C16 121.7(3)
C14 C15 H15 119.2
C16 C15 H15 119.2
O2 C1 O1 115.8(3)
O2 C1 C2 127.2(4)
O1 C1 C2 117.0(4)
C3 C2 C1 122.3(4)
C3 C2 H2 118.8
C1 C2 H2 118.8
C19 C17 C14 110.7(3)
C19 C17 C18 107.5(4)
C14 C17 C18 112.2(3)
C19 C17 C20 110.6(4)
C14 C17 C20 108.4(3)
C18 C17 C20 107.3(4)
C17 C18 H18A 109.5
C17 C18 H18B 109.5
H18A C18 H18B 109.5
C17 C18 H18C 109.5
H18A C18 H18C 109.5
H18B C18 H18C 109.5
C17 C19 H19A 109.5
C17 C19 H19B 109.5
H19A C19 H19B 109.5
C17 C19 H19C 109.5
H19A C19 H19C 109.5
H19B C19 H19C 109.5
C17 C20 H20A 109.5
C17 C20 H20B 109.5
H20A C20 H20B 109.5
C17 C20 H20C 109.5
H20A C20 H20C 109.5
H20B C20 H20C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O3 C10 1.357(3)
O3 C7 1.399(4)
O1 C1 1.383(4)
O1 C5 1.387(3)
O4 C10 1.184(3)
C7 C6 1.379(4)
C7 C8 1.382(4)
C4 C5 1.375(4)
C4 C9 1.395(5)
C4 C3 1.436(5)
C6 C5 1.379(4)
C6 H6 0.9300
C11 C16 1.378(4)
C11 C12 1.379(4)
C11 C10 1.488(5)
C9 C8 1.369(5)
C9 H9 0.9300
C12 C13 1.380(5)
C12 H12 0.9300
C14 C13 1.381(4)
C14 C15 1.383(4)
C14 C17 1.531(5)
C8 H8 0.9300
C3 C2 1.338(5)
C3 H3 0.9300
O2 C1 1.206(4)
C13 H13 0.9300
C16 C15 1.385(5)
C16 H16 0.9300
C15 H15 0.9300
C1 C2 1.426(5)
C2 H2 0.9300
C17 C19 1.517(5)
C17 C18 1.536(5)
C17 C20 1.545(5)
C18 H18A 0.9600
C18 H18B 0.9600
C18 H18C 0.9600
C19 H19A 0.9600
C19 H19B 0.9600
C19 H19C 0.9600
C20 H20A 0.9600
C20 H20B 0.9600
C20 H20C 0.9600
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
C8 H8 O4 1_545 0.93 2.32 3.114(4) 143.5
C15 H15 O2 2_546 0.93 2.65 3.310(4) 128.1
C6 H6 O4 . 0.93 2.41 2.813(4) 105.8
C10 O4 Cg2 2_556 1.184(3) 3.760(3) 3.560(3) 71.23(18)
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
C10 O3 C7 C6 -41.5(4)
C10 O3 C7 C8 141.3(3)
C8 C7 C6 C5 -1.7(4)
O3 C7 C6 C5 -178.7(2)
C9 C4 C5 C6 0.3(4)
C3 C4 C5 C6 179.7(3)
C9 C4 C5 O1 180.0(2)
C3 C4 C5 O1 -0.6(4)
C7 C6 C5 C4 1.2(4)
C7 C6 C5 O1 -178.5(2)
C1 O1 C5 C4 -0.5(4)
C1 O1 C5 C6 179.2(3)
C5 C4 C9 C8 -1.3(4)
C3 C4 C9 C8 179.4(3)
C7 O3 C10 O4 9.6(4)
C7 O3 C10 C11 -168.7(2)
C16 C11 C10 O4 -175.9(3)
C12 C11 C10 O4 2.4(5)
C16 C11 C10 O3 2.3(4)
C12 C11 C10 O3 -179.4(2)
C16 C11 C12 C13 0.6(4)
C10 C11 C12 C13 -177.8(3)
C4 C9 C8 C7 0.7(4)
C6 C7 C8 C9 0.8(4)
O3 C7 C8 C9 178.1(3)
C5 C4 C3 C2 1.5(5)
C9 C4 C3 C2 -179.2(3)
C11 C12 C13 C14 0.8(5)
C15 C14 C13 C12 -1.5(5)
C17 C14 C13 C12 177.9(3)
C12 C11 C16 C15 -1.1(5)
C10 C11 C16 C15 177.2(3)
C13 C14 C15 C16 0.9(5)
C17 C14 C15 C16 -178.5(3)
C11 C16 C15 C14 0.4(5)
C5 O1 C1 O2 -179.1(3)
C5 O1 C1 C2 0.8(5)
C4 C3 C2 C1 -1.2(5)
O2 C1 C2 C3 180.0(4)
O1 C1 C2 C3 0.1(6)
C13 C14 C17 C19 122.1(4)
C15 C14 C17 C19 -58.5(5)
C13 C14 C17 C18 1.9(5)
C15 C14 C17 C18 -178.7(4)
C13 C14 C17 C20 -116.5(4)
C15 C14 C17 C20 62.9(4)
_cod_database_fobs_code 2242429