#------------------------------------------------------------------------------
#$Date: 2025-01-31 04:49:21 +0200 (Fri, 31 Jan 2025) $
#$Revision: 297542 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/33/2023367.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_2023367
loop_
_publ_author_name
'Liu, Mo'
'Izod, Keith'
'Waddell, Paul G.'
_publ_section_title
;
Polymorphism in a secondary phosphine
;
_journal_coeditor_code OJ3027
_journal_issue 2
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_page_first 109
_journal_page_last 113
_journal_paper_doi 10.1107/S2053229625000555
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac 'C20 H27 P'
_chemical_formula_moiety 'C20 H27 P'
_chemical_formula_sum 'C20 H27 P'
_chemical_formula_weight 298.38
_chemical_name_systematic
;
Bis(2,3,5,6-tetramethylphenyl)phosphine
;
_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'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 90
_cell_angle_beta 104.108(5)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.8874(6)
_cell_length_b 8.8455(3)
_cell_length_c 15.4635(7)
_cell_measurement_reflns_used 3351
_cell_measurement_temperature 150.0(2)
_cell_measurement_theta_max 66.6950
_cell_measurement_theta_min 5.7820
_cell_volume 1709.60(13)
_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
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015)
;
_diffrn_ambient_temperature 150.0(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Xcalibur Gemini ultra diffractometer with an Atlas detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0391
_diffrn_reflns_av_unetI/netI 0.0288
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 12709
_diffrn_reflns_theta_full 66.781
_diffrn_reflns_theta_max 66.781
_diffrn_reflns_theta_min 3.536
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 1.333
_exptl_absorpt_correction_T_max 0.939
_exptl_absorpt_correction_T_min 0.746
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Rigaku OD, 2015), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.159
_exptl_crystal_description block
_exptl_crystal_F_000 648
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.05
_refine_diff_density_max 0.426
_refine_diff_density_min -0.347
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.056
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 214
_refine_ls_number_reflns 3021
_refine_ls_number_restraints 182
_refine_ls_restrained_S_all 1.028
_refine_ls_R_factor_all 0.0610
_refine_ls_R_factor_gt 0.0472
_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^)+(0.0698P)^2^+0.7357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1242
_refine_ls_wR_factor_ref 0.1353
_reflns_number_gt 2424
_reflns_number_total 3021
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file oj3027.cif
_cod_data_source_block kji190003_fa
_cod_original_cell_volume 1709.61(13)
_cod_database_code 2023367
_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
;
1 0 0 40309.1 476.865 1
2 0 0 3954.95 231.902 2
2 0 0 3829.50 217.943 1
3 0 0 274717. 2280.58 2
4 0 0 185857. 2191.27 2
5 0 0 20930.0 847.202 2
6 0 0 42858.2 1373.38 2
7 0 0 3244.21 445.029 2
8 0 0 2329.89 435.164 2
8 0 0 2390.88 212.592 12
-8 0 0 2406.84 213.444 9
9 0 0 4250.14 612.114 2
-9 0 0 4070.09 290.602 9
9 0 0 3640.23 270.768 12
10 0 0 7059.20 399.795 12
-10 0 0 6915.77 397.641 9
10 0 0 6820.51 825.543 2
-11 0 0 170.377 171.152 9
11 0 0 103.757 123.230 12
-12 0 0 3512.13 316.294 9
12 0 0 2833.81 286.977 12
13 0 0-35.3538 112.143 12
-13 0 0 18.3295 141.595 9
-14 0 0 1024.41 162.789 9
-14 0 0 719.320 139.647 8
14 0 0 767.126 145.211 12
0 -1 0 18.2042 28.1228 2
1 -1 0 67731.9 835.054 2
1 1 0 68861.4 654.572 1
2 -1 0 19286.9 555.035 2
2 1 0 18468.8 430.056 1
3 1 0 241381. 1925.97 1
3 -1 0 244126. 2321.11 2
4 -1 0 89722.6 1649.42 2
4 1 0 93145.1 1408.64 1
4 1 0 91232.9 1480.42 2
5 -1 0 8438.21 597.773 2
5 1 0 8795.27 528.680 2
6 -1 0 28270.1 1171.57 2
6 1 0 28496.4 1059.08 2
-7 1 0 1465.08 161.354 9
7 1 0 1849.35 326.938 2
7 -1 0 1690.33 368.117 2
7 -1 0 1539.80 169.539 12
-8 -1 0 36.6453 108.087 9
8 1 0 106.103 97.0357 12
8 -1 0 142.797 96.2203 12
8 -1 0 171.486 196.200 2
-8 1 0 31.7259 106.346 9
8 1 0-113.487 162.525 2
-9 1 0 4935.66 315.972 9
9 -1 0 4658.65 315.096 12
-9 -1 0 5057.23 314.100 9
9 1 0 5113.71 645.322 2
9 1 0 4613.25 298.170 12
9 -1 0 5600.92 728.583 2
-10 1 0 120.229 138.211 9
10 -1 0 58.1960 123.271 12
10 1 0 34.9917 104.975 12
-10 -1 0 4.71012 137.530 9
10 -1 0-118.040 250.212 2
-11 -1 0 1113.13 211.255 9
-11 1 0 1209.06 223.381 9
11 1 0 1131.70 195.232 12
11 -1 0 1286.68 219.602 12
12 -1 0 23.6097 144.484 12
-12 -1 0 115.169 154.510 9
-12 1 0 53.3365 172.098 9
12 1 0-61.6797 122.896 12
13 1 0 992.890 177.106 12
-13 -1 0 960.222 185.973 9
-13 1 0 1019.26 203.325 9
13 -1 0 1134.65 194.939 12
-14 -1 0 1219.66 162.722 9
14 1 0 1433.70 172.865 12
-14 1 0 1259.35 179.548 9
14 -1 0 1283.62 169.507 12
-14 -1 0 1355.68 178.107 8
0 -2 0 12513.4 378.932 2
1 2 0 11373.6 372.102 1
1 -2 0 11185.1 427.987 2
2 2 0 26271.4 583.362 1
2 -2 0 25714.2 740.097 2
3 2 0 4262.13 264.709 1
3 -2 0 4633.88 374.698 2
4 -2 0 123460. 2095.94 2
4 2 0 127834. 1626.63 1
5 2 0 12027.1 600.641 2
5 -2 0 9944.35 697.989 2
5 2 0 11276.8 562.704 1
6 -2 0 62592.3 1829.83 2
6 2 0 62446.2 1514.25 2
-7 2 0 14735.0 442.289 9
7 -2 0 15885.1 492.971 12
-7 -2 0 14815.3 433.638 9
7 -2 0 16453.0 1041.97 2
7 2 0 15231.6 440.811 12
7 2 0 15641.7 865.234 2
8 2 0 342.040 166.083 2
-8 2 0 179.551 108.780 9
8 2 0 76.8992 91.8118 12
8 -2 0 87.9695 100.439 12
-8 -2 0 279.508 111.780 9
9 2 0 866.508 155.447 12
9 -2 0 501.704 369.626 2
-9 2 0 385.233 147.430 9
9 -2 0 373.197 144.666 12
-9 -2 0 503.255 140.796 9
-10 -2 0 239.794 146.446 9
10 2 0 303.072 128.991 12
-10 2 0 311.318 153.807 9
10 -2 0 125.169 140.935 12
-11 -2 0 3.08730 142.234 9
11 -2 0 103.727 157.529 12
-11 2 0 225.934 169.998 9
11 2 0 17.3756 113.301 12
12 -2 0 970.482 207.357 12
12 2 0 986.135 175.865 12
-12 -2 0 976.554 192.240 9
-12 2 0 1165.06 217.432 9
-13 -2 0 1736.51 203.876 9
-13 2 0 2123.41 237.493 9
13 2 0 1744.98 196.048 12
13 -2 0 2148.75 237.011 12
14 2 0 2355.01 192.376 12
-14 2 0 2533.36 209.320 9
-14 -2 0 2279.74 191.898 9
-14 -2 0 2022.52 198.291 8
0 -3 0 35.0746 72.5172 2
1 -3 0 65947.5 1178.34 2
1 3 0 66581.9 1115.92 1
2 3 0 29.4479 57.5803 1
2 -3 0 37.6958 128.199 2
3 3 0 19921.8 621.421 1
3 -3 0 20096.3 831.752 2
4 -3 0 9183.74 632.049 2
4 3 0 10202.3 480.997 1
5 3 0 3060.01 297.600 1
5 -3 0 2262.09 401.682 2
6 -3 0 4408.96 262.357 12
6 -3 0 4180.05 542.544 2
-7 3 0 16392.9 476.343 9
-7 -3 0 16912.2 495.371 5
7 -3 0 16761.7 505.729 7
7 3 0 16147.7 471.275 12
7 -3 0 17547.7 1133.10 2
-7 -3 0 16164.6 452.875 9
7 -3 0 16285.0 497.804 6
7 -3 0 16054.1 530.530 12
-8 -3 0 5917.39 310.320 5
-8 -3 0 6040.47 315.674 9
8 3 0 5711.61 308.490 12
8 -3 0 5582.70 321.387 7
8 -3 0 6037.98 736.908 2
-8 3 0 5803.32 320.622 9
8 -3 0 6058.04 354.253 12
8 -3 0 6056.84 325.881 6
9 -3 0 28972.5 789.672 12
9 -3 0 29069.4 703.438 7
9 3 0 28977.7 716.501 12
9 -3 0 30326.4 715.368 6
-9 -3 0 28968.5 692.223 9
-9 3 0 29130.5 714.766 9
-10 -3 0 206.572 127.648 9
-10 3 0 43.3321 139.789 9
10 -3 0-35.6331 129.672 12
10 3 0 163.700 112.179 12
11 -3 0 316.411 152.793 12
11 3 0 308.832 137.363 12
-11 -3 0 397.078 147.453 9
-11 3 0 182.323 121.502 13
-11 3 0 242.110 146.987 9
12 3 0 7533.91 379.502 12
-12 -3 0 6838.63 351.215 9
-12 3 0 7708.88 389.579 9
-13 -3 0 19.2214 106.446 8
13 3 0 38.1409 79.4005 12
-13 3 0-17.0324 119.491 9
-13 -3 0-226.781 100.459 9
-14 -3 0 186.641 89.4292 8
0 -4 0 584.517 140.143 2
0 4 0 744.610 193.624 1
1 4 0 48.8294 89.9930 1
1 -4 0 43.8189 116.297 2
2 4 0 59945.0 1197.37 1
2 -4 0 59151.2 1427.42 2
3 -4 0 24860.4 1012.55 2
3 4 0 28547.4 820.317 1
4 -4 0-380.973 218.383 2
5 -4 0 5511.74 291.142 7
-5 -4 0 5898.57 297.677 3
5 -4 0 5455.85 292.657 6
5 -4 0 5079.44 557.421 2
-5 -4 0 5634.75 291.055 5
6 -4 0 489.653 250.018 2
-6 -4 0 780.610 141.315 5
6 -4 0 1053.90 158.437 7
-6 -4 0 882.859 145.513 3
6 -4 0 921.416 147.928 6
7 -4 0 9343.54 412.319 6
-7 -4 0 9657.68 410.813 5
7 -4 0 9199.56 421.811 12
7 4 0 9383.31 371.862 12
7 -4 0 9237.13 410.960 7
7 -4 0 8177.62 839.881 2
-7 -4 0 8453.27 376.401 3
8 -4 0 25060.8 684.512 7
8 4 0 25514.0 644.416 12
8 -4 0 24775.2 721.644 12
8 -4 0 25687.5 693.286 6
8 -4 0 27172.2 1599.73 2
-8 -4 0 25641.0 675.309 5
9 4 0 32.1114 116.835 12
-9 -4 0 134.655 121.531 5
9 -4 0-49.5078 117.345 7
9 -4 0-209.030 286.201 2
9 -4 0 167.211 119.479 6
10 -4 0 7.34733 108.719 6
10 4 0 127.980 108.505 12
10 -4 0-4.07249 107.925 7
11 4 0 4653.59 294.746 12
-12 -4 0 550.079 151.654 8
-13 -4 0 66.0426 90.9796 8
0 5 0 425.976 169.898 1
1 5 0 10419.5 616.269 1
2 -5 0 20620.7 540.092 7
-2 -5 0 22090.0 550.030 3
2 -5 0 21023.1 930.705 2
2 -5 0 20609.8 544.223 6
-2 -5 0 21446.3 541.742 5
-3 -5 0 209.630 109.610 5
-3 -5 0 20.3307 124.062 3
3 -5 0 144.912 184.295 2
3 -5 0 42.0874 93.7565 7
3 -5 0 53.9305 91.2749 6
4 -5 0-234.698 230.686 2
4 -5 0-46.7367 92.3971 6
4 -5 0 19.1556 99.7173 7
-4 -5 0-8.22208 98.9095 5
-4 -5 0-54.0817 112.513 3
-5 -5 0 6138.85 333.354 3
5 -5 0 6341.85 344.892 7
5 -5 0 6593.03 350.544 6
-5 -5 0 6010.02 329.530 5
5 -5 0 7106.16 713.575 2
-6 -5 0 1612.48 207.430 3
-6 -5 0 1753.22 209.068 5
6 -5 0 1765.31 208.339 7
6 -5 0 1817.20 215.316 6
6 -5 0 1985.36 434.511 2
7 -5 0 6156.97 366.614 7
-7 -5 0 6251.51 375.429 5
-7 -5 0 5945.38 344.713 3
7 -5 0 5070.92 723.827 2
7 -5 0 5723.67 354.637 6
8 -5 0 3132.09 278.824 6
8 -5 0 3158.36 580.976 2
8 -5 0 3049.94 275.617 7
-8 -5 0 3416.31 282.409 3
-8 -5 0 2803.35 267.592 5
9 -5 0 2768.73 260.066 6
9 -5 0 2788.80 260.259 7
-9 -5 0 3115.77 270.323 5
-10 -5 0-10.6364 124.540 8
-10 -5 0-138.812 113.152 5
10 -5 0-326.424 117.883 6
10 -5 0-108.015 119.769 7
-11 -5 0 319.911 123.308 8
-12 5 0 762.211 131.412 13
-12 -5 0 684.368 123.442 8
0 -6 0 2341.00 210.021 6
0 -6 0 2043.96 198.361 7
0 -6 0 2400.07 202.857 4
0 -6 0 2228.90 212.836 3
0 -6 0 2290.84 210.058 5
1 -6 0 5377.36 297.362 3
-1 -6 0 5395.45 306.694 5
-1 -6 0 5305.07 288.624 7
-1 -6 0 5384.10 281.467 4
1 -6 0 5684.00 306.448 5
-1 -6 0 5368.80 307.234 3
1 -6 0 5795.36 316.740 7
-1 6 0 4972.03 549.345 1
1 -6 0 5585.16 315.877 6
-1 -6 0 5360.48 294.656 6
1 -6 0 5319.25 292.360 4
2 -6 0 5429.51 322.418 6
-2 -6 0 5639.55 287.940 4
2 -6 0 5549.06 297.885 5
-2 -6 0 5086.71 308.306 3
-2 -6 0 5459.56 287.290 6
-2 -6 0 5076.36 275.401 7
2 -6 0 5969.56 332.382 7
-2 6 0 4901.76 570.952 1
-2 -6 0 5212.15 307.106 5
-3 -6 0 5807.04 336.019 5
3 -6 0 5668.89 343.378 6
3 -6 0 5578.62 334.711 7
-3 -6 0 6008.13 348.015 3
4 -6 0 1489.98 207.938 7
4 -6 0 1136.21 193.684 6
-4 -6 0 1317.60 193.323 5
-4 -6 0 1452.08 197.430 3
-5 -6 0 14136.9 536.912 3
-5 -6 0 14066.1 531.120 5
5 -6 0 14418.0 554.354 6
5 -6 0 13932.4 545.025 7
-6 -6 0 7112.54 397.740 5
-6 -6 0 7008.84 399.497 3
6 -6 0 7424.48 417.441 6
6 -6 0 6884.63 400.888 7
7 -6 0-63.8112 141.166 6
-7 -6 0-39.0427 142.081 5
-7 -6 0 16.8405 133.518 3
7 -6 0-67.9404 151.368 7
8 -6 0 25.0194 126.295 6
-8 -6 0-44.1037 119.938 5
8 -6 0 184.990 154.602 7
9 -6 0 4032.14 300.136 6
9 -6 0 3736.74 297.108 7
-9 -6 0 3625.57 283.416 5
10 -6 0-64.4704 100.993 6
-10 -6 0 20.9140 100.167 5
10 -6 0 85.4487 101.521 7
-11 6 0 126.948 108.611 13
0 -7 0 5.41473 115.482 5
0 -7 0-50.1993 124.723 6
0 -7 0 111.747 104.121 7
0 -7 0 27.1225 138.845 3
-1 -7 0 17883.3 565.394 7
-1 -7 0 17290.2 577.838 5
-1 -7 0 17629.0 561.844 6
-1 -7 0 17280.1 583.099 3
1 -7 0 17223.0 587.146 6
-1 -7 0 17787.3 543.282 4
1 -7 0 17940.8 597.466 7
1 -7 0 18235.6 561.565 3
1 -7 0 17070.9 558.454 5
2 -7 0 13284.7 481.783 5
-2 -7 0 12527.4 460.011 7
2 -7 0 12660.5 520.495 6
-2 -7 0 12788.8 465.145 6
2 -7 0 12861.7 524.667 7
-2 -7 0 12782.9 515.780 3
-2 -7 0 13406.4 519.135 5
-3 -7 0 22136.7 687.302 3
3 -7 0 21118.5 676.089 6
3 -7 0 20952.8 670.847 7
-3 -7 0 22263.9 675.051 5
-4 -7 0 6455.72 386.784 5
4 -7 0 6456.58 400.695 6
4 -7 0 6343.78 395.880 7
-4 -7 0 6186.42 390.818 3
5 -7 0 815.270 208.517 6
5 -7 0 807.040 208.741 7
-5 -7 0 554.229 177.471 3
-5 -7 0 798.748 189.590 5
-6 -7 0 2596.57 270.627 5
-6 -7 0 2493.96 270.342 3
6 -7 0 2531.29 277.080 6
6 -7 0 2710.68 290.009 7
7 -7 0 58.5334 145.748 6
-7 -7 0 291.144 156.434 5
-7 -7 0 327.062 155.708 3
7 -7 0 80.1737 150.958 7
8 -7 0 62.5952 125.392 6
8 -7 0-55.1937 134.932 7
-8 -7 0 10.0656 121.323 5
9 -7 0 1965.01 210.323 6
9 -7 0 1925.09 212.768 7
-9 -7 0 1793.17 206.625 5
-10 -7 0-81.1786 83.7892 5
10 -7 0 28.3228 79.5108 6
-11 7 0 381.216 97.9586 13
0 -8 0 406.818 137.371 5
0 -8 0 500.498 146.687 6
0 -8 0 524.161 163.480 3
0 -8 0 663.380 156.053 7
-1 -8 0-75.0370 105.780 7
1 -8 0 38.1057 120.003 5
1 -8 0 94.8437 125.627 6
-1 -8 0 130.402 131.968 6
-1 -8 0-155.817 182.227 3
1 -8 0 34.1127 134.768 7
-1 -8 0-40.2504 132.463 5
1 -8 0-111.401 165.455 3
-2 -8 0-197.694 140.773 5
2 -8 0-82.6117 140.961 7
2 -8 0 44.6185 112.102 5
-2 -8 0 78.9869 143.481 3
2 -8 0-6.36641 150.998 6
-3 -8 0-34.5071 159.605 3
3 -8 0-49.5720 142.080 6
-3 -8 0 35.8819 138.625 5
3 -8 0 36.0798 145.665 7
4 -8 0 1647.30 236.448 6
4 -8 0 1474.24 234.281 7
-4 -8 0 1647.37 239.780 5
-4 -8 0 1409.02 232.724 3
5 -8 0 180.288 152.200 6
-5 -8 0 256.982 148.988 5
-5 -8 0 118.839 150.226 3
5 -8 0 256.409 145.072 7
6 -8 0 300.311 156.442 7
-6 -8 0 335.213 156.535 5
6 -8 0 293.919 146.066 6
-7 -8 0 73.8745 110.839 5
7 -8 0-9.70598 112.119 6
7 -8 0-8.02536 126.439 7
8 -8 0-38.4161 112.825 7
-8 -8 0-68.0467 105.365 5
8 -8 0 18.6658 93.9884 6
9 -8 0 197.189 97.3563 6
-9 -8 0 231.181 93.9067 5
9 -8 0 228.388 98.6483 7
0 -9 0 182.402 115.582 7
0 -9 0 87.3097 101.403 6
0 -9 0 77.0036 97.9867 5
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6 -1 -17 502.638 119.366 10
-6 1 17 177.788 100.328 9
-6 -1 17 386.389 114.405 9
6 -1 -17 497.696 115.073 8
5 -1 -17 220.283 105.173 10
5 1 -17 227.619 82.3786 10
-5 1 17 21.5402 110.103 9
-5 -1 17 459.528 137.239 9
5 1 -17 313.573 108.526 8
5 -1 -17 355.912 117.886 8
4 -1 -17 494.805 119.444 10
4 1 -17 333.192 99.7063 10
-4 1 17 426.487 119.118 9
4 1 -17 448.423 108.106 8
4 -1 -17 604.907 134.947 8
3 -1 -17-54.6689 98.3295 10
3 1 -17-64.3045 82.4077 10
3 1 -17-11.3794 81.8422 8
3 -1 -17 22.4466 98.7306 8
2 -1 -17 87.8516 85.1783 14
2 1 -17-102.086 77.2648 8
2 -1 -17-49.3658 88.9743 8
1 -1 -17 26.0737 82.1930 14
1 1 -17 31.4487 89.4967 8
1 -1 -17 1.45223 89.8937 8
0 -1 -17 85.6771 80.8522 14
0 1 -17-126.536 75.0409 14
0 1 -17 124.429 68.5467 8
0 -1 -17 19.7095 85.9878 8
-1 -1 -17 51.9700 83.3445 14
-1 1 -17 59.4386 68.9739 14
-1 -1 -17 39.3615 75.3723 8
-2 -1 -17 34.0455 65.1356 14
8 -2 -17 144.905 73.4734 10
-8 -2 17 149.117 86.1974 9
7 -2 -17 221.266 87.5110 10
-7 -2 17 81.0806 83.8045 9
-6 -2 17 417.558 121.845 3
6 -2 -17 701.784 125.395 10
-6 -2 17 273.772 100.720 9
6 -2 -17 482.512 110.853 8
-5 -2 17 608.301 131.906 3
5 -2 -17 512.188 109.558 10
-5 2 17 389.188 101.937 9
-5 -2 17 456.835 123.853 9
5 -2 -17 431.541 104.874 8
-4 -2 17-5.16070 100.625 3
4 -2 -17 123.585 90.8807 10
-4 2 17-157.167 96.4960 9
4 -2 -17-31.7251 84.2287 8
3 -2 -17 7.07375 80.2174 10
3 2 -17 77.6381 69.8968 10
-3 2 17-104.548 88.8894 9
3 -2 -17 57.2118 82.4381 8
2 -2 -17 95.9007 78.9857 10
2 -2 -17-2.63246 89.9078 8
1 -2 -17-28.7384 91.7484 14
1 -2 -17-92.6325 73.0859 10
1 -2 -17 28.4985 90.4594 8
0 -2 -17 1605.91 165.416 14
0 -2 -17 1785.16 162.013 8
-1 -2 -17 3186.21 213.118 14
-1 -2 -17 3262.85 198.098 8
7 -3 -17 80.7269 62.9720 10
-6 -3 17 309.011 95.9103 3
6 -3 -17 120.446 73.9519 10
-6 -3 17 211.334 87.9461 9
6 -3 -17 248.412 81.8499 8
-5 -3 17-105.703 105.555 3
5 -3 -17 44.7604 68.4650 10
-5 -3 17-15.4875 87.2656 9
5 -3 -17 93.9214 76.5327 8
-4 -3 17 1247.06 158.662 3
4 -3 -17 1492.87 154.685 10
-4 -3 17 1391.15 152.133 9
4 -3 -17 1518.98 148.220 8
-3 -3 17 86.5754 92.8482 3
3 -3 -17 114.630 74.8998 10
3 -3 -17 211.615 88.2308 8
-2 -3 17 621.587 118.247 3
2 -3 -17 528.564 103.268 10
2 -3 -17 542.031 108.289 8
-1 -3 17 313.250 103.498 3
1 -3 -17 365.465 89.3240 10
1 -3 -17 132.032 72.9448 8
0 -3 -17 157.030 68.7209 8
-4 -4 17 135.113 96.7690 3
-3 -4 17 436.666 94.9334 3
-6 0 18 1781.54 155.147 9
5 0 -18 233.494 81.9056 10
5 0 -18 169.792 82.1863 8
4 0 -18 739.298 113.321 10
-4 0 18 970.569 136.366 9
4 0 -18 879.459 117.152 8
3 0 -18 1319.41 143.611 10
3 0 -18 1242.84 137.073 8
2 0 -18 1267.42 137.804 10
2 0 -18 1427.01 136.180 8
1 0 -18-192.495 75.0665 10
6 -1 -18 109.105 65.1227 10
-6 -1 18-140.122 84.4338 9
-5 -1 18 174.283 88.8608 3
5 -1 -18 309.533 91.1550 10
-5 -1 18 80.9393 95.9927 9
5 -1 -18 86.9772 77.6082 8
-4 -1 18 858.593 130.565 3
4 -1 -18 748.361 113.901 10
-4 1 18 658.577 114.294 9
-4 -1 18 1019.86 138.272 9
4 -1 -18 923.199 120.680 8
3 -1 -18 1924.84 165.633 10
3 1 -18 1568.19 143.650 10
-3 1 18 1715.64 151.453 9
3 -1 -18 1786.50 154.940 8
2 -1 -18-7.68646 59.2560 10
2 -1 -18-137.778 81.7068 8
1 -1 -18 785.654 111.288 10
5 -2 -18-82.8912 60.8521 10
5 -2 -18-58.4352 69.8650 8
-4 -2 18 61.9433 85.3525 3
4 -2 -18 248.610 75.7749 10
-4 -2 18 231.168 84.8918 9
4 -2 -18 234.438 79.2485 8
-3 -2 18 65.4241 79.0890 3
3 -2 -18-72.1618 59.1979 10
-3 -2 18-49.1048 81.4988 9
3 -2 -18-42.7773 73.0729 8
0 0 0 0.00 0.00 0
TITL kji190003_fa in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184 12.887442 8.845548 15.463470 90.0000 104.1083 90.0000
ZERR 4.00 0.000559 0.000304 0.000676 0.0000 0.0046 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H P
UNIT 80.00 108.00 4.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 41320
_shelx_res_file
;
kji190003_fa.res created by SHELXL-2014/7
TITL kji190003_fa in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184 12.887442 8.845548 15.46347 90 104.1083 90
ZERR 4 0.000559 0.000304 0.000676 0 0.0046 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H P
UNIT 80 108 4
SADI P1 H1a P1 H1b
SADI C6 C10B C6 C10A
SIMU C10A C10B
RIGU
L.S. 4 0 0
PLAN 20
BOND $H
list 4
fmap 2 53
acta
REM
REM
REM
WGHT 0.069800 0.735700
FVAR 4.51948
P1 3 0.756499 0.712037 0.503668 11.00000 0.03971 0.03974 =
0.04115 -0.00479 0.00459 0.00507
PART 1
H1A 2 0.822071 0.827170 0.527141 10.63232 -1.20000
PART 0
PART 2
H1B 2 0.745469 0.638906 0.574423 10.36768 -1.20000
PART 0
C1 1 0.817828 0.573804 0.441113 11.00000 0.03025 0.03245 =
0.04239 0.00082 0.00500 0.00008
C2 1 0.829416 0.609269 0.354863 11.00000 0.02936 0.03205 =
0.04285 0.00217 0.00587 -0.00079
C3 1 0.870997 0.499889 0.306939 11.00000 0.03457 0.03858 =
0.04793 0.00019 0.01165 0.00094
C4 1 0.902092 0.361002 0.346467 11.00000 0.03841 0.03625 =
0.05660 -0.00367 0.01524 0.00441
AFIX 43
H4 2 0.927218 0.287589 0.313611 11.00000 -1.20000
AFIX 0
C5 1 0.897284 0.327265 0.432532 11.00000 0.02878 0.03104 =
0.06156 0.00449 0.00942 0.00080
C6 1 0.855357 0.434828 0.481754 11.00000 0.02819 0.03615 =
0.04816 0.00752 0.00579 0.00168
C7 1 0.800333 0.762767 0.314180 11.00000 0.04085 0.03548 =
0.04960 0.00713 0.00975 0.00386
AFIX 137
H7A 2 0.725209 0.780161 0.307172 11.00000 -1.50000
H7B 2 0.816832 0.767163 0.256951 11.00000 -1.50000
H7C 2 0.840407 0.838894 0.352466 11.00000 -1.50000
AFIX 0
C8 1 0.885069 0.529634 0.214251 11.00000 0.05871 0.05785 =
0.05278 0.00117 0.02245 0.00456
AFIX 137
H8A 2 0.913013 0.440734 0.192397 11.00000 -1.50000
H8B 2 0.933981 0.612118 0.216133 11.00000 -1.50000
H8C 2 0.817152 0.554947 0.175334 11.00000 -1.50000
AFIX 0
C9 1 0.938769 0.176413 0.472143 11.00000 0.03684 0.03522 =
0.07769 0.01120 0.01145 0.00624
AFIX 137
H9A 2 0.885026 0.127768 0.495763 11.00000 -1.50000
H9B 2 1.001995 0.191742 0.519129 11.00000 -1.50000
H9C 2 0.955652 0.113860 0.426709 11.00000 -1.50000
AFIX 0
C11 1 0.620507 0.749354 0.432856 11.00000 0.03418 0.02929 =
0.03715 -0.00390 0.01350 -0.00056
C12 1 0.551124 0.628369 0.399596 11.00000 0.03630 0.03007 =
0.03937 -0.00303 0.01681 -0.00266
C13 1 0.448287 0.659746 0.346214 11.00000 0.03758 0.03518 =
0.03862 -0.00682 0.01620 -0.00672
C14 1 0.416512 0.808291 0.329531 11.00000 0.03144 0.04280 =
0.03907 -0.00316 0.01153 -0.00085
AFIX 43
H14 2 0.348820 0.827938 0.293482 11.00000 -1.20000
AFIX 0
C15 1 0.482049 0.929525 0.364671 11.00000 0.03602 0.03261 =
0.03842 -0.00055 0.01514 0.00154
C16 1 0.585306 0.900186 0.417120 11.00000 0.03417 0.02961 =
0.03653 -0.00239 0.01316 -0.00167
C17 1 0.582732 0.465991 0.420983 11.00000 0.04446 0.02833 =
0.05706 -0.00113 0.01797 -0.00236
AFIX 137
H17A 2 0.521363 0.409410 0.427121 11.00000 -1.50000
H17B 2 0.637151 0.461489 0.475774 11.00000 -1.50000
H17C 2 0.609811 0.423670 0.373673 11.00000 -1.50000
AFIX 0
C18 1 0.373318 0.533484 0.305590 11.00000 0.04280 0.04433 =
0.05491 -0.01390 0.01718 -0.01279
AFIX 137
H18A 2 0.408083 0.468619 0.271570 11.00000 -1.50000
H18B 2 0.309881 0.575441 0.267227 11.00000 -1.50000
H18C 2 0.354323 0.476112 0.352143 11.00000 -1.50000
AFIX 0
C19 1 0.440517 1.088617 0.344678 11.00000 0.04289 0.03616 =
0.05321 0.00311 0.01522 0.00632
AFIX 137
H19A 2 0.372795 1.085660 0.301679 11.00000 -1.50000
H19B 2 0.490583 1.146060 0.321131 11.00000 -1.50000
H19C 2 0.431778 1.135240 0.398517 11.00000 -1.50000
AFIX 0
C20 1 0.654940 1.033514 0.455478 11.00000 0.04111 0.02933 =
0.05360 -0.00434 0.01024 -0.00300
AFIX 137
H20A 2 0.693090 1.067968 0.413079 11.00000 -1.50000
H20B 2 0.705074 1.003359 0.509418 11.00000 -1.50000
H20C 2 0.610844 1.113824 0.468276 11.00000 -1.50000
AFIX 0
PART 1
C10A 1 0.848026 0.403729 0.576483 10.63232 0.04348 0.04230 =
0.05323 0.01678 0.00616 0.01259
AFIX 137
H10A 2 0.832156 0.496009 0.603312 10.63232 -1.50000
H10B 2 0.914997 0.364052 0.610309 10.63232 -1.50000
H10C 2 0.792281 0.331431 0.575821 10.63232 -1.50000
AFIX 0
PART 0
PART 2
C10B 1 0.858966 0.383549 0.575870 10.36768 0.04527 0.04533 =
0.05019 0.00935 0.01623 0.01883
AFIX 137
H10D 2 0.865709 0.470074 0.614317 10.36768 -1.50000
H10E 2 0.919209 0.317835 0.596480 10.36768 -1.50000
H10F 2 0.794267 0.330229 0.576479 10.36768 -1.50000
AFIX 0
HKLF 4
REM kji190003_fa in P2(1)/c
REM R1 = 0.0472 for 2424 Fo > 4sig(Fo) and 0.0610 for all 3021 data
REM 214 parameters refined using 182 restraints
END
WGHT 0.0698 0.7358
REM Highest difference peak 0.426, deepest hole -0.347, 1-sigma level 0.046
Q1 1 0.7038 0.6399 0.5000 11.00000 0.05 0.43
Q2 1 0.8018 0.8233 0.4700 11.00000 0.05 0.31
Q3 1 0.7925 0.7126 0.5820 11.00000 0.05 0.28
Q4 1 0.8167 0.8013 0.5610 11.00000 0.05 0.27
Q5 1 0.8715 0.8153 0.3046 11.00000 0.05 0.26
Q6 1 0.7790 0.8338 0.3593 11.00000 0.05 0.23
Q7 1 0.7533 0.7589 0.2552 11.00000 0.05 0.23
Q8 1 0.5859 0.6955 0.4228 11.00000 0.05 0.21
Q9 1 0.6051 0.8220 0.4319 11.00000 0.05 0.21
Q10 1 0.8404 0.5559 0.3252 11.00000 0.05 0.19
Q11 1 0.8448 0.5979 0.4032 11.00000 0.05 0.19
Q12 1 0.8280 0.4906 0.4556 11.00000 0.05 0.18
Q13 1 0.4997 0.6388 0.3591 11.00000 0.05 0.18
Q14 1 0.8613 0.5732 0.3367 11.00000 0.05 0.18
Q15 1 0.4187 0.6071 0.3320 11.00000 0.05 0.17
Q16 1 0.4590 0.8719 0.3542 11.00000 0.05 0.17
Q17 1 0.6157 0.9556 0.4408 11.00000 0.05 0.16
Q18 1 0.8054 0.5938 0.3733 11.00000 0.05 0.16
Q19 1 0.9008 0.4437 0.3432 11.00000 0.05 0.16
Q20 1 0.9566 0.4973 0.2095 11.00000 0.05 0.16
;
_shelx_res_checksum 58875
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
_atom_site_disorder_assembly
_atom_site_disorder_group
P P1 0.75650(5) 0.71204(7) 0.50367(4) 0.0411(2) Uani d 1 . .
H H1A 0.822(3) 0.827(4) 0.527(3) 0.049 Uiso d 0.6323 A 1
H H1B 0.745(6) 0.639(7) 0.574(3) 0.049 Uiso d 0.3677 B 2
C C1 0.81783(16) 0.5738(2) 0.44111(15) 0.0357(5) Uani d 1 . .
C C2 0.82942(16) 0.6093(2) 0.35486(15) 0.0353(5) Uani d 1 . .
C C3 0.87100(17) 0.4999(3) 0.30694(16) 0.0401(5) Uani d 1 . .
C C4 0.90209(18) 0.3610(3) 0.34647(17) 0.0431(5) Uani d 1 . .
H H4 0.9272 0.2876 0.3136 0.052 Uiso calc 1 . .
C C5 0.89728(17) 0.3273(2) 0.43253(17) 0.0407(5) Uani d 1 . .
C C6 0.85536(16) 0.4348(2) 0.48175(15) 0.0381(5) Uani d 1 . .
C C7 0.80033(19) 0.7628(3) 0.31418(16) 0.0422(5) Uani d 1 . .
H H7A 0.7252 0.7802 0.3072 0.063 Uiso calc 1 . .
H H7B 0.8168 0.7672 0.2570 0.063 Uiso calc 1 . .
H H7C 0.8404 0.8389 0.3525 0.063 Uiso calc 1 . .
C C8 0.8851(2) 0.5296(3) 0.21425(18) 0.0549(6) Uani d 1 . .
H H8A 0.9130 0.4407 0.1924 0.082 Uiso calc 1 . .
H H8B 0.9340 0.6121 0.2161 0.082 Uiso calc 1 . .
H H8C 0.8172 0.5549 0.1753 0.082 Uiso calc 1 . .
C C9 0.93877(19) 0.1764(3) 0.47214(19) 0.0504(6) Uani d 1 . .
H H9A 0.8850 0.1278 0.4958 0.076 Uiso calc 1 . .
H H9B 1.0020 0.1917 0.5191 0.076 Uiso calc 1 . .
H H9C 0.9557 0.1139 0.4267 0.076 Uiso calc 1 . .
C C11 0.62051(16) 0.7494(2) 0.43286(14) 0.0327(4) Uani d 1 . .
C C12 0.55112(17) 0.6284(2) 0.39960(14) 0.0339(5) Uani d 1 . .
C C13 0.44829(17) 0.6597(2) 0.34621(14) 0.0359(5) Uani d 1 . .
C C14 0.41651(17) 0.8083(3) 0.32953(14) 0.0373(5) Uani d 1 . .
H H14 0.3488 0.8279 0.2935 0.045 Uiso calc 1 . .
C C15 0.48205(17) 0.9295(2) 0.36467(14) 0.0346(5) Uani d 1 . .
C C16 0.58531(16) 0.9002(2) 0.41712(14) 0.0326(5) Uani d 1 . .
C C17 0.58273(19) 0.4660(2) 0.42098(17) 0.0423(5) Uani d 1 . .
H H17A 0.5214 0.4094 0.4271 0.063 Uiso calc 1 . .
H H17B 0.6372 0.4615 0.4758 0.063 Uiso calc 1 . .
H H17C 0.6098 0.4237 0.3737 0.063 Uiso calc 1 . .
C C18 0.37332(19) 0.5335(3) 0.30559(17) 0.0464(6) Uani d 1 . .
H H18A 0.4081 0.4686 0.2716 0.070 Uiso calc 1 . .
H H18B 0.3099 0.5754 0.2672 0.070 Uiso calc 1 . .
H H18C 0.3543 0.4761 0.3521 0.070 Uiso calc 1 . .
C C19 0.44052(19) 1.0886(3) 0.34468(17) 0.0435(5) Uani d 1 . .
H H19A 0.3728 1.0857 0.3017 0.065 Uiso calc 1 . .
H H19B 0.4906 1.1461 0.3211 0.065 Uiso calc 1 . .
H H19C 0.4318 1.1352 0.3985 0.065 Uiso calc 1 . .
C C20 0.65494(19) 1.0335(2) 0.45548(16) 0.0416(5) Uani d 1 . .
H H20A 0.6931 1.0680 0.4131 0.062 Uiso calc 1 . .
H H20B 0.7051 1.0034 0.5094 0.062 Uiso calc 1 . .
H H20C 0.6108 1.1138 0.4683 0.062 Uiso calc 1 . .
C C10A 0.848(2) 0.404(3) 0.5765(8) 0.047(3) Uani d 0.6323 C 1
H H10A 0.8322 0.4960 0.6033 0.071 Uiso calc 0.6323 C 1
H H10B 0.9150 0.3641 0.6103 0.071 Uiso calc 0.6323 C 1
H H10C 0.7923 0.3314 0.5758 0.071 Uiso calc 0.6323 C 1
C C10B 0.859(4) 0.384(5) 0.5759(14) 0.046(5) Uani d 0.3677 C 2
H H10D 0.8657 0.4701 0.6143 0.069 Uiso calc 0.3677 C 2
H H10E 0.9192 0.3178 0.5965 0.069 Uiso calc 0.3677 C 2
H H10F 0.7943 0.3302 0.5765 0.069 Uiso calc 0.3677 C 2
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
P1 0.0397(3) 0.0397(3) 0.0411(3) 0.0051(2) 0.0046(2) -0.0048(2)
C1 0.0302(10) 0.0325(10) 0.0424(11) 0.0001(8) 0.0050(8) 0.0008(9)
C2 0.0294(10) 0.0320(10) 0.0429(11) -0.0008(8) 0.0059(9) 0.0022(8)
C3 0.0346(11) 0.0386(11) 0.0479(12) 0.0009(9) 0.0116(9) 0.0002(9)
C4 0.0384(12) 0.0362(12) 0.0566(14) 0.0044(10) 0.0152(10) -0.0037(10)
C5 0.0288(10) 0.0310(11) 0.0616(14) 0.0008(9) 0.0094(10) 0.0045(10)
C6 0.0282(10) 0.0361(11) 0.0482(12) 0.0017(9) 0.0058(9) 0.0075(9)
C7 0.0409(12) 0.0355(11) 0.0496(13) 0.0039(9) 0.0097(10) 0.0071(9)
C8 0.0587(15) 0.0579(16) 0.0528(15) 0.0046(13) 0.0225(12) 0.0012(12)
C9 0.0368(12) 0.0352(12) 0.0777(18) 0.0062(10) 0.0114(12) 0.0112(11)
C11 0.0342(10) 0.0293(10) 0.0372(11) -0.0006(8) 0.0135(8) -0.0039(8)
C12 0.0363(11) 0.0301(10) 0.0394(11) -0.0027(8) 0.0168(9) -0.0030(8)
C13 0.0376(11) 0.0352(11) 0.0386(11) -0.0067(9) 0.0162(9) -0.0068(9)
C14 0.0314(10) 0.0428(12) 0.0391(11) -0.0008(9) 0.0115(9) -0.0032(9)
C15 0.0360(11) 0.0326(10) 0.0384(11) 0.0015(9) 0.0151(9) -0.0006(8)
C16 0.0342(10) 0.0296(10) 0.0365(11) -0.0017(8) 0.0132(8) -0.0024(8)
C17 0.0445(12) 0.0283(11) 0.0571(14) -0.0024(9) 0.0180(11) -0.0011(10)
C18 0.0428(13) 0.0443(13) 0.0549(14) -0.0128(10) 0.0172(11) -0.0139(11)
C19 0.0429(12) 0.0362(12) 0.0532(14) 0.0063(10) 0.0152(11) 0.0031(10)
C20 0.0411(12) 0.0293(11) 0.0536(14) -0.0030(9) 0.0102(10) -0.0043(9)
C10A 0.043(6) 0.042(6) 0.053(3) 0.013(5) 0.006(3) 0.017(3)
C10B 0.045(9) 0.045(10) 0.050(5) 0.019(6) 0.016(5) 0.009(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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0572
-1 0 0 0.0582
0 -1 0 0.1700
0 1 0 0.1940
-1 0 2 0.0215
1 0 -2 0.0285
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
C1 P1 H1A . . 109.1(18) ?
C1 P1 H1B . . 105(3) ?
C1 P1 C11 . . 105.74(9) ?
C11 P1 H1A . . 118.4(18) ?
C11 P1 H1B . . 108(3) ?
C2 C1 P1 . . 120.22(16) ?
C6 C1 P1 . . 119.09(17) ?
C6 C1 C2 . . 120.7(2) ?
C1 C2 C7 . . 121.5(2) ?
C3 C2 C1 . . 119.18(19) ?
C3 C2 C7 . . 119.3(2) ?
C2 C3 C8 . . 122.1(2) ?
C4 C3 C2 . . 119.0(2) ?
C4 C3 C8 . . 118.9(2) ?
C3 C4 H4 . . 118.6 ?
C5 C4 C3 . . 122.7(2) ?
C5 C4 H4 . . 118.6 ?
C4 C5 C6 . . 119.3(2) ?
C4 C5 C9 . . 119.2(2) ?
C6 C5 C9 . . 121.5(2) ?
C1 C6 C10A . . 119.5(9) ?
C1 C6 C10B . . 128.0(15) ?
C5 C6 C1 . . 118.9(2) ?
C5 C6 C10A . . 121.5(9) ?
C5 C6 C10B . . 113.1(15) ?
C2 C7 H7A . . 109.5 ?
C2 C7 H7B . . 109.5 ?
C2 C7 H7C . . 109.5 ?
H7A C7 H7B . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C3 C8 H8A . . 109.5 ?
C3 C8 H8B . . 109.5 ?
C3 C8 H8C . . 109.5 ?
H8A C8 H8B . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
C5 C9 H9A . . 109.5 ?
C5 C9 H9B . . 109.5 ?
C5 C9 H9C . . 109.5 ?
H9A C9 H9B . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
C12 C11 P1 . . 120.29(16) ?
C12 C11 C16 . . 120.43(19) ?
C16 C11 P1 . . 119.18(15) ?
C11 C12 C17 . . 122.0(2) ?
C13 C12 C11 . . 119.16(19) ?
C13 C12 C17 . . 118.81(19) ?
C12 C13 C18 . . 120.9(2) ?
C14 C13 C12 . . 119.39(19) ?
C14 C13 C18 . . 119.7(2) ?
C13 C14 H14 . . 118.8 ?
C13 C14 C15 . . 122.4(2) ?
C15 C14 H14 . . 118.8 ?
C14 C15 C16 . . 118.89(19) ?
C14 C15 C19 . . 119.2(2) ?
C16 C15 C19 . . 121.96(19) ?
C11 C16 C20 . . 122.31(19) ?
C15 C16 C11 . . 119.61(19) ?
C15 C16 C20 . . 118.08(18) ?
C12 C17 H17A . . 109.5 ?
C12 C17 H17B . . 109.5 ?
C12 C17 H17C . . 109.5 ?
H17A C17 H17B . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
C13 C18 H18A . . 109.5 ?
C13 C18 H18B . . 109.5 ?
C13 C18 H18C . . 109.5 ?
H18A C18 H18B . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
C15 C19 H19A . . 109.5 ?
C15 C19 H19B . . 109.5 ?
C15 C19 H19C . . 109.5 ?
H19A C19 H19B . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 109.5 ?
C16 C20 H20A . . 109.5 ?
C16 C20 H20B . . 109.5 ?
C16 C20 H20C . . 109.5 ?
H20A C20 H20B . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
C6 C10A H10A . . 109.5 ?
C6 C10A H10B . . 109.5 ?
C6 C10A H10C . . 109.5 ?
H10A C10A H10B . . 109.5 ?
H10A C10A H10C . . 109.5 ?
H10B C10A H10C . . 109.5 ?
C6 C10B H10D . . 109.5 ?
C6 C10B H10E . . 109.5 ?
C6 C10B H10F . . 109.5 ?
H10D C10B H10E . . 109.5 ?
H10D C10B H10F . . 109.5 ?
H10E C10B H10F . . 109.5 ?
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
P1 H1A . 1.32(4) ?
P1 H1B . 1.31(4) ?
P1 C1 . 1.852(2) ?
P1 C11 . 1.856(2) ?
C1 C2 . 1.413(3) ?
C1 C6 . 1.411(3) ?
C2 C3 . 1.402(3) ?
C2 C7 . 1.505(3) ?
C3 C4 . 1.387(3) ?
C3 C8 . 1.511(3) ?
C4 H4 . 0.9300 ?
C4 C5 . 1.380(3) ?
C5 C6 . 1.406(3) ?
C5 C9 . 1.511(3) ?
C6 C10A . 1.516(8) ?
C6 C10B . 1.514(13) ?
C7 H7A . 0.9600 ?
C7 H7B . 0.9600 ?
C7 H7C . 0.9600 ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
C9 H9A . 0.9600 ?
C9 H9B . 0.9600 ?
C9 H9C . 0.9600 ?
C11 C12 . 1.409(3) ?
C11 C16 . 1.411(3) ?
C12 C13 . 1.408(3) ?
C12 C17 . 1.508(3) ?
C13 C14 . 1.382(3) ?
C13 C18 . 1.510(3) ?
C14 H14 . 0.9300 ?
C14 C15 . 1.391(3) ?
C15 C16 . 1.404(3) ?
C15 C19 . 1.511(3) ?
C16 C20 . 1.513(3) ?
C17 H17A . 0.9600 ?
C17 H17B . 0.9600 ?
C17 H17C . 0.9600 ?
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 ?
C10A H10A . 0.9600 ?
C10A H10B . 0.9600 ?
C10A H10C . 0.9600 ?
C10B H10D . 0.9600 ?
C10B H10E . 0.9600 ?
C10B H10F . 0.9600 ?