#------------------------------------------------------------------------------
#$Date: 2025-01-31 04:49:21 +0200 (Fri, 31 Jan 2025) $
#$Revision: 297542 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/33/2023366.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_2023366
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 13
_space_group_name_Hall '-P 2yac'
_space_group_name_H-M_alt 'P 1 2/n 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 96.020(2)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 6.5476(2)
_cell_length_b 5.9910(2)
_cell_length_c 21.5676(6)
_cell_measurement_reflns_used 4245
_cell_measurement_temperature 150.0(2)
_cell_measurement_theta_max 66.3590
_cell_measurement_theta_min 4.0830
_cell_volume 841.36(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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 0.0400
_diffrn_reflns_av_unetI/netI 0.0199
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 11409
_diffrn_reflns_theta_full 66.852
_diffrn_reflns_theta_max 66.852
_diffrn_reflns_theta_min 4.122
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 1.354
_exptl_absorpt_correction_T_max 0.866
_exptl_absorpt_correction_T_min 0.696
_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 1.178
_exptl_crystal_description block
_exptl_crystal_F_000 324
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.06
_refine_diff_density_max 0.272
_refine_diff_density_min -0.236
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.063
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 103
_refine_ls_number_reflns 1500
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.063
_refine_ls_R_factor_all 0.0470
_refine_ls_R_factor_gt 0.0393
_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^)+(0.0665P)^2^+0.3189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1096
_refine_ls_wR_factor_ref 0.1181
_reflns_number_gt 1299
_reflns_number_total 1500
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file oj3027.cif
_cod_data_source_block kji190001_fa
_cod_database_code 2023366
_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 0.737
_shelx_estimated_absorpt_t_max 0.923
_shelx_hkl_file
;
0 0 -2 1136.84 11.36
0 0 -3 0.62 1.30
0 0 -4 2643.62 24.69
0 0 -5 -0.42 2.31
0 0 -6 554.05 14.24
0 0 -7 3.03 2.64
0 0 -8 659.29 18.21
0 0 -9 2.20 3.51
0 0 -10 80.64 8.18
0 0 -11 0.33 3.45
0 0 -12 1313.46 33.11
0 0 -13 -0.15 1.04
0 0 -13 2.88 3.49
0 0 -14 255.57 7.77
0 0 -14 254.90 7.81
0 0 -14 268.45 8.79
0 0 -14 266.59 8.62
0 0 14 258.21 8.01
0 0 -14 265.79 16.96
0 0 15 -2.93 1.09
0 0 -15 -1.86 5.43
0 0 -15 0.93 1.56
0 0 -15 0.79 2.34
0 0 -15 1.48 1.70
0 0 -15 1.67 1.48
0 0 -16 -1.46 1.11
0 0 -16 2.10 2.24
0 0 -16 0.59 1.78
0 0 16 4.44 1.49
0 0 -16 0.35 1.56
0 0 -16 -0.38 3.89
0 0 -17 2.08 1.39
0 0 -17 -4.47 1.91
0 0 -17 0.25 2.06
0 0 17 0.76 1.24
0 0 -17 1.45 2.41
0 0 -17 3.63 4.67
0 0 -18 72.91 5.50
0 0 -18 70.95 4.69
0 0 -18 78.08 10.98
0 0 -18 71.48 5.61
0 0 -18 72.44 4.80
0 0 -19 4.99 2.00
0 0 -19 2.48 1.81
0 0 -19 0.22 2.37
0 0 -20 176.19 8.82
0 0 -20 181.61 8.48
0 0 -21 -0.88 2.64
0 0 -21 -3.61 2.45
0 0 -21 0.35 2.24
0 0 -22 26.69 3.48
0 0 -22 28.04 4.01
0 0 -22 32.43 3.86
0 0 -23 -2.16 2.21
0 0 -23 -0.83 2.32
0 0 -23 0.25 1.63
0 0 -24 48.67 3.96
0 0 -24 47.53 4.05
0 0 -24 46.04 3.84
0 0 -25 1.40 1.70
0 0 -25 -1.10 1.46
0 0 -25 2.96 1.29
0 -1 0 4402.02 30.72
0 1 0 4522.57 26.13
0 -1 1 32.14 3.11
0 1 -1 33.18 2.84
0 1 1 35.57 2.49
0 -1 -1 31.88 2.90
0 -1 -1 34.14 3.32
0 -1 -2 227.66 7.71
0 -1 2 235.79 7.66
0 -1 -2 218.42 7.12
0 1 2 228.19 6.09
0 1 -2 225.28 7.45
0 1 -3 2142.04 25.00
0 -1 -3 2134.01 24.18
0 1 -3 2155.18 20.05
0 -1 3 2102.09 23.82
0 1 -4 1.35 2.67
0 1 -4 0.97 1.65
0 -1 -4 1.61 2.37
0 -1 -5 0.94 2.40
0 1 -5 2.16 1.88
0 1 -5 1.40 2.61
0 1 -6 284.09 10.08
0 -1 -6 288.94 11.62
0 1 -7 6.49 2.98
0 -1 -7 7.72 3.83
0 -1 -8 293.60 13.62
0 1 -8 274.87 11.56
0 1 -9 2014.40 33.05
0 -1 -9 1983.16 36.50
0 1 -10 255.48 12.93
0 -1 -10 276.22 15.03
0 -1 -11 578.53 22.70
0 1 -11 618.99 20.83
0 1 -12 52.53 3.86
0 1 -12 49.28 3.52
0 1 -12 48.61 6.42
0 -1 -12 45.38 3.55
0 -1 -12 50.95 8.15
0 1 -12 50.76 3.66
0 1 -13 24.14 2.71
0 -1 -13 28.27 2.73
0 1 -13 32.36 3.17
0 -1 -13 25.74 2.64
0 1 13 24.01 2.91
0 1 -13 28.85 3.02
0 1 -13 20.90 4.28
0 -1 -13 31.81 6.40
0 1 -13 28.27 3.06
0 -1 -13 29.75 2.93
0 1 14 15.34 2.39
0 -1 -14 14.04 6.73
0 1 -14 15.69 2.29
0 -1 -14 11.39 2.02
0 -1 -14 13.36 2.26
0 1 -14 7.91 2.27
0 1 -14 16.06 2.69
0 -1 -14 18.10 2.60
0 1 -14 9.22 4.53
0 -1 -15 92.66 11.83
0 1 -15 91.96 5.47
0 1 -15 87.62 5.53
0 1 -15 92.20 10.37
0 -1 -15 90.20 5.39
0 1 15 91.30 5.41
0 -1 -15 89.18 5.41
0 1 -15 92.67 5.37
0 -1 -15 89.45 5.16
0 -1 -16 24.58 3.41
0 -1 -16 22.28 3.52
0 -1 -16 27.34 3.48
0 -1 -16 20.28 8.85
0 1 -16 21.45 3.41
0 1 16 22.61 2.85
0 1 -16 25.26 3.66
0 1 -16 24.92 3.21
0 1 -16 36.93 7.38
0 -1 -16 22.45 3.04
0 -1 -17 33.41 4.39
0 1 -17 26.67 3.75
0 1 17 32.35 3.63
0 -1 -17 34.99 3.83
0 -1 -17 31.38 9.30
0 1 -17 31.52 4.06
0 -1 -17 30.04 3.47
0 -1 -17 28.84 3.52
0 1 -17 32.04 3.69
0 1 -18 5.62 2.44
0 1 -18 0.93 2.35
0 1 -18 0.78 2.07
0 -1 -18 3.24 2.76
0 -1 -18 2.48 1.83
0 -1 -18 2.08 1.70
0 -1 -18 6.20 1.98
0 1 18 5.04 1.40
0 1 -19 63.10 5.12
0 1 19 66.45 5.24
0 1 -19 66.54 5.68
0 1 -19 62.84 5.19
0 -1 -19 69.56 5.20
0 -1 -19 58.10 4.65
0 -1 -19 62.72 4.81
0 -1 -19 66.28 6.01
0 1 -20 38.14 4.17
0 -1 -20 33.77 3.63
0 -1 -20 36.28 4.88
0 1 -20 33.19 3.98
0 1 -20 36.67 4.15
0 1 -20 34.57 4.69
0 -1 -20 29.97 3.66
0 -1 -20 34.26 3.94
0 1 20 28.32 3.44
0 1 -21 13.33 2.93
0 1 -21 22.52 3.39
0 -1 -21 24.93 3.86
0 -1 -21 19.12 2.81
0 1 -21 23.38 3.90
0 1 -21 16.02 2.82
0 -1 -21 24.74 3.72
0 1 -22 5.82 2.70
0 1 -22 10.03 2.58
0 -1 -22 4.19 1.53
0 -1 -22 6.73 2.92
0 -1 -22 6.33 2.81
0 1 -22 5.53 2.10
0 1 -22 6.69 1.92
0 1 -23 6.54 1.64
0 -1 -23 6.48 2.96
0 -1 -23 1.63 1.43
0 1 -23 5.73 1.85
0 1 -23 3.18 2.23
0 -1 -23 5.03 2.48
0 1 -23 2.83 1.96
0 -1 -24 4.28 2.39
0 1 -24 1.97 1.68
0 -1 -24 3.35 1.77
0 1 -24 3.18 1.63
0 -1 -25 28.31 2.96
0 -1 -25 26.92 2.87
0 1 -25 24.84 2.66
0 -2 0 210.86 9.90
0 2 0 221.15 8.41
0 2 1 0.30 1.77
0 2 -1 4.99 2.22
0 -2 1 1.52 2.20
0 -2 -1 -0.02 3.03
0 2 2 1440.59 20.34
0 -2 -2 1458.67 25.96
0 -2 -2 1485.55 24.28
0 2 -2 1422.36 23.81
0 -2 2 1477.55 26.03
0 -2 -3 44.93 5.02
0 2 3 39.72 3.70
0 2 -3 39.21 4.98
0 -2 -3 46.29 5.65
0 -2 3 39.94 5.37
0 -2 4 227.62 11.25
0 2 -4 243.24 9.44
0 -2 -4 236.99 11.08
0 -2 -4 234.51 11.78
0 2 -4 220.12 10.77
0 2 4 236.00 8.66
0 2 -5 144.70 9.47
0 2 5 154.76 7.58
0 -2 5 148.60 9.43
0 2 -5 154.30 7.77
0 -2 -5 151.17 10.05
0 -2 -5 151.03 9.50
0 -2 -6 -0.63 3.53
0 2 6 3.90 2.42
0 2 -6 -1.05 2.76
0 2 -6 0.42 1.99
0 -2 6 -4.12 3.90
0 -2 -6 4.29 3.73
0 -2 -7 265.78 14.11
0 -2 7 271.05 13.79
0 2 -7 271.94 11.40
0 2 7 274.31 11.27
0 -2 -7 278.15 13.97
0 -2 8 336.03 15.98
0 2 -8 351.81 13.69
0 -2 -8 321.85 15.88
0 -2 -9 330.96 17.09
0 -2 9 327.50 16.37
0 2 -9 322.98 13.85
0 -2 -10 75.15 4.52
0 2 -10 78.79 4.44
0 2 10 88.93 4.74
0 -2 10 78.48 8.95
0 -2 -10 83.88 9.09
0 -2 -10 81.54 4.59
0 2 -10 70.27 6.88
0 2 -11 6.11 1.82
0 -2 -11 7.16 2.01
0 2 -11 8.02 2.00
0 -2 -11 5.86 2.15
0 -2 -11 5.84 1.87
0 -2 -11 10.03 5.19
0 2 -11 3.16 2.38
0 -2 11 12.98 3.88
0 2 11 14.33 2.25
0 2 -11 6.30 1.69
0 2 -11 5.88 1.53
0 2 -12 39.67 3.43
0 -2 -12 42.49 8.22
0 -2 -12 44.26 3.83
0 2 -12 42.21 3.69
0 2 -12 41.15 3.38
0 2 -12 45.95 3.61
0 -2 12 43.73 8.12
0 -2 -12 47.80 3.97
0 -2 -12 37.58 3.41
0 2 -12 40.78 3.25
0 2 12 36.57 3.29
0 2 -12 42.45 5.69
0 2 -12 43.53 3.25
0 2 -13 0.45 0.46
0 2 13 -0.01 1.21
0 -2 -13 0.03 2.02
0 2 -13 1.77 1.65
0 -2 13 -0.04 4.93
0 -2 -13 -6.02 4.70
0 2 -13 1.59 0.90
0 2 -13 1.86 1.75
0 -2 -13 0.81 1.68
0 -2 -13 1.71 1.30
0 2 -13 1.09 1.35
0 -2 -14 28.02 3.64
0 -2 -14 21.28 3.24
0 -2 -14 25.77 3.39
0 2 -14 28.70 3.21
0 2 -14 27.69 3.02
0 -2 14 14.45 4.82
0 2 -14 24.93 3.63
0 2 -14 25.67 2.81
0 -2 -14 25.04 6.83
0 2 -14 27.46 3.39
0 2 14 27.43 3.39
0 -2 -15 72.51 5.01
0 -2 -15 78.77 10.59
0 -2 -15 68.18 5.31
0 2 -15 67.42 5.17
0 2 -15 68.12 4.64
0 2 15 69.17 5.01
0 2 -15 67.97 5.23
0 2 -15 73.32 4.60
0 -2 -15 61.63 5.04
0 -2 -16 57.00 10.93
0 -2 -16 50.12 4.98
0 2 16 50.46 4.75
0 2 -16 49.23 4.60
0 -2 16 55.47 9.13
0 2 -16 54.41 4.38
0 2 -16 47.95 4.73
0 -2 -16 54.73 4.65
0 2 -16 56.47 4.15
0 -2 -16 50.48 4.96
0 2 17 45.33 4.35
0 -2 -17 46.93 4.66
0 2 -17 56.46 4.32
0 -2 -17 49.61 5.05
0 -2 -17 51.14 4.97
0 2 -17 51.49 4.43
0 2 -17 49.59 4.72
0 2 -17 51.86 5.10
0 -2 -18 2.52 2.59
0 -2 -18 4.46 2.78
0 2 -18 3.06 2.05
0 2 -18 3.36 3.06
0 2 -18 5.30 2.98
0 2 18 4.15 1.99
0 -2 -18 6.35 2.47
0 2 -19 52.95 4.32
0 -2 -19 49.21 4.93
0 -2 -19 53.50 5.20
0 2 19 44.97 4.37
0 2 -19 58.42 5.38
0 2 -19 52.83 5.57
0 -2 -20 1.69 2.02
0 -2 -20 2.73 2.20
0 2 -20 1.06 2.54
0 -2 -20 -0.69 2.29
0 2 -20 -0.54 2.47
0 2 20 2.48 1.93
0 2 -21 13.30 3.24
0 -2 -21 12.26 2.94
0 2 21 11.07 2.61
0 -2 -21 16.15 3.23
0 -2 -21 7.51 2.46
0 2 -21 14.91 3.19
0 2 -22 497.65 12.63
0 -2 -22 468.72 12.44
0 -2 -22 508.83 12.58
0 -2 -22 462.18 11.66
0 2 -22 490.19 12.45
0 2 -23 11.91 2.67
0 -2 -23 11.78 2.75
0 -2 -23 11.12 2.40
0 -2 -23 9.63 1.94
0 2 -23 15.76 2.58
0 -2 -24 66.54 4.26
0 2 -24 75.17 4.35
0 2 -24 68.81 4.18
0 -2 -24 69.49 4.26
0 -3 0 7.96 5.33
0 3 0 23.71 3.81
0 -3 -1 6.50 5.08
0 -3 1 11.93 5.26
0 3 -1 16.39 3.37
0 3 1 9.08 2.81
0 -3 2 217.77 12.85
0 -3 -2 210.07 13.05
0 3 2 219.15 10.07
0 3 -2 224.72 11.77
0 -3 3 175.12 11.93
0 -3 -3 160.82 11.76
0 3 -3 152.53 10.42
0 3 -4 208.51 10.80
0 -3 4 192.83 12.39
0 -3 -4 186.71 12.71
0 3 -4 181.82 11.69
0 -3 -5 151.50 11.55
0 -3 5 155.44 11.40
0 -3 -5 146.13 11.61
0 3 -5 159.67 11.57
0 3 -5 154.98 9.21
0 -3 6 102.07 9.79
0 3 -6 103.24 5.05
0 -3 -6 96.00 9.62
0 3 6 114.87 5.37
0 -3 -6 105.66 5.19
0 3 -6 104.94 5.01
0 -3 -6 94.40 10.25
0 3 -6 97.78 4.86
0 -3 -7 77.58 4.77
0 -3 -7 63.36 8.67
0 -3 -7 72.05 9.40
0 3 -7 69.17 4.10
0 3 7 67.07 4.30
0 -3 -7 74.06 4.23
0 -3 7 78.07 9.00
0 3 -7 71.92 4.50
0 3 -7 70.71 4.29
0 -3 -7 71.29 4.14
0 3 7 75.15 4.50
0 3 -7 67.69 4.37
0 3 -8 80.84 4.68
0 3 -8 74.74 4.63
0 3 -8 77.99 4.77
0 3 -8 66.67 4.31
0 -3 -8 83.23 4.96
0 3 8 69.30 4.43
0 -3 -8 81.94 9.83
0 -3 -8 74.44 4.55
0 -3 -8 75.63 4.52
0 3 -8 71.55 4.14
0 -3 -8 69.80 9.25
0 3 8 73.35 4.68
0 -3 8 73.76 8.95
0 3 -9 34.48 3.40
0 3 9 36.91 3.57
0 -3 -9 37.01 3.47
0 3 -9 37.81 3.54
0 -3 -9 36.38 3.42
0 3 -9 38.85 3.56
0 3 9 40.96 3.30
0 -3 -9 36.36 3.55
0 -3 -9 18.65 5.86
0 3 -9 38.54 3.39
0 -3 9 38.96 7.16
0 3 -10 46.92 3.88
0 -3 -10 52.61 4.20
0 3 10 48.30 4.19
0 -3 10 59.96 8.71
0 -3 -10 53.10 4.34
0 3 -10 47.83 3.87
0 -3 -10 47.60 8.95
0 3 -10 46.71 3.56
0 3 10 48.81 4.01
0 3 -10 49.43 3.99
0 3 -10 49.36 4.00
0 -3 -10 53.27 4.33
0 -3 -10 48.39 3.62
0 3 -11 144.69 6.13
0 -3 -11 141.80 6.93
0 3 -11 147.07 6.91
0 3 -11 142.82 6.50
0 3 -11 149.11 6.75
0 -3 -11 155.24 7.01
0 3 11 143.87 6.96
0 3 -11 152.37 6.78
0 -3 -11 145.92 15.11
0 3 -11 138.93 5.93
0 -3 -11 143.69 7.12
0 -3 11 157.09 14.75
0 -3 12 239.72 17.35
0 3 -12 230.02 8.41
0 3 12 213.18 8.65
0 -3 -12 223.17 8.96
0 3 -12 215.46 7.80
0 -3 -12 219.16 8.75
0 3 -12 217.60 8.55
0 3 -12 213.56 8.07
0 -3 -12 215.30 18.22
0 3 -12 218.12 7.83
0 -3 -12 218.28 8.91
0 3 -12 224.37 8.46
0 -3 -13 299.45 10.54
0 3 -13 283.12 9.15
0 3 -13 293.01 9.64
0 3 -13 276.40 9.18
0 -3 -13 287.22 10.14
0 3 -13 277.63 9.76
0 3 13 273.62 10.02
0 3 -13 276.10 9.05
0 3 -13 294.74 10.11
0 3 13 251.81 9.09
0 -3 -13 280.12 21.10
0 -3 -13 281.02 10.32
0 -3 13 295.78 20.86
0 -3 -14 4.29 4.80
0 3 14 5.29 1.86
0 3 -14 8.39 1.98
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7 2 2 5.58 1.98
-7 -2 -2 6.60 1.77
-7 2 -2 7.46 1.97
-7 -2 -2 5.70 2.26
-7 2 -2 2.09 0.68
-7 -2 -2 6.20 2.23
-7 -2 -2 3.55 0.93
7 2 2 5.61 1.48
-7 -2 -3 6.69 2.01
7 2 3 10.71 1.76
-7 -2 -3 10.41 2.25
-7 2 -3 10.43 2.15
-7 -2 -3 16.68 2.68
-7 -2 -3 12.27 2.43
-7 -2 -3 8.95 1.87
7 2 3 10.40 2.19
-7 -2 -4 0.28 0.98
7 2 4 1.76 1.73
-7 -2 -4 -1.36 1.12
-7 2 -4 0.02 1.48
-7 -2 -4 3.94 1.79
-7 -2 -4 2.53 1.50
-7 -2 -4 1.48 1.30
-7 -2 -5 -0.40 1.22
7 2 5 0.76 1.28
-7 -2 -5 -2.69 1.31
-7 2 -5 -0.52 1.44
-7 -2 -5 3.26 1.39
7 2 6 11.89 1.90
-7 -2 -6 9.48 1.54
-7 2 -6 13.83 2.08
7 3 -6 -0.37 1.53
7 3 -5 23.42 2.33
7 3 -5 19.95 2.49
-7 -3 5 25.32 2.47
7 3 -4 0.30 0.98
-7 -3 4 1.91 0.74
7 3 -4 -1.21 1.33
-7 -3 4 -1.61 1.06
-7 -3 3 13.37 2.08
7 3 -3 14.02 1.87
-7 -3 3 10.20 2.11
-7 -3 3 12.39 1.85
7 3 -3 13.97 2.30
-7 -3 2 5.90 1.46
7 3 -2 3.62 1.47
-7 -3 2 2.49 1.83
-7 -3 2 4.91 1.68
7 3 -2 4.32 2.03
7 3 -1 23.54 2.41
-7 -3 1 21.58 2.40
-7 -3 1 24.58 2.67
-7 -3 1 23.03 2.62
7 3 -1 22.29 2.47
-7 -3 0 9.10 1.76
7 3 0 9.59 1.82
-7 -3 0 7.07 1.80
-7 -3 0 6.09 1.86
7 3 0 6.52 1.73
7 3 1 13.01 2.08
-7 -3 -1 14.38 2.39
-7 -3 -1 12.61 2.16
0 0 0 0.00 0.00
TITL kji190001_fa in P2/n
REM P2/n (#13 in standard setting)
CELL 1.54184 6.547571 5.990979 21.567568 90.0000 96.0195 90.0000
ZERR 1.00 0.000172 0.000165 0.000570 0.0000 0.0025 0.0000
LATT 1
SYMM -x+1/2, y,-z+1/2
SFAC C H P Cl
UNIT 40.00 52.00 3.00 1.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 80973
_shelx_res_file
;
kji190001_fa.res created by SHELXL-2014/7
TITL kji190001_fa_a.res in P2/n
REM Old TITL kji190001_fa in P2/n
REM SHELXT solution in P2/n
REM R1 0.138, Rweak 0.339, Alpha 0.020, Orientation as input
REM Formula found by SHELXT: C20 Cl
CELL 1.54184 6.5476 5.991 21.5676 90 96.02 90
ZERR 2 0.0002 0.0002 0.0006 0 0.002 0
LATT 1
SYMM 0.5-X,+Y,0.5-Z
SFAC C H P
UNIT 40 54 2
L.S. 5
PLAN 20
SIZE 0.06 0.08 0.24
TEMP -123.1(2)
BOND $H
list 4
fmap 2
ACTA
REM
REM
REM
WGHT 0.066500 0.318900
FVAR 0.91688
P1 3 0.750000 0.700106 0.750000 10.50000 0.03992 0.03245 =
0.03623 0.00000 -0.00707 0.00000
H1 2 0.929813 0.759564 0.736196 10.50000 -1.50000
C1 1 0.668099 0.520588 0.682300 11.00000 0.02822 0.03378 =
0.02883 0.00407 -0.00023 -0.00221
C2 1 0.483715 0.580400 0.646062 11.00000 0.02878 0.03809 =
0.03245 0.00656 -0.00027 0.00104
C3 1 0.418218 0.454778 0.592716 11.00000 0.02762 0.04853 =
0.02944 0.00913 -0.00144 -0.00058
C4 1 0.536978 0.277171 0.577007 11.00000 0.03664 0.05090 =
0.02594 -0.00175 -0.00243 -0.00270
AFIX 43
H4 2 0.490386 0.191045 0.541318 11.00000 -1.20000
AFIX 0
C5 1 0.721364 0.218397 0.610900 11.00000 0.03348 0.04009 =
0.02946 0.00167 0.00112 0.00065
C6 1 0.790529 0.343901 0.664134 11.00000 0.02815 0.03553 =
0.02895 0.00557 0.00044 -0.00114
C7 1 0.356068 0.777248 0.662226 11.00000 0.03694 0.04856 =
0.05057 0.00031 -0.00626 0.01031
AFIX 137
H7A 2 0.253935 0.728138 0.689433 11.00000 -1.50000
H7B 2 0.285953 0.841254 0.623932 11.00000 -1.50000
H7C 2 0.445324 0.890336 0.683821 11.00000 -1.50000
AFIX 0
C8 1 0.221320 0.509471 0.552580 11.00000 0.03371 0.06826 =
0.03515 0.00753 -0.00695 0.00338
AFIX 137
H8A 2 0.105087 0.496533 0.577520 11.00000 -1.50000
H8B 2 0.202778 0.405061 0.517462 11.00000 -1.50000
H8C 2 0.228433 0.662281 0.536736 11.00000 -1.50000
AFIX 0
C9 1 0.842895 0.024862 0.589562 11.00000 0.04900 0.04837 =
0.03971 -0.00680 -0.00100 0.00830
AFIX 137
H9A 2 0.764894 -0.047715 0.553857 11.00000 -1.50000
H9B 2 0.868940 -0.082808 0.623683 11.00000 -1.50000
H9C 2 0.973966 0.079116 0.577255 11.00000 -1.50000
AFIX 0
C10 1 0.994057 0.285459 0.700032 11.00000 0.02981 0.04105 =
0.03395 0.00248 -0.00239 0.00299
AFIX 137
H10A 2 1.052013 0.418374 0.721761 11.00000 -1.50000
H10B 2 1.088812 0.231518 0.671084 11.00000 -1.50000
H10C 2 0.973396 0.168568 0.730543 11.00000 -1.50000
AFIX 0
HKLF 4
REM kji190001_fa_a.res in P2/n
REM R1 = 0.0393 for 1299 Fo > 4sig(Fo) and 0.0470 for all 1500 data
REM 103 parameters refined using 0 restraints
END
WGHT 0.0666 0.3182
REM Highest difference peak 0.272, deepest hole -0.236, 1-sigma level 0.044
Q1 1 0.3614 0.7944 0.7124 11.00000 0.05 0.27
Q2 1 0.1882 0.7353 0.6500 11.00000 0.05 0.27
Q3 1 0.7748 0.2903 0.6310 11.00000 0.05 0.22
Q4 1 0.4511 0.5092 0.6170 11.00000 0.05 0.21
Q5 1 0.6946 0.5787 0.7113 11.00000 0.05 0.21
Q6 1 0.7278 0.4213 0.6787 11.00000 0.05 0.20
Q7 1 0.5661 0.5327 0.6683 11.00000 0.05 0.20
Q8 1 0.4122 0.9273 0.6474 11.00000 0.05 0.18
Q9 1 0.8876 0.3173 0.6782 11.00000 0.05 0.18
Q10 1 0.3261 0.4953 0.5725 11.00000 0.05 0.18
Q11 1 0.7796 0.1322 0.6022 11.00000 0.05 0.16
Q12 1 1.0145 0.3074 0.7434 11.00000 0.05 0.15
Q13 1 0.6574 0.2513 0.5983 11.00000 0.05 0.15
Q14 1 1.0641 0.1369 0.6903 11.00000 0.05 0.15
Q15 1 1.0836 0.7160 0.7220 11.00000 0.05 0.14
Q16 1 0.8728 0.8879 0.7387 11.00000 0.05 0.13
Q17 1 0.4398 0.6635 0.6541 11.00000 0.05 0.12
Q18 1 0.8347 0.0100 0.5438 11.00000 0.05 0.12
Q19 1 1.1065 0.3402 0.6790 11.00000 0.05 0.11
Q20 1 0.2386 0.5119 0.5081 11.00000 0.05 0.10
;
_shelx_res_checksum 77999
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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 0.7500 0.70011(11) 0.7500 0.0370(2) Uani d 1 . .
H H1 0.930(8) 0.760(8) 0.736(2) 0.055 Uiso d 0.5 . .
C C1 0.6681(2) 0.5206(3) 0.68230(8) 0.0305(4) Uani d 1 . .
C C2 0.4837(3) 0.5804(3) 0.64606(8) 0.0334(4) Uani d 1 . .
C C3 0.4182(3) 0.4548(3) 0.59272(8) 0.0355(4) Uani d 1 . .
C C4 0.5370(3) 0.2772(3) 0.57701(8) 0.0382(4) Uani d 1 . .
H H4 0.4904 0.1910 0.5413 0.046 Uiso calc 1 . .
C C5 0.7214(3) 0.2184(3) 0.61090(8) 0.0345(4) Uani d 1 . .
C C6 0.7905(2) 0.3439(3) 0.66413(8) 0.0311(4) Uani d 1 . .
C C7 0.3561(3) 0.7772(4) 0.66223(10) 0.0461(5) Uani d 1 . .
H H7A 0.2539 0.7281 0.6894 0.069 Uiso calc 1 . .
H H7B 0.2860 0.8413 0.6239 0.069 Uiso calc 1 . .
H H7C 0.4453 0.8903 0.6838 0.069 Uiso calc 1 . .
C C8 0.2213(3) 0.5095(4) 0.55258(9) 0.0465(5) Uani d 1 . .
H H8A 0.1051 0.4965 0.5775 0.070 Uiso calc 1 . .
H H8B 0.2028 0.4051 0.5175 0.070 Uiso calc 1 . .
H H8C 0.2284 0.6623 0.5367 0.070 Uiso calc 1 . .
C C9 0.8429(3) 0.0249(4) 0.58956(9) 0.0461(5) Uani d 1 . .
H H9A 0.7649 -0.0477 0.5539 0.069 Uiso calc 1 . .
H H9B 0.8689 -0.0828 0.6237 0.069 Uiso calc 1 . .
H H9C 0.9740 0.0791 0.5773 0.069 Uiso calc 1 . .
C C10 0.9941(3) 0.2855(3) 0.70003(8) 0.0353(4) Uani d 1 . .
H H10A 1.0520 0.4184 0.7218 0.053 Uiso calc 1 . .
H H10B 1.0888 0.2315 0.6711 0.053 Uiso calc 1 . .
H H10C 0.9734 0.1686 0.7305 0.053 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
P1 0.0399(4) 0.0324(4) 0.0362(4) 0.000 -0.0071(3) 0.000
C1 0.0282(8) 0.0338(9) 0.0288(8) -0.0022(7) -0.0002(6) 0.0041(7)
C2 0.0288(8) 0.0381(9) 0.0324(9) 0.0010(7) -0.0003(7) 0.0066(7)
C3 0.0276(8) 0.0485(11) 0.0294(9) -0.0006(8) -0.0014(7) 0.0091(8)
C4 0.0366(9) 0.0509(11) 0.0259(8) -0.0027(8) -0.0024(7) -0.0018(8)
C5 0.0335(9) 0.0401(10) 0.0295(8) 0.0007(7) 0.0011(7) 0.0017(7)
C6 0.0282(8) 0.0355(9) 0.0290(8) -0.0011(7) 0.0004(7) 0.0056(7)
C7 0.0369(10) 0.0486(11) 0.0506(11) 0.0103(9) -0.0063(8) 0.0003(9)
C8 0.0337(9) 0.0683(14) 0.0351(10) 0.0034(9) -0.0070(8) 0.0075(9)
C9 0.0490(11) 0.0484(11) 0.0397(10) 0.0083(9) -0.0010(8) -0.0068(9)
C10 0.0298(9) 0.0410(10) 0.0340(9) 0.0030(7) -0.0024(7) 0.0025(8)
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 -1 1 0.0352
1 1 -1 0.0252
1 -1 -1 0.0344
-1 1 1 0.0414
0 0 1 0.1076
0 0 -1 0.1046
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 H1 2_656 . 98(2) ?
C1 P1 H1 . . 100(2) ?
C1 P1 C1 . 2_656 108.78(11) ?
C2 C1 P1 . . 116.72(13) ?
C6 C1 P1 . . 122.08(12) ?
C6 C1 C2 . . 120.98(16) ?
C1 C2 C7 . . 122.17(16) ?
C3 C2 C1 . . 119.14(16) ?
C3 C2 C7 . . 118.68(15) ?
C2 C3 C8 . . 121.47(17) ?
C4 C3 C2 . . 118.86(15) ?
C4 C3 C8 . . 119.67(17) ?
C3 C4 H4 . . 118.4 ?
C3 C4 C5 . . 123.14(17) ?
C5 C4 H4 . . 118.4 ?
C4 C5 C6 . . 118.78(17) ?
C4 C5 C9 . . 119.49(17) ?
C6 C5 C9 . . 121.73(16) ?
C1 C6 C10 . . 121.94(15) ?
C5 C6 C1 . . 119.01(15) ?
C5 C6 C10 . . 119.05(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 ?
C6 C10 H10A . . 109.5 ?
C6 C10 H10B . . 109.5 ?
C6 C10 H10C . . 109.5 ?
H10A C10 H10B . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 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 H1 . 1.29(5) ?
P1 C1 2_656 1.8472(17) ?
P1 C1 . 1.8471(17) ?
C1 C2 . 1.414(2) ?
C1 C6 . 1.408(2) ?
C2 C3 . 1.404(3) ?
C2 C7 . 1.507(3) ?
C3 C4 . 1.381(3) ?
C3 C8 . 1.512(2) ?
C4 H4 . 0.9500 ?
C4 C5 . 1.390(3) ?
C5 C6 . 1.407(3) ?
C5 C9 . 1.505(3) ?
C6 C10 . 1.510(2) ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C8 H8A . 0.9800 ?
C8 H8B . 0.9800 ?
C8 H8C . 0.9800 ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
C9 H9C . 0.9800 ?
C10 H10A . 0.9800 ?
C10 H10B . 0.9800 ?
C10 H10C . 0.9800 ?