# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_khor3cult
_database_code_depnum_ccdc_archive 'CCDC 1917740'
loop_
_audit_author_name
_audit_author_address
'Michidmaa Khorloo'
;Hong Kong University of Science and Technology
Hong Kong
;
_audit_update_record
;
2019-05-22 deposited with the CCDC. 2019-12-11 downloaded from the CCDC.
;
_audit_creation_date 2018-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common TPE-Py
_chemical_name_systematic TPE-EP-G
_chemical_formula_moiety 'C H2 Cl2, 2(F6 P), 2(C34 H28 N)'
_chemical_formula_sum 'C69 H58 Cl2 F12 N2 P2'
_chemical_formula_weight 1276.01
_chemical_melting_point ?
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 11.2525(2)
_cell_length_b 9.21940(13)
_cell_length_c 59.1397(9)
_cell_angle_alpha 90
_cell_angle_beta 93.8053(14)
_cell_angle_gamma 90
_cell_volume 6121.68(17)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 11185
_cell_measurement_temperature 100.03(11)
_cell_measurement_theta_max 73.0670
_cell_measurement_theta_min 4.0480
_shelx_estimated_absorpt_T_max 0.958
_shelx_estimated_absorpt_T_min 0.674
_exptl_absorpt_coefficient_mu 2.143
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.72507
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.384
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 2632
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.02
_exptl_crystal_size_min 0.02
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0416
_diffrn_reflns_av_unetI/netI 0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 70
_diffrn_reflns_limit_l_min -35
_diffrn_reflns_number 32777
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full 66.500
_diffrn_reflns_theta_max 67.498
_diffrn_reflns_theta_min 3.959
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.03(11)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w 29.00 105.50 0.75 25.00 -- 106.99 -77.00 -90.00 102
2 \w -117.00 -15.00 0.75 10.00 -- -40.57 -37.00 0.00 136
3 \w -69.00 32.25 0.75 10.00 -- -40.57 57.00 150.00 135
4 \w -92.00 -2.00 0.75 10.00 -- -40.57 125.00-150.00 120
5 \w 65.00 116.00 0.75 25.00 -- 106.99-125.00 -90.00 68
6 \w 38.00 115.25 0.75 25.00 -- 106.99-125.00 60.00 103
7 \w 46.00 164.50 0.75 25.00 -- 106.99 15.00 30.00 158
8 \w 33.00 134.25 0.75 25.00 -- 106.99 -45.00 0.00 135
9 \w 32.00 116.00 0.75 25.00 -- 106.99-125.00-180.00 112
10 \w 32.00 130.25 0.75 25.00 -- 106.99 -45.00 120.00 131
11 \w 109.00 178.00 0.75 25.00 -- 106.99 45.00 60.00 92
;
_diffrn_measurement_device 'kappa diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.1136970000
_diffrn_orient_matrix_UB_12 0.0206380000
_diffrn_orient_matrix_UB_13 -0.0156822000
_diffrn_orient_matrix_UB_21 0.0009888000
_diffrn_orient_matrix_UB_22 -0.1626067000
_diffrn_orient_matrix_UB_23 -0.0059458000
_diffrn_orient_matrix_UB_31 -0.0768846000
_diffrn_orient_matrix_UB_32 -0.0322975000
_diffrn_orient_matrix_UB_33 0.0200047000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_current 0.80
_diffrn_source_power 0.040
_diffrn_source_target Cu
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage 50
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 9143
_reflns_number_total 10976
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.949
_refine_diff_density_min -0.711
_refine_diff_density_rms 0.061
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 849
_refine_ls_number_reflns 10976
_refine_ls_number_restraints 86
_refine_ls_R_factor_all 0.0744
_refine_ls_R_factor_gt 0.0623
_refine_ls_restrained_S_all 1.034
_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^)+(0.0660P)^2^+8.2250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1501
_refine_ls_wR_factor_ref 0.1577
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
C3B-C2B \\sim C4B-C3B \\sim C5B-C4B \\sim C6B-C5B
with sigma of 0.02
C3A-C2A \\sim C4A-C3A \\sim C5A-C4A \\sim C6A-C5A
with sigma of 0.02
N1A-C2B \\sim N1A-C6B
with sigma of 0.02
N1A-C6A \\sim N1A-C2A
with sigma of 0.02
3. Rigid body (RIGU) restrains
N1A, C2B, C3B, C4B, C5B, C6B
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
N1A, C2A, C3A, C4A, C5A, C6A
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
Fixed Sof: C2A(0.75) H2A(0.75) C2B(0.25) H2B(0.25) C3A(0.75) H3A(0.75)
C3B(0.25) H3B(0.25) C4A(0.75) C4B(0.25) C5A(0.75) H5A(0.75) C5B(0.25)
H5B(0.25) C6A(0.75) H6A(0.75) C6B(0.25) H6B(0.25) C7A(0.75) H7A(0.75)
C7B(0.25) H7B(0.25) C8A(0.75) H8A(0.75) C8B(0.25) H8B(0.25)
5.a Secondary CH2 refined with riding coordinates:
C1S(H1SA,H1SB)
5.b Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C15(H15),
C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33),
C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45),
C46(H46), C2A(H2A), C2B(H2B), C3A(H3A), C3B(H3B), C5A(H5A), C5B(H5B), C6A(H6A),
C6B(H6B), C7A(H7A), C7B(H7B), C8A(H8A), C8B(H8B), C12A(H12A), C13A(H13A),
C15A(H15A), C16A(H16A), C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A),
C26A(H26A), C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A),
C42A(H42A), C43A(H43A), C44A(H44A), C45A(H45A), C46A(H46A)
5.c Idealised Me refined as rotating group:
C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.88412(10) 0.42676(10) 0.15237(2) 0.0542(2) Uani 1 1 d . . . . .
Cl2 Cl 0.80461(9) 0.13577(11) 0.16170(2) 0.0553(3) Uani 1 1 d . . . . .
C1S C 0.9271(3) 0.2555(4) 0.16402(6) 0.0422(8) Uani 1 1 d . . . . .
H1SA H 0.9935 0.2151 0.1558 0.051 Uiso 1 1 calc R . . . .
H1SB H 0.9549 0.2671 0.1801 0.051 Uiso 1 1 calc R . . . .
P1 P 0.18654(7) 0.97003(9) 0.19499(2) 0.02918(18) Uani 1 1 d . . . . .
F1 F 0.12725(19) 0.9487(2) 0.21863(3) 0.0495(5) Uani 1 1 d . . . . .
F2 F 0.24704(19) 0.9915(2) 0.17167(3) 0.0491(5) Uani 1 1 d . . . . .
F3 F 0.1559(3) 1.1374(3) 0.19555(4) 0.0766(8) Uani 1 1 d . . . . .
F4 F 0.3079(2) 1.0017(4) 0.20871(4) 0.0807(9) Uani 1 1 d . . . . .
F5 F 0.2185(4) 0.8042(3) 0.19468(4) 0.0922(11) Uani 1 1 d . . . . .
F6 F 0.0648(2) 0.9419(4) 0.18131(5) 0.0958(12) Uani 1 1 d . . . . .
P1A P 0.90751(8) 0.46478(10) 0.22744(2) 0.0401(2) Uani 1 1 d . . . . .
F1A F 0.8466(2) 0.3652(2) 0.24553(3) 0.0481(5) Uani 1 1 d . . . . .
F2A F 0.9705(2) 0.5637(3) 0.20964(4) 0.0690(7) Uani 1 1 d . . . . .
F3A F 0.8336(3) 0.6008(3) 0.23553(5) 0.0776(9) Uani 1 1 d . . . . .
F4A F 1.0111(3) 0.5019(3) 0.24627(5) 0.0770(8) Uani 1 1 d . . . . .
F5A F 0.9841(2) 0.3310(3) 0.21972(4) 0.0552(6) Uani 1 1 d . . . . .
F6A F 0.8054(2) 0.4272(4) 0.20890(4) 0.0744(8) Uani 1 1 d . . . . .
N1 N 0.7755(2) 0.9436(3) 0.21073(4) 0.0296(5) Uani 1 1 d . . . . .
C1 C 0.8545(3) 1.0139(4) 0.22842(6) 0.0429(8) Uani 1 1 d . . . . .
H1A H 0.8133 1.0968 0.2347 0.064 Uiso 1 1 calc GR . . . .
H1B H 0.9271 1.0476 0.2218 0.064 Uiso 1 1 calc GR . . . .
H1C H 0.8755 0.9440 0.2405 0.064 Uiso 1 1 calc GR . . . .
C2 C 0.8206(3) 0.8385(3) 0.19804(5) 0.0313(6) Uani 1 1 d . . . . .
H2 H 0.9015 0.8103 0.2007 0.038 Uiso 1 1 calc R . . . .
C3 C 0.7502(3) 0.7718(3) 0.18125(5) 0.0318(6) Uani 1 1 d . . . . .
H3 H 0.7830 0.6977 0.1724 0.038 Uiso 1 1 calc R . . . .
C4 C 0.6308(3) 0.8118(3) 0.17706(5) 0.0255(6) Uani 1 1 d . . . . .
C5 C 0.5872(3) 0.9209(3) 0.19079(5) 0.0289(6) Uani 1 1 d . . . . .
H5 H 0.5064 0.9507 0.1886 0.035 Uiso 1 1 calc R . . . .
C6 C 0.6609(3) 0.9847(4) 0.20730(5) 0.0325(7) Uani 1 1 d . . . . .
H6 H 0.6306 1.0590 0.2165 0.039 Uiso 1 1 calc R . . . .
C7 C 0.5575(3) 0.7391(3) 0.15927(5) 0.0271(6) Uani 1 1 d . . . . .
H7 H 0.5971 0.6894 0.1479 0.032 Uiso 1 1 calc R . . . .
C8 C 0.4391(3) 0.7375(3) 0.15783(5) 0.0252(6) Uani 1 1 d . . . . .
H8 H 0.4001 0.7872 0.1693 0.030 Uiso 1 1 calc R . . . .
C10 C 0.1367(3) 0.4462(3) 0.08951(5) 0.0257(6) Uani 1 1 d . . . . .
C11 C 0.2151(3) 0.5258(3) 0.10673(5) 0.0255(6) Uani 1 1 d . . . . .
C12 C 0.1715(3) 0.5687(3) 0.12722(5) 0.0303(6) Uani 1 1 d . . . . .
H12 H 0.0911 0.5486 0.1301 0.036 Uiso 1 1 calc R . . . .
C13 C 0.2442(3) 0.6403(3) 0.14345(5) 0.0285(6) Uani 1 1 d . . . . .
H13 H 0.2121 0.6724 0.1570 0.034 Uiso 1 1 calc R . . . .
C14 C 0.3637(3) 0.6658(3) 0.14007(4) 0.0246(6) Uani 1 1 d . . . . .
C15 C 0.4078(3) 0.6216(3) 0.11954(5) 0.0259(6) Uani 1 1 d . . . . .
H15 H 0.4890 0.6385 0.1169 0.031 Uiso 1 1 calc R . . . .
C16 C 0.3345(3) 0.5541(3) 0.10319(5) 0.0269(6) Uani 1 1 d . . . . .
H16 H 0.3656 0.5263 0.0893 0.032 Uiso 1 1 calc R . . . .
C20 C 0.1166(3) 0.4946(3) 0.06796(5) 0.0261(6) Uani 1 1 d . . . . .
C21 C 0.1589(3) 0.6403(3) 0.06061(5) 0.0280(6) Uani 1 1 d . . . . .
C22 C 0.1445(3) 0.7646(3) 0.07341(5) 0.0361(7) Uani 1 1 d . . . . .
H22 H 0.1026 0.7593 0.0868 0.043 Uiso 1 1 calc R . . . .
C23 C 0.1906(4) 0.8966(4) 0.06683(6) 0.0450(8) Uani 1 1 d . . . . .
H23 H 0.1810 0.9805 0.0759 0.054 Uiso 1 1 calc R . . . .
C24 C 0.2504(3) 0.9066(4) 0.04715(6) 0.0415(8) Uani 1 1 d . . . . .
H24 H 0.2832 0.9965 0.0428 0.050 Uiso 1 1 calc R . . . .
C25 C 0.2620(3) 0.7843(3) 0.03387(5) 0.0328(7) Uani 1 1 d . . . . .
H25 H 0.3018 0.7905 0.0202 0.039 Uiso 1 1 calc R . . . .
C26 C 0.2157(3) 0.6532(3) 0.04045(5) 0.0279(6) Uani 1 1 d . . . . .
H26 H 0.2226 0.5704 0.0311 0.033 Uiso 1 1 calc R . . . .
C31 C 0.0875(3) 0.3079(3) 0.09797(4) 0.0253(6) Uani 1 1 d . . . . .
C32 C 0.1612(3) 0.2175(3) 0.11186(5) 0.0307(6) Uani 1 1 d . . . . .
H32 H 0.2407 0.2466 0.1160 0.037 Uiso 1 1 calc R . . . .
C33 C 0.1191(3) 0.0857(4) 0.11959(5) 0.0364(7) Uani 1 1 d . . . . .
H33 H 0.1704 0.0243 0.1287 0.044 Uiso 1 1 calc R . . . .
C34 C 0.0020(3) 0.0437(4) 0.11402(5) 0.0353(7) Uani 1 1 d . . . . .
H34 H -0.0270 -0.0460 0.1193 0.042 Uiso 1 1 calc R . . . .
C35 C -0.0716(3) 0.1340(3) 0.10071(5) 0.0322(7) Uani 1 1 d . . . . .
H35 H -0.1518 0.1063 0.0970 0.039 Uiso 1 1 calc R . . . .
C36 C -0.0296(3) 0.2643(3) 0.09276(5) 0.0273(6) Uani 1 1 d . . . . .
H36 H -0.0815 0.3249 0.0836 0.033 Uiso 1 1 calc R . . . .
C41 C 0.0555(3) 0.4036(3) 0.04976(5) 0.0259(6) Uani 1 1 d . . . . .
C42 C 0.0872(3) 0.2595(3) 0.04671(5) 0.0279(6) Uani 1 1 d . . . . .
H42 H 0.1497 0.2185 0.0562 0.033 Uiso 1 1 calc R . . . .
C43 C 0.0294(3) 0.1746(4) 0.03010(5) 0.0326(7) Uani 1 1 d . . . . .
H43 H 0.0510 0.0757 0.0285 0.039 Uiso 1 1 calc R . . . .
C44 C -0.0597(3) 0.2340(4) 0.01579(5) 0.0367(7) Uani 1 1 d . . . . .
H44 H -0.1004 0.1761 0.0045 0.044 Uiso 1 1 calc R . . . .
C45 C -0.0892(3) 0.3782(4) 0.01811(5) 0.0379(8) Uani 1 1 d . . . . .
H45 H -0.1487 0.4202 0.0080 0.046 Uiso 1 1 calc R . . . .
C46 C -0.0330(3) 0.4627(4) 0.03499(5) 0.0336(7) Uani 1 1 d . . . . .
H46 H -0.0549 0.5616 0.0365 0.040 Uiso 1 1 calc R . . . .
N1A N 0.3419(2) 0.6037(3) 0.22853(4) 0.0282(5) Uani 1 1 d D U . . .
C1A C 0.2918(4) 0.6953(4) 0.24606(5) 0.0448(9) Uani 1 1 d . . . . .
H1AA H 0.3498 0.7037 0.2591 0.067 Uiso 1 1 calc GR . . . .
H1AB H 0.2185 0.6509 0.2509 0.067 Uiso 1 1 calc GR . . . .
H1AC H 0.2740 0.7919 0.2398 0.067 Uiso 1 1 calc GR . . . .
C2A C 0.4576(5) 0.6164(6) 0.22550(10) 0.0259(11) Uani 0.75 1 d D U P A 1
H2A H 0.5052 0.6795 0.2350 0.031 Uiso 0.75 1 calc R . P A 1
C2B C 0.4580(16) 0.591(3) 0.2213(4) 0.035(4) Uani 0.25 1 d D U P A 2
H2B H 0.5203 0.6483 0.2283 0.042 Uiso 0.25 1 calc R . P A 2
C3A C 0.5091(4) 0.5397(5) 0.20880(8) 0.0252(9) Uani 0.75 1 d D U P A 1
H3A H 0.5923 0.5479 0.2072 0.030 Uiso 0.75 1 calc R . P A 1
C3B C 0.4821(15) 0.4973(17) 0.2042(3) 0.035(3) Uani 0.25 1 d D U P A 2
H3B H 0.5605 0.4893 0.1993 0.041 Uiso 0.25 1 calc R . P A 2
C4A C 0.4403(4) 0.4498(5) 0.19410(7) 0.0232(8) Uani 0.75 1 d D U P A 1
C4B C 0.3914(15) 0.4152(17) 0.1943(2) 0.031(3) Uani 0.25 1 d D U P A 2
C5A C 0.3191(5) 0.4386(5) 0.19787(9) 0.0306(10) Uani 0.75 1 d D U P A 1
H5A H 0.2688 0.3779 0.1884 0.037 Uiso 0.75 1 calc R . P A 1
C5B C 0.2813(14) 0.4249(18) 0.2028(3) 0.034(3) Uani 0.25 1 d D U P A 2
H5B H 0.2203 0.3621 0.1967 0.040 Uiso 0.25 1 calc R . P A 2
C6A C 0.2725(5) 0.5147(8) 0.21512(12) 0.0303(13) Uani 0.75 1 d D U P A 1
H6A H 0.1905 0.5048 0.2177 0.036 Uiso 0.75 1 calc R . P A 1
C6B C 0.2545(18) 0.519(3) 0.2192(4) 0.036(4) Uani 0.25 1 d D U P A 2
H6B H 0.1759 0.5245 0.2241 0.043 Uiso 0.25 1 calc R . P A 2
C7A C 0.4933(3) 0.3787(4) 0.17497(8) 0.0244(8) Uani 0.75 1 d . . P A 1
H7A H 0.5730 0.4029 0.1722 0.029 Uiso 0.75 1 calc R . P A 1
C7B C 0.4091(13) 0.3178(15) 0.1750(3) 0.038(3) Uani 0.25 1 d . . P A 2
H7B H 0.3565 0.2379 0.1725 0.045 Uiso 0.25 1 calc R . P A 2
C8A C 0.4371(5) 0.2824(5) 0.16121(8) 0.0242(8) Uani 0.75 1 d . . P A 1
H8A H 0.3599 0.2516 0.1648 0.029 Uiso 0.75 1 calc R . P A 1
C8B C 0.4950(14) 0.3366(17) 0.1609(2) 0.031(3) Uani 0.25 1 d . . P A 2
H8B H 0.5541 0.4101 0.1626 0.037 Uiso 0.25 1 calc R . P A 2
C10A C 0.6076(3) -0.0058(3) 0.08284(5) 0.0261(6) Uani 1 1 d . . . . .
C11A C 0.5629(2) 0.0798(3) 0.10200(5) 0.0235(6) Uani 1 1 d . . . . .
C12A C 0.6068(3) 0.2165(3) 0.10811(5) 0.0279(6) Uani 1 1 d . . . . .
H12A H 0.6622 0.2630 0.0991 0.033 Uiso 1 1 calc R . . . .
C13A C 0.5701(3) 0.2857(3) 0.12738(6) 0.0363(7) Uani 1 1 d . . . . .
H13A H 0.6017 0.3783 0.1315 0.044 Uiso 1 1 calc R . . . .
C14A C 0.4870(3) 0.2204(4) 0.14081(5) 0.0373(8) Uani 1 1 d . . . . .
C15A C 0.4418(3) 0.0864(3) 0.13425(5) 0.0357(7) Uani 1 1 d . . . . .
H15A H 0.3837 0.0417 0.1429 0.043 Uiso 1 1 calc R . . . .
C16A C 0.4794(3) 0.0161(3) 0.11538(5) 0.0299(6) Uani 1 1 d . . . . .
H16A H 0.4481 -0.0768 0.1114 0.036 Uiso 1 1 calc R . . . .
C20A C 0.6124(2) 0.0429(3) 0.06149(5) 0.0255(6) Uani 1 1 d . . . . .
C21A C 0.5642(3) 0.1857(3) 0.05346(5) 0.0266(6) Uani 1 1 d . . . . .
C22A C 0.4526(3) 0.2364(3) 0.05852(4) 0.0246(6) Uani 1 1 d . . . . .
H22A H 0.4054 0.1815 0.0681 0.029 Uiso 1 1 calc R . . . .
C23A C 0.4101(3) 0.3665(3) 0.04956(5) 0.0284(6) Uani 1 1 d . . . . .
H23A H 0.3334 0.3996 0.0530 0.034 Uiso 1 1 calc R . . . .
C24A C 0.4776(3) 0.4492(3) 0.03567(5) 0.0322(7) Uani 1 1 d . . . . .
H24A H 0.4476 0.5384 0.0296 0.039 Uiso 1 1 calc R . . . .
C25A C 0.5890(3) 0.4010(4) 0.03069(5) 0.0357(7) Uani 1 1 d . . . . .
H25A H 0.6364 0.4579 0.0214 0.043 Uiso 1 1 calc R . . . .
C26A C 0.6315(3) 0.2702(3) 0.03921(5) 0.0322(7) Uani 1 1 d . . . . .
H26A H 0.7074 0.2367 0.0354 0.039 Uiso 1 1 calc R . . . .
C31A C 0.6541(3) -0.1539(3) 0.08967(5) 0.0260(6) Uani 1 1 d . . . . .
C32A C 0.6224(3) -0.2790(3) 0.07734(5) 0.0311(6) Uani 1 1 d . . . . .
H32A H 0.5667 -0.2731 0.0646 0.037 Uiso 1 1 calc R . . . .
C33A C 0.6722(3) -0.4115(3) 0.08369(5) 0.0367(7) Uani 1 1 d . . . . .
H33A H 0.6498 -0.4961 0.0753 0.044 Uiso 1 1 calc R . . . .
C34A C 0.7533(3) -0.4220(3) 0.10196(6) 0.0354(7) Uani 1 1 d . . . . .
H34A H 0.7894 -0.5127 0.1058 0.042 Uiso 1 1 calc R . . . .
C35A C 0.7829(3) -0.2979(3) 0.11499(5) 0.0321(7) Uani 1 1 d . . . . .
H35A H 0.8378 -0.3046 0.1279 0.039 Uiso 1 1 calc R . . . .
C36A C 0.7316(3) -0.1664(3) 0.10897(5) 0.0265(6) Uani 1 1 d . . . . .
H36A H 0.7494 -0.0834 0.1181 0.032 Uiso 1 1 calc R . . . .
C41A C 0.6681(3) -0.0448(3) 0.04355(5) 0.0287(6) Uani 1 1 d . . . . .
C42A C 0.7880(3) -0.0826(3) 0.04512(5) 0.0320(7) Uani 1 1 d . . . . .
H42A H 0.8375 -0.0540 0.0580 0.038 Uiso 1 1 calc R . . . .
C43A C 0.8353(3) -0.1619(4) 0.02796(6) 0.0398(8) Uani 1 1 d . . . . .
H43A H 0.9177 -0.1849 0.0289 0.048 Uiso 1 1 calc R . . . .
C44A C 0.7635(3) -0.2073(4) 0.00962(6) 0.0421(8) Uani 1 1 d . . . . .
H44A H 0.7958 -0.2649 -0.0018 0.051 Uiso 1 1 calc R . . . .
C45A C 0.6450(4) -0.1697(4) 0.00774(5) 0.0402(8) Uani 1 1 d . . . . .
H45A H 0.5958 -0.2009 -0.0050 0.048 Uiso 1 1 calc R . . . .
C46A C 0.5972(3) -0.0863(4) 0.02437(5) 0.0347(7) Uani 1 1 d . . . . .
H46A H 0.5160 -0.0573 0.0227 0.042 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0716(6) 0.0438(5) 0.0489(5) 0.0085(4) 0.0174(4) 0.0016(4)
Cl2 0.0561(6) 0.0607(6) 0.0486(5) 0.0176(4) -0.0017(4) -0.0107(5)
C1S 0.0409(19) 0.044(2) 0.0417(19) 0.0016(15) 0.0055(15) 0.0046(15)
P1 0.0299(4) 0.0323(4) 0.0263(4) 0.0035(3) 0.0089(3) 0.0025(3)
F1 0.0560(13) 0.0562(13) 0.0394(11) 0.0087(9) 0.0267(9) 0.0074(10)
F2 0.0588(13) 0.0582(13) 0.0325(10) 0.0154(9) 0.0199(9) 0.0139(10)
F3 0.123(2) 0.0450(14) 0.0652(16) 0.0093(11) 0.0319(16) 0.0223(14)
F4 0.0421(13) 0.149(3) 0.0506(14) 0.0133(16) -0.0002(11) -0.0111(15)
F5 0.200(4) 0.0401(13) 0.0411(13) 0.0098(10) 0.0457(17) 0.0298(17)
F6 0.0572(16) 0.164(3) 0.0641(16) 0.0285(19) -0.0102(13) -0.0506(19)
P1A 0.0400(5) 0.0437(5) 0.0381(5) 0.0057(4) 0.0134(4) 0.0077(4)
F1A 0.0610(13) 0.0436(11) 0.0416(11) 0.0046(9) 0.0172(9) 0.0018(10)
F2A 0.0656(15) 0.0690(16) 0.0773(17) 0.0278(13) 0.0429(13) 0.0178(13)
F3A 0.097(2) 0.0473(13) 0.096(2) 0.0219(13) 0.0633(17) 0.0250(13)
F4A 0.0708(17) 0.093(2) 0.0675(16) -0.0161(15) 0.0022(13) -0.0212(15)
F5A 0.0548(13) 0.0552(13) 0.0571(13) 0.0015(10) 0.0152(10) 0.0186(11)
F6A 0.0426(13) 0.133(3) 0.0479(13) 0.0091(14) 0.0031(10) 0.0105(15)
N1 0.0258(13) 0.0381(14) 0.0254(12) -0.0034(10) 0.0054(10) -0.0062(11)
C1 0.0323(17) 0.057(2) 0.0389(18) -0.0159(16) 0.0007(14) -0.0130(16)
C2 0.0249(15) 0.0391(17) 0.0301(15) 0.0000(13) 0.0042(12) -0.0021(13)
C3 0.0317(16) 0.0324(16) 0.0317(15) -0.0035(12) 0.0059(12) 0.0013(13)
C4 0.0289(15) 0.0265(14) 0.0217(13) 0.0008(11) 0.0054(11) -0.0049(12)
C5 0.0260(14) 0.0325(16) 0.0283(15) -0.0033(12) 0.0032(11) -0.0019(12)
C6 0.0331(16) 0.0369(17) 0.0281(15) -0.0063(12) 0.0071(12) -0.0026(13)
C7 0.0327(16) 0.0274(15) 0.0217(13) -0.0017(11) 0.0054(11) -0.0002(12)
C8 0.0320(15) 0.0229(14) 0.0209(13) -0.0008(10) 0.0040(11) -0.0015(11)
C10 0.0267(14) 0.0266(14) 0.0241(14) -0.0027(11) 0.0040(11) 0.0006(11)
C11 0.0298(15) 0.0240(14) 0.0226(13) 0.0005(11) 0.0018(11) -0.0007(11)
C12 0.0296(15) 0.0342(16) 0.0275(15) -0.0033(12) 0.0049(12) -0.0050(12)
C13 0.0321(15) 0.0332(16) 0.0207(13) -0.0026(11) 0.0071(11) -0.0030(12)
C14 0.0325(15) 0.0220(13) 0.0194(13) -0.0004(10) 0.0029(11) -0.0001(11)
C15 0.0297(15) 0.0241(14) 0.0242(14) 0.0002(11) 0.0042(11) -0.0010(11)
C16 0.0353(16) 0.0271(14) 0.0185(13) -0.0019(11) 0.0045(11) 0.0022(12)
C20 0.0275(14) 0.0246(14) 0.0263(14) -0.0004(11) 0.0029(11) 0.0024(11)
C21 0.0298(15) 0.0276(15) 0.0262(14) 0.0018(11) -0.0017(11) 0.0010(12)
C22 0.052(2) 0.0279(16) 0.0287(16) 0.0012(12) 0.0063(14) 0.0048(14)
C23 0.068(2) 0.0269(17) 0.0403(19) -0.0048(14) 0.0024(17) 0.0016(16)
C24 0.053(2) 0.0291(17) 0.0420(19) 0.0051(14) -0.0003(15) -0.0058(15)
C25 0.0337(16) 0.0338(16) 0.0306(15) 0.0052(12) -0.0001(12) -0.0010(13)
C26 0.0292(15) 0.0280(15) 0.0258(14) 0.0012(11) -0.0035(11) 0.0015(12)
C31 0.0294(15) 0.0286(15) 0.0181(13) -0.0020(11) 0.0043(11) 0.0007(12)
C32 0.0324(16) 0.0317(16) 0.0277(15) -0.0004(12) -0.0005(12) -0.0029(13)
C33 0.0456(19) 0.0331(17) 0.0301(16) 0.0060(13) -0.0007(13) 0.0029(14)
C34 0.0406(18) 0.0328(17) 0.0331(16) 0.0031(13) 0.0076(13) -0.0082(14)
C35 0.0306(16) 0.0383(17) 0.0287(15) 0.0002(12) 0.0079(12) -0.0048(13)
C36 0.0279(15) 0.0314(15) 0.0231(14) -0.0017(11) 0.0052(11) 0.0028(12)
C41 0.0255(14) 0.0302(15) 0.0221(13) 0.0025(11) 0.0034(11) -0.0036(12)
C42 0.0286(15) 0.0332(16) 0.0221(13) 0.0007(11) 0.0044(11) -0.0027(12)
C43 0.0314(16) 0.0395(17) 0.0278(15) -0.0084(13) 0.0094(12) -0.0080(13)
C44 0.0331(17) 0.053(2) 0.0246(15) -0.0066(13) 0.0058(12) -0.0148(15)
C45 0.0295(16) 0.057(2) 0.0265(15) 0.0092(14) -0.0014(12) -0.0077(15)
C46 0.0301(16) 0.0388(17) 0.0316(16) 0.0074(13) -0.0004(12) -0.0027(13)
N1A 0.0354(10) 0.0266(11) 0.0227(10) 0.0014(8) 0.0023(8) 0.0007(8)
C1A 0.070(2) 0.0425(19) 0.0232(15) -0.0058(13) 0.0102(15) 0.0128(18)
C2A 0.0345(13) 0.021(2) 0.022(2) 0.0007(17) 0.0010(12) 0.0002(12)
C2B 0.036(2) 0.036(7) 0.033(7) -0.008(6) 0.005(3) -0.003(2)
C3A 0.0297(16) 0.022(2) 0.0237(18) -0.0002(14) 0.0009(12) -0.0024(13)
C3B 0.036(4) 0.035(6) 0.033(6) -0.008(4) 0.007(4) -0.005(3)
C4A 0.0272(18) 0.0209(19) 0.0216(16) 0.0005(14) 0.0030(14) -0.0021(14)
C4B 0.036(4) 0.031(5) 0.027(4) -0.003(4) 0.006(4) -0.004(4)
C5A 0.0287(19) 0.034(2) 0.030(2) -0.0079(16) 0.0053(14) -0.0043(15)
C5B 0.037(4) 0.034(5) 0.031(5) -0.006(4) 0.008(3) -0.005(4)
C6A 0.0312(18) 0.032(2) 0.028(2) -0.0040(18) 0.0065(14) -0.0019(15)
C6B 0.037(2) 0.038(6) 0.032(7) -0.008(6) 0.006(3) -0.004(3)
C7A 0.025(2) 0.0237(19) 0.025(2) -0.0024(17) 0.0038(16) -0.0021(17)
C7B 0.039(8) 0.032(7) 0.042(8) -0.005(6) 0.004(6) -0.005(6)
C8A 0.027(2) 0.020(2) 0.027(2) -0.0026(17) 0.0028(18) 0.004(2)
C8B 0.032(8) 0.033(7) 0.028(8) -0.002(6) -0.001(6) -0.020(6)
C10A 0.0249(14) 0.0285(15) 0.0252(14) -0.0032(11) 0.0045(11) -0.0046(11)
C11A 0.0242(14) 0.0230(14) 0.0231(13) 0.0008(10) -0.0003(10) 0.0033(11)
C12A 0.0272(15) 0.0257(15) 0.0303(15) 0.0001(11) -0.0013(11) 0.0018(12)
C13A 0.0405(18) 0.0266(15) 0.0403(17) -0.0114(13) -0.0096(14) 0.0088(13)
C14A 0.0456(19) 0.0432(19) 0.0230(15) -0.0003(13) 0.0014(13) 0.0244(15)
C15A 0.0458(19) 0.0326(17) 0.0302(16) 0.0075(13) 0.0145(14) 0.0144(14)
C16A 0.0341(16) 0.0277(15) 0.0286(15) 0.0029(12) 0.0081(12) 0.0029(12)
C20A 0.0259(14) 0.0239(14) 0.0271(14) -0.0007(11) 0.0042(11) -0.0031(11)
C21A 0.0289(15) 0.0245(14) 0.0266(14) -0.0033(11) 0.0029(11) -0.0010(12)
C22A 0.0281(14) 0.0267(14) 0.0192(13) -0.0028(10) 0.0042(11) -0.0011(11)
C23A 0.0292(15) 0.0322(16) 0.0233(14) -0.0045(11) -0.0005(11) 0.0041(12)
C24A 0.0390(17) 0.0290(15) 0.0282(15) 0.0028(12) -0.0006(12) 0.0005(13)
C25A 0.0426(18) 0.0328(17) 0.0330(16) 0.0041(13) 0.0115(13) -0.0053(14)
C26A 0.0287(15) 0.0321(16) 0.0373(16) -0.0035(13) 0.0133(13) -0.0016(13)
C31A 0.0310(15) 0.0229(14) 0.0252(14) -0.0007(11) 0.0095(11) -0.0049(11)
C32A 0.0406(17) 0.0268(15) 0.0265(14) -0.0031(12) 0.0063(12) -0.0040(13)
C33A 0.050(2) 0.0282(16) 0.0328(16) -0.0057(12) 0.0088(14) -0.0006(14)
C34A 0.0427(18) 0.0211(15) 0.0437(18) 0.0023(12) 0.0134(14) 0.0071(13)
C35A 0.0315(16) 0.0300(16) 0.0351(16) 0.0035(12) 0.0050(12) 0.0001(13)
C36A 0.0300(15) 0.0214(14) 0.0290(14) -0.0013(11) 0.0088(11) -0.0027(11)
C41A 0.0365(16) 0.0263(15) 0.0244(14) 0.0001(11) 0.0101(12) -0.0012(12)
C42A 0.0338(16) 0.0311(16) 0.0321(16) 0.0015(12) 0.0092(12) 0.0002(13)
C43A 0.0393(18) 0.0294(16) 0.054(2) 0.0004(14) 0.0237(16) 0.0029(14)
C44A 0.061(2) 0.0308(17) 0.0375(18) -0.0059(14) 0.0291(16) -0.0022(16)
C45A 0.066(2) 0.0320(17) 0.0236(15) -0.0025(12) 0.0076(15) -0.0028(16)
C46A 0.0403(18) 0.0340(17) 0.0303(16) -0.0010(13) 0.0056(13) 0.0034(14)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C1S 1.777(4) . ?
Cl2 C1S 1.764(4) . ?
P1 F1 1.6006(19) . ?
P1 F2 1.5904(19) . ?
P1 F3 1.582(3) . ?
P1 F4 1.568(3) . ?
P1 F5 1.571(2) . ?
P1 F6 1.566(3) . ?
P1A F1A 1.598(2) . ?
P1A F2A 1.594(2) . ?
P1A F3A 1.595(2) . ?
P1A F4A 1.595(3) . ?
P1A F5A 1.589(2) . ?
P1A F6A 1.573(3) . ?
N1 C1 1.477(4) . ?
N1 C2 1.346(4) . ?
N1 C6 1.347(4) . ?
C2 C3 1.374(4) . ?
C3 C4 1.399(4) . ?
C4 C5 1.402(4) . ?
C4 C7 1.457(4) . ?
C5 C6 1.371(4) . ?
C7 C8 1.330(4) . ?
C8 C14 1.463(4) . ?
C10 C11 1.495(4) . ?
C10 C20 1.355(4) . ?
C10 C31 1.490(4) . ?
C11 C12 1.394(4) . ?
C11 C16 1.398(4) . ?
C12 C13 1.386(4) . ?
C13 C14 1.392(4) . ?
C14 C15 1.403(4) . ?
C15 C16 1.377(4) . ?
C20 C21 1.499(4) . ?
C20 C41 1.495(4) . ?
C21 C22 1.389(4) . ?
C21 C26 1.394(4) . ?
C22 C23 1.389(5) . ?
C23 C24 1.385(5) . ?
C24 C25 1.385(5) . ?
C25 C26 1.382(4) . ?
C31 C32 1.402(4) . ?
C31 C36 1.392(4) . ?
C32 C33 1.393(4) . ?
C33 C34 1.391(5) . ?
C34 C35 1.383(5) . ?
C35 C36 1.385(4) . ?
C41 C42 1.390(4) . ?
C41 C46 1.391(4) . ?
C42 C43 1.384(4) . ?
C43 C44 1.382(5) . ?
C44 C45 1.379(5) . ?
C45 C46 1.386(5) . ?
N1A C1A 1.477(4) . ?
N1A C2A 1.331(6) . ?
N1A C2B 1.406(18) . ?
N1A C6A 1.353(6) . ?
N1A C6B 1.347(17) . ?
C2A C3A 1.374(6) . ?
C2B C3B 1.371(14) . ?
C3A C4A 1.398(6) . ?
C3B C4B 1.371(14) . ?
C4A C5A 1.400(6) . ?
C4A C7A 1.468(6) . ?
C4B C5B 1.370(14) . ?
C4B C7B 1.48(2) . ?
C5A C6A 1.371(6) . ?
C5B C6B 1.350(14) . ?
C7A C8A 1.335(6) . ?
C7B C8B 1.33(2) . ?
C8A C14A 1.479(5) . ?
C8B C14A 1.599(17) . ?
C10A C11A 1.495(4) . ?
C10A C20A 1.344(4) . ?
C10A C31A 1.507(4) . ?
C11A C12A 1.393(4) . ?
C11A C16A 1.397(4) . ?
C12A C13A 1.393(4) . ?
C13A C14A 1.402(5) . ?
C14A C15A 1.382(5) . ?
C15A C16A 1.381(4) . ?
C20A C21A 1.489(4) . ?
C20A C41A 1.504(4) . ?
C21A C22A 1.391(4) . ?
C21A C26A 1.405(4) . ?
C22A C23A 1.384(4) . ?
C23A C24A 1.385(4) . ?
C24A C25A 1.379(5) . ?
C25A C26A 1.380(5) . ?
C31A C32A 1.399(4) . ?
C31A C36A 1.395(4) . ?
C32A C33A 1.385(5) . ?
C33A C34A 1.371(5) . ?
C34A C35A 1.407(5) . ?
C35A C36A 1.379(4) . ?
C41A C42A 1.390(4) . ?
C41A C46A 1.396(4) . ?
C42A C43A 1.385(4) . ?
C43A C44A 1.375(5) . ?
C44A C45A 1.374(5) . ?
C45A C46A 1.385(5) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 C1S Cl1 109.6(2) . . ?
F2 P1 F1 179.27(13) . . ?
F3 P1 F1 89.85(13) . . ?
F3 P1 F2 90.16(13) . . ?
F4 P1 F1 88.28(13) . . ?
F4 P1 F2 91.00(13) . . ?
F4 P1 F3 89.49(19) . . ?
F4 P1 F5 89.7(2) . . ?
F5 P1 F1 89.97(12) . . ?
F5 P1 F2 90.01(12) . . ?
F5 P1 F3 179.2(2) . . ?
F6 P1 F1 91.71(14) . . ?
F6 P1 F2 89.02(14) . . ?
F6 P1 F3 89.3(2) . . ?
F6 P1 F4 178.8(2) . . ?
F6 P1 F5 91.5(2) . . ?
F2A P1A F1A 178.96(15) . . ?
F2A P1A F3A 90.69(13) . . ?
F2A P1A F4A 90.10(16) . . ?
F3A P1A F1A 89.74(12) . . ?
F4A P1A F1A 88.96(14) . . ?
F4A P1A F3A 89.63(18) . . ?
F5A P1A F1A 90.64(12) . . ?
F5A P1A F2A 88.91(13) . . ?
F5A P1A F3A 178.53(18) . . ?
F5A P1A F4A 88.96(15) . . ?
F6A P1A F1A 90.82(14) . . ?
F6A P1A F2A 90.12(16) . . ?
F6A P1A F3A 90.60(17) . . ?
F6A P1A F4A 179.7(2) . . ?
F6A P1A F5A 90.81(15) . . ?
C2 N1 C1 118.7(3) . . ?
C2 N1 C6 120.7(3) . . ?
C6 N1 C1 120.6(3) . . ?
N1 C2 C3 120.3(3) . . ?
C2 C3 C4 120.7(3) . . ?
C3 C4 C5 117.1(3) . . ?
C3 C4 C7 119.9(3) . . ?
C5 C4 C7 123.0(3) . . ?
C6 C5 C4 120.1(3) . . ?
N1 C6 C5 121.0(3) . . ?
C8 C7 C4 124.7(3) . . ?
C7 C8 C14 125.6(3) . . ?
C20 C10 C11 122.2(3) . . ?
C20 C10 C31 123.7(3) . . ?
C31 C10 C11 114.0(2) . . ?
C12 C11 C10 120.4(3) . . ?
C12 C11 C16 118.3(3) . . ?
C16 C11 C10 121.3(2) . . ?
C13 C12 C11 120.8(3) . . ?
C12 C13 C14 120.8(3) . . ?
C13 C14 C8 119.5(2) . . ?
C13 C14 C15 118.4(3) . . ?
C15 C14 C8 122.0(3) . . ?
C16 C15 C14 120.6(3) . . ?
C15 C16 C11 121.1(3) . . ?
C10 C20 C21 122.1(3) . . ?
C10 C20 C41 122.2(3) . . ?
C41 C20 C21 115.7(2) . . ?
C22 C21 C20 122.0(3) . . ?
C22 C21 C26 118.2(3) . . ?
C26 C21 C20 119.8(3) . . ?
C23 C22 C21 120.7(3) . . ?
C24 C23 C22 120.3(3) . . ?
C25 C24 C23 119.4(3) . . ?
C26 C25 C24 120.0(3) . . ?
C25 C26 C21 121.2(3) . . ?
C32 C31 C10 119.1(3) . . ?
C36 C31 C10 122.7(3) . . ?
C36 C31 C32 118.2(3) . . ?
C33 C32 C31 120.7(3) . . ?
C34 C33 C32 120.2(3) . . ?
C35 C34 C33 119.3(3) . . ?
C34 C35 C36 120.7(3) . . ?
C35 C36 C31 121.0(3) . . ?
C42 C41 C20 121.3(3) . . ?
C42 C41 C46 118.2(3) . . ?
C46 C41 C20 120.5(3) . . ?
C43 C42 C41 121.4(3) . . ?
C44 C43 C42 119.9(3) . . ?
C45 C44 C43 119.4(3) . . ?
C44 C45 C46 120.8(3) . . ?
C45 C46 C41 120.4(3) . . ?
C2A N1A C1A 117.8(3) . . ?
C2A N1A C6A 120.4(4) . . ?
C2B N1A C1A 131.8(7) . . ?
C6A N1A C1A 121.8(3) . . ?
C6B N1A C1A 108.5(8) . . ?
C6B N1A C2B 119.7(11) . . ?
N1A C2A C3A 121.0(4) . . ?
C3B C2B N1A 120.6(14) . . ?
C2A C3A C4A 120.6(4) . . ?
C2B C3B C4B 119.1(14) . . ?
C3A C4A C5A 116.8(4) . . ?
C3A C4A C7A 120.5(4) . . ?
C5A C4A C7A 122.6(4) . . ?
C3B C4B C7B 122.2(14) . . ?
C5B C4B C3B 118.2(12) . . ?
C5B C4B C7B 119.6(13) . . ?
C6A C5A C4A 120.3(4) . . ?
C6B C5B C4B 123.8(15) . . ?
N1A C6A C5A 120.9(5) . . ?
N1A C6B C5B 118.4(15) . . ?
C8A C7A C4A 124.5(4) . . ?
C8B C7B C4B 123.1(15) . . ?
C7A C8A C14A 124.4(5) . . ?
C7B C8B C14A 111.8(15) . . ?
C11A C10A C31A 113.8(2) . . ?
C20A C10A C11A 124.9(3) . . ?
C20A C10A C31A 121.3(3) . . ?
C12A C11A C10A 122.8(3) . . ?
C12A C11A C16A 118.3(3) . . ?
C16A C11A C10A 118.7(3) . . ?
C13A C12A C11A 120.5(3) . . ?
C12A C13A C14A 120.8(3) . . ?
C13A C14A C8A 126.8(4) . . ?
C13A C14A C8B 97.3(6) . . ?
C15A C14A C8A 114.9(4) . . ?
C15A C14A C8B 144.0(6) . . ?
C15A C14A C13A 118.2(3) . . ?
C16A C15A C14A 121.3(3) . . ?
C15A C16A C11A 121.0(3) . . ?
C10A C20A C21A 124.0(3) . . ?
C10A C20A C41A 121.8(3) . . ?
C21A C20A C41A 114.2(2) . . ?
C22A C21A C20A 122.9(3) . . ?
C22A C21A C26A 118.2(3) . . ?
C26A C21A C20A 118.8(3) . . ?
C23A C22A C21A 120.2(3) . . ?
C22A C23A C24A 121.0(3) . . ?
C25A C24A C23A 119.4(3) . . ?
C24A C25A C26A 120.1(3) . . ?
C25A C26A C21A 121.1(3) . . ?
C32A C31A C10A 122.4(3) . . ?
C36A C31A C10A 118.8(2) . . ?
C36A C31A C32A 118.8(3) . . ?
C33A C32A C31A 120.1(3) . . ?
C34A C33A C32A 120.8(3) . . ?
C33A C34A C35A 119.6(3) . . ?
C36A C35A C34A 119.6(3) . . ?
C35A C36A C31A 120.8(3) . . ?
C42A C41A C20A 122.4(3) . . ?
C42A C41A C46A 119.0(3) . . ?
C46A C41A C20A 118.5(3) . . ?
C43A C42A C41A 120.1(3) . . ?
C44A C43A C42A 120.3(3) . . ?
C43A C44A C45A 120.2(3) . . ?
C44A C45A C46A 120.2(3) . . ?
C45A C46A C41A 120.0(3) . . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 C4 0.0(5) . . . . ?
C1 N1 C2 C3 -179.3(3) . . . . ?
C1 N1 C6 C5 179.4(3) . . . . ?
C2 N1 C6 C5 -0.1(5) . . . . ?
C2 C3 C4 C5 -0.5(4) . . . . ?
C2 C3 C4 C7 -179.7(3) . . . . ?
C3 C4 C5 C6 0.7(4) . . . . ?
C3 C4 C7 C8 160.3(3) . . . . ?
C4 C5 C6 N1 -0.4(5) . . . . ?
C4 C7 C8 C14 179.8(3) . . . . ?
C5 C4 C7 C8 -18.8(5) . . . . ?
C6 N1 C2 C3 0.3(5) . . . . ?
C7 C4 C5 C6 179.8(3) . . . . ?
C7 C8 C14 C13 163.7(3) . . . . ?
C7 C8 C14 C15 -16.5(4) . . . . ?
C8 C14 C15 C16 179.9(3) . . . . ?
C10 C11 C12 C13 178.8(3) . . . . ?
C10 C11 C16 C15 -177.0(3) . . . . ?
C10 C20 C21 C22 -45.4(4) . . . . ?
C10 C20 C21 C26 134.0(3) . . . . ?
C10 C20 C41 C42 -46.5(4) . . . . ?
C10 C20 C41 C46 135.2(3) . . . . ?
C10 C31 C32 C33 -178.3(3) . . . . ?
C10 C31 C36 C35 179.1(3) . . . . ?
C11 C10 C20 C21 -7.8(4) . . . . ?
C11 C10 C20 C41 169.5(3) . . . . ?
C11 C10 C31 C32 -40.7(4) . . . . ?
C11 C10 C31 C36 138.9(3) . . . . ?
C11 C12 C13 C14 -2.7(5) . . . . ?
C12 C11 C16 C15 0.5(4) . . . . ?
C12 C13 C14 C8 -178.0(3) . . . . ?
C12 C13 C14 C15 2.1(4) . . . . ?
C13 C14 C15 C16 -0.3(4) . . . . ?
C14 C15 C16 C11 -1.0(4) . . . . ?
C16 C11 C12 C13 1.4(4) . . . . ?
C20 C10 C11 C12 124.0(3) . . . . ?
C20 C10 C11 C16 -58.6(4) . . . . ?
C20 C10 C31 C32 137.1(3) . . . . ?
C20 C10 C31 C36 -43.3(4) . . . . ?
C20 C21 C22 C23 176.3(3) . . . . ?
C20 C21 C26 C25 -176.1(3) . . . . ?
C20 C41 C42 C43 179.0(3) . . . . ?
C20 C41 C46 C45 179.9(3) . . . . ?
C21 C20 C41 C42 130.9(3) . . . . ?
C21 C20 C41 C46 -47.4(4) . . . . ?
C21 C22 C23 C24 0.9(6) . . . . ?
C22 C21 C26 C25 3.3(4) . . . . ?
C22 C23 C24 C25 1.2(6) . . . . ?
C23 C24 C25 C26 -1.0(5) . . . . ?
C24 C25 C26 C21 -1.3(5) . . . . ?
C26 C21 C22 C23 -3.1(5) . . . . ?
C31 C10 C11 C12 -58.2(4) . . . . ?
C31 C10 C11 C16 119.2(3) . . . . ?
C31 C10 C20 C21 174.6(3) . . . . ?
C31 C10 C20 C41 -8.1(4) . . . . ?
C31 C32 C33 C34 -1.6(5) . . . . ?
C32 C31 C36 C35 -1.2(4) . . . . ?
C32 C33 C34 C35 0.2(5) . . . . ?
C33 C34 C35 C36 0.6(5) . . . . ?
C34 C35 C36 C31 -0.1(4) . . . . ?
C36 C31 C32 C33 2.0(4) . . . . ?
C41 C20 C21 C22 137.2(3) . . . . ?
C41 C20 C21 C26 -43.4(4) . . . . ?
C41 C42 C43 C44 1.6(4) . . . . ?
C42 C41 C46 C45 1.4(4) . . . . ?
C42 C43 C44 C45 0.7(4) . . . . ?
C43 C44 C45 C46 -1.9(5) . . . . ?
C44 C45 C46 C41 0.8(5) . . . . ?
C46 C41 C42 C43 -2.6(4) . . . . ?
N1A C2A C3A C4A 2.0(7) . . . . ?
N1A C2B C3B C4B 0(3) . . . . ?
C1A N1A C2A C3A -177.0(4) . . . . ?
C1A N1A C2B C3B -179.4(12) . . . . ?
C1A N1A C6A C5A 175.2(5) . . . . ?
C1A N1A C6B C5B -179.5(17) . . . . ?
C2A N1A C6A C5A -1.5(10) . . . . ?
C2A C3A C4A C5A -2.3(6) . . . . ?
C2A C3A C4A C7A 174.2(4) . . . . ?
C2B N1A C6B C5B -1(3) . . . . ?
C2B C3B C4B C5B -3(2) . . . . ?
C2B C3B C4B C7B 176.6(17) . . . . ?
C3A C4A C5A C6A 0.7(7) . . . . ?
C3A C4A C7A C8A 174.4(4) . . . . ?
C3B C4B C5B C6B 5(3) . . . . ?
C3B C4B C7B C8B -24(2) . . . . ?
C4A C5A C6A N1A 1.2(10) . . . . ?
C4A C7A C8A C14A 174.5(4) . . . . ?
C4B C5B C6B N1A -3(3) . . . . ?
C4B C7B C8B C14A -176.4(12) . . . . ?
C5A C4A C7A C8A -9.3(6) . . . . ?
C5B C4B C7B C8B 155.9(15) . . . . ?
C6A N1A C2A C3A -0.1(9) . . . . ?
C6B N1A C2B C3B 3(3) . . . . ?
C7A C4A C5A C6A -175.7(5) . . . . ?
C7A C8A C14A C13A -27.6(6) . . . . ?
C7A C8A C14A C15A 155.0(4) . . . . ?
C7B C4B C5B C6B -174.9(18) . . . . ?
C7B C8B C14A C13A 169.0(10) . . . . ?
C7B C8B C14A C15A -20.5(17) . . . . ?
C8A C14A C15A C16A 179.4(3) . . . . ?
C8B C14A C15A C16A -167.5(9) . . . . ?
C10A C11A C12A C13A -173.9(3) . . . . ?
C10A C11A C16A C15A 175.3(3) . . . . ?
C10A C20A C21A C22A -45.7(4) . . . . ?
C10A C20A C21A C26A 137.5(3) . . . . ?
C10A C20A C41A C42A -62.6(4) . . . . ?
C10A C20A C41A C46A 119.1(3) . . . . ?
C10A C31A C32A C33A 176.8(3) . . . . ?
C10A C31A C36A C35A -175.4(3) . . . . ?
C11A C10A C20A C21A -5.3(5) . . . . ?
C11A C10A C20A C41A 174.8(3) . . . . ?
C11A C10A C31A C32A 133.1(3) . . . . ?
C11A C10A C31A C36A -47.1(3) . . . . ?
C11A C12A C13A C14A -1.0(4) . . . . ?
C12A C11A C16A C15A -0.3(4) . . . . ?
C12A C13A C14A C8A -177.9(3) . . . . ?
C12A C13A C14A C8B 173.0(6) . . . . ?
C12A C13A C14A C15A -0.6(5) . . . . ?
C13A C14A C15A C16A 1.8(5) . . . . ?
C14A C15A C16A C11A -1.3(5) . . . . ?
C16A C11A C12A C13A 1.5(4) . . . . ?
C20A C10A C11A C12A -54.1(4) . . . . ?
C20A C10A C11A C16A 130.6(3) . . . . ?
C20A C10A C31A C32A -49.6(4) . . . . ?
C20A C10A C31A C36A 130.3(3) . . . . ?
C20A C21A C22A C23A -176.6(3) . . . . ?
C20A C21A C26A C25A 177.8(3) . . . . ?
C20A C41A C42A C43A -179.1(3) . . . . ?
C20A C41A C46A C45A -178.7(3) . . . . ?
C21A C20A C41A C42A 117.4(3) . . . . ?
C21A C20A C41A C46A -60.9(4) . . . . ?
C21A C22A C23A C24A -0.6(4) . . . . ?
C22A C21A C26A C25A 0.9(4) . . . . ?
C22A C23A C24A C25A 0.0(4) . . . . ?
C23A C24A C25A C26A 1.1(5) . . . . ?
C24A C25A C26A C21A -1.6(5) . . . . ?
C26A C21A C22A C23A 0.2(4) . . . . ?
C31A C10A C11A C12A 123.2(3) . . . . ?
C31A C10A C11A C16A -52.2(3) . . . . ?
C31A C10A C20A C21A 177.7(3) . . . . ?
C31A C10A C20A C41A -2.3(4) . . . . ?
C31A C32A C33A C34A -0.4(5) . . . . ?
C32A C31A C36A C35A 4.4(4) . . . . ?
C32A C33A C34A C35A 2.6(5) . . . . ?
C33A C34A C35A C36A -1.3(5) . . . . ?
C34A C35A C36A C31A -2.3(4) . . . . ?
C36A C31A C32A C33A -3.1(4) . . . . ?
C41A C20A C21A C22A 134.2(3) . . . . ?
C41A C20A C21A C26A -42.5(4) . . . . ?
C41A C42A C43A C44A -1.9(5) . . . . ?
C42A C41A C46A C45A 3.0(5) . . . . ?
C42A C43A C44A C45A 2.5(5) . . . . ?
C43A C44A C45A C46A -0.3(5) . . . . ?
C44A C45A C46A C41A -2.4(5) . . . . ?
C46A C41A C42A C43A -0.8(5) . . . . ?
_shelx_res_file
;
khor3cult.res created by SHELXL-2014/7
TITL khor3CuLT in P21/n #14
REM reset to P21/n #14
CELL 1.54184 11.252458 9.219397 59.13975 90 93.8053 90
ZERR 4 0.000203 0.000135 0.000913 0 0.0014 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cl F N P
UNIT 276 232 8 48 8 8
SADI C3B C2B C4B C3B C5B C4B C6B C5B
SADI C3A C2A C4A C3A C5A C4A C6A C5A
SADI N1A C2B N1A C6B
SADI N1A C6A N1A C2A
RIGU 0.001 0.001 N1A C2B C3B C4B C5B C6B
RIGU 0.001 0.001 N1A C2A C3A C4A C5A C6A
L.S. 10
PLAN 20
SIZE 0.02 0.02 0.2
TEMP -173
CONF
BOND
fmap 2
acta 133
OMIT 0 135
OMIT -2 0 8
OMIT -4 2 5
OMIT 1 0 21
OMIT 2 1 11
OMIT -7 2 61
OMIT 3 2 3
OMIT -5 1 2
OMIT -4 0 4
OMIT 1 8 5
OMIT 6 9 7
OMIT 2 0 28
OMIT -8 1 58
OMIT -2 2 2
OMIT 2 1 15
OMIT -8 2 56
OMIT 2 3 8
OMIT 2 3 16
OMIT -3 3 18
OMIT 0 0 30
OMIT -6 1 8
OMIT -6 1 11
OMIT 1 2 20
OMIT -3 2 2
OMIT 2 0 2
OMIT -4 1 3
OMIT 0 3 2
OMIT -5 0 7
OMIT 3 2 13
OMIT -1 4 22
REM
REM
REM
WGHT 0.066000 8.225000
FVAR 2.67257
CL1 3 0.884124 0.426757 0.152366 11.00000 0.07165 0.04375 =
0.04889 0.00853 0.01739 0.00159
CL2 3 0.804609 0.135768 0.161695 11.00000 0.05605 0.06065 =
0.04859 0.01764 -0.00167 -0.01069
C1S 1 0.927087 0.255452 0.164017 11.00000 0.04086 0.04425 =
0.04175 0.00160 0.00550 0.00457
AFIX 23
H1SA 2 0.993471 0.215141 0.155805 11.00000 -1.20000
H1SB 2 0.954904 0.267056 0.180150 11.00000 -1.20000
AFIX 0
P1 6 0.186540 0.970032 0.194988 11.00000 0.02986 0.03226 =
0.02634 0.00353 0.00885 0.00252
F1 4 0.127254 0.948740 0.218627 11.00000 0.05604 0.05620 =
0.03936 0.00868 0.02667 0.00738
F2 4 0.247038 0.991545 0.171668 11.00000 0.05883 0.05816 =
0.03245 0.01541 0.01985 0.01390
F3 4 0.155914 1.137366 0.195546 11.00000 0.12315 0.04504 =
0.06518 0.00928 0.03188 0.02233
F4 4 0.307858 1.001676 0.208706 11.00000 0.04206 0.14890 =
0.05057 0.01332 -0.00024 -0.01109
F5 4 0.218463 0.804226 0.194685 11.00000 0.20045 0.04009 =
0.04108 0.00981 0.04573 0.02981
F6 4 0.064795 0.941926 0.181312 11.00000 0.05717 0.16431 =
0.06412 0.02846 -0.01021 -0.05058
P1A 6 0.907508 0.464778 0.227439 11.00000 0.04001 0.04365 =
0.03813 0.00572 0.01335 0.00770
F1A 4 0.846625 0.365172 0.245531 11.00000 0.06104 0.04364 =
0.04155 0.00462 0.01719 0.00176
F2A 4 0.970508 0.563693 0.209643 11.00000 0.06562 0.06901 =
0.07732 0.02776 0.04286 0.01783
F3A 4 0.833576 0.600757 0.235529 11.00000 0.09688 0.04732 =
0.09631 0.02188 0.06332 0.02501
F4A 4 1.011136 0.501918 0.246274 11.00000 0.07075 0.09257 =
0.06746 -0.01606 0.00215 -0.02125
F5A 4 0.984125 0.330961 0.219718 11.00000 0.05478 0.05517 =
0.05706 0.00148 0.01522 0.01857
F6A 4 0.805384 0.427241 0.208905 11.00000 0.04256 0.13281 =
0.04786 0.00913 0.00307 0.01046
N1 5 0.775518 0.943625 0.210732 11.00000 0.02577 0.03807 =
0.02541 -0.00338 0.00539 -0.00618
C1 1 0.854485 1.013905 0.228423 11.00000 0.03229 0.05717 =
0.03894 -0.01590 0.00067 -0.01300
AFIX 137
H1A 2 0.813266 1.096802 0.234711 11.00000 -1.50000
H1B 2 0.927083 1.047551 0.221782 11.00000 -1.50000
H1C 2 0.875514 0.944003 0.240517 11.00000 -1.50000
AFIX 0
C2 1 0.820617 0.838506 0.198036 11.00000 0.02486 0.03908 =
0.03014 -0.00003 0.00420 -0.00209
AFIX 43
H2 2 0.901540 0.810305 0.200696 11.00000 -1.20000
AFIX 0
C3 1 0.750221 0.771781 0.181251 11.00000 0.03167 0.03244 =
0.03167 -0.00352 0.00588 0.00132
AFIX 43
H3 2 0.782951 0.697685 0.172390 11.00000 -1.20000
AFIX 0
C4 1 0.630839 0.811761 0.177061 11.00000 0.02889 0.02650 =
0.02174 0.00082 0.00540 -0.00492
C5 1 0.587228 0.920873 0.190785 11.00000 0.02597 0.03252 =
0.02833 -0.00330 0.00324 -0.00190
AFIX 43
H5 2 0.506448 0.950672 0.188639 11.00000 -1.20000
AFIX 0
C6 1 0.660868 0.984686 0.207297 11.00000 0.03310 0.03689 =
0.02810 -0.00630 0.00705 -0.00259
AFIX 43
H6 2 0.630597 1.058961 0.216451 11.00000 -1.20000
AFIX 0
C7 1 0.557480 0.739124 0.159266 11.00000 0.03268 0.02736 =
0.02170 -0.00170 0.00544 -0.00017
AFIX 43
H7 2 0.597064 0.689358 0.147876 11.00000 -1.20000
AFIX 0
C8 1 0.439053 0.737523 0.157831 11.00000 0.03196 0.02291 =
0.02091 -0.00085 0.00397 -0.00150
AFIX 43
H8 2 0.400068 0.787172 0.169312 11.00000 -1.20000
AFIX 0
C10 1 0.136721 0.446198 0.089505 11.00000 0.02670 0.02662 =
0.02414 -0.00271 0.00400 0.00061
C11 1 0.215083 0.525814 0.106727 11.00000 0.02984 0.02401 =
0.02257 0.00055 0.00180 -0.00070
C12 1 0.171547 0.568710 0.127220 11.00000 0.02961 0.03419 =
0.02748 -0.00327 0.00487 -0.00502
AFIX 43
H12 2 0.091126 0.548627 0.130094 11.00000 -1.20000
AFIX 0
C13 1 0.244213 0.640311 0.143449 11.00000 0.03215 0.03325 =
0.02074 -0.00259 0.00706 -0.00304
AFIX 43
H13 2 0.212098 0.672369 0.157040 11.00000 -1.20000
AFIX 0
C14 1 0.363659 0.665806 0.140075 11.00000 0.03247 0.02204 =
0.01942 -0.00039 0.00288 -0.00008
C15 1 0.407832 0.621649 0.119538 11.00000 0.02967 0.02408 =
0.02418 0.00017 0.00420 -0.00101
AFIX 43
H15 2 0.489027 0.638478 0.116883 11.00000 -1.20000
AFIX 0
C16 1 0.334513 0.554105 0.103188 11.00000 0.03533 0.02714 =
0.01851 -0.00186 0.00453 0.00219
AFIX 43
H16 2 0.365594 0.526294 0.089283 11.00000 -1.20000
AFIX 0
C20 1 0.116567 0.494564 0.067959 11.00000 0.02745 0.02455 =
0.02632 -0.00036 0.00292 0.00237
C21 1 0.158882 0.640280 0.060607 11.00000 0.02979 0.02755 =
0.02623 0.00182 -0.00172 0.00104
C22 1 0.144473 0.764601 0.073410 11.00000 0.05235 0.02788 =
0.02867 0.00117 0.00633 0.00482
AFIX 43
H22 2 0.102620 0.759266 0.086818 11.00000 -1.20000
AFIX 0
C23 1 0.190571 0.896582 0.066827 11.00000 0.06762 0.02689 =
0.04029 -0.00478 0.00241 0.00156
AFIX 43
H23 2 0.181029 0.980462 0.075859 11.00000 -1.20000
AFIX 0
C24 1 0.250411 0.906575 0.047154 11.00000 0.05276 0.02913 =
0.04203 0.00514 -0.00031 -0.00576
AFIX 43
H24 2 0.283203 0.996528 0.042810 11.00000 -1.20000
AFIX 0
C25 1 0.262018 0.784263 0.033870 11.00000 0.03371 0.03376 =
0.03063 0.00519 -0.00008 -0.00097
AFIX 43
H25 2 0.301841 0.790478 0.020233 11.00000 -1.20000
AFIX 0
C26 1 0.215669 0.653171 0.040453 11.00000 0.02921 0.02801 =
0.02577 0.00118 -0.00349 0.00147
AFIX 43
H26 2 0.222639 0.570358 0.031074 11.00000 -1.20000
AFIX 0
C31 1 0.087491 0.307901 0.097968 11.00000 0.02944 0.02863 =
0.01814 -0.00200 0.00426 0.00074
C32 1 0.161210 0.217548 0.111860 11.00000 0.03239 0.03170 =
0.02767 -0.00035 -0.00054 -0.00290
AFIX 43
H32 2 0.240652 0.246566 0.116042 11.00000 -1.20000
AFIX 0
C33 1 0.119108 0.085691 0.119587 11.00000 0.04564 0.03307 =
0.03005 0.00602 -0.00070 0.00287
AFIX 43
H33 2 0.170445 0.024261 0.128682 11.00000 -1.20000
AFIX 0
C34 1 0.002037 0.043720 0.114018 11.00000 0.04057 0.03277 =
0.03313 0.00310 0.00761 -0.00821
AFIX 43
H34 2 -0.027002 -0.046013 0.119304 11.00000 -1.20000
AFIX 0
C35 1 -0.071605 0.133983 0.100707 11.00000 0.03055 0.03828 =
0.02869 0.00018 0.00792 -0.00476
AFIX 43
H35 2 -0.151841 0.106296 0.096978 11.00000 -1.20000
AFIX 0
C36 1 -0.029609 0.264302 0.092757 11.00000 0.02786 0.03138 =
0.02313 -0.00170 0.00523 0.00281
AFIX 43
H36 2 -0.081450 0.324854 0.083613 11.00000 -1.20000
AFIX 0
C41 1 0.055527 0.403566 0.049758 11.00000 0.02546 0.03022 =
0.02213 0.00251 0.00341 -0.00359
C42 1 0.087164 0.259486 0.046707 11.00000 0.02862 0.03324 =
0.02207 0.00067 0.00440 -0.00270
AFIX 43
H42 2 0.149717 0.218456 0.056220 11.00000 -1.20000
AFIX 0
C43 1 0.029418 0.174589 0.030098 11.00000 0.03144 0.03947 =
0.02785 -0.00845 0.00936 -0.00795
AFIX 43
H43 2 0.051014 0.075657 0.028535 11.00000 -1.20000
AFIX 0
C44 1 -0.059746 0.234029 0.015789 11.00000 0.03314 0.05301 =
0.02457 -0.00662 0.00581 -0.01480
AFIX 43
H44 2 -0.100376 0.176096 0.004460 11.00000 -1.20000
AFIX 0
C45 1 -0.089179 0.378227 0.018111 11.00000 0.02945 0.05739 =
0.02647 0.00923 -0.00139 -0.00768
AFIX 43
H45 2 -0.148749 0.420156 0.008009 11.00000 -1.20000
AFIX 0
C46 1 -0.032957 0.462718 0.034992 11.00000 0.03007 0.03885 =
0.03162 0.00741 -0.00039 -0.00271
AFIX 43
H46 2 -0.054944 0.561565 0.036493 11.00000 -1.20000
AFIX 0
N1A 5 0.341852 0.603733 0.228527 11.00000 0.03543 0.02657 =
0.02270 0.00144 0.00229 0.00075
C1A 1 0.291812 0.695263 0.246058 11.00000 0.06957 0.04252 =
0.02317 -0.00581 0.01021 0.01280
AFIX 137
H1AA 2 0.349766 0.703660 0.259111 11.00000 -1.50000
H1AB 2 0.218463 0.650942 0.250871 11.00000 -1.50000
H1AC 2 0.274006 0.791919 0.239822 11.00000 -1.50000
AFIX 0
PART 1
C2A 1 0.457583 0.616448 0.225503 10.75000 0.03454 0.02083 =
0.02227 0.00072 0.00097 0.00024
AFIX 43
H2A 2 0.505224 0.679486 0.235030 10.75000 -1.20000
AFIX 0
PART 0
PART 2
C2B 1 0.457952 0.591152 0.221290 10.25000 0.03646 0.03636 =
0.03302 -0.00841 0.00517 -0.00286
AFIX 43
H2B 2 0.520275 0.648252 0.228306 10.25000 -1.20000
AFIX 0
PART 0
PART 1
C3A 1 0.509133 0.539712 0.208802 10.75000 0.02966 0.02209 =
0.02367 -0.00019 0.00087 -0.00242
AFIX 43
H3A 2 0.592344 0.547854 0.207232 10.75000 -1.20000
AFIX 0
PART 0
PART 2
C3B 1 0.482070 0.497314 0.204212 10.25000 0.03643 0.03497 =
0.03292 -0.00798 0.00729 -0.00500
AFIX 43
H3B 2 0.560531 0.489294 0.199321 10.25000 -1.20000
AFIX 0
PART 0
PART 1
C4A 1 0.440277 0.449797 0.194102 10.75000 0.02724 0.02087 =
0.02164 0.00046 0.00304 -0.00215
PART 0
PART 2
C4B 1 0.391375 0.415174 0.194284 10.25000 0.03628 0.03148 =
0.02715 -0.00262 0.00597 -0.00403
PART 0
PART 1
C5A 1 0.319054 0.438553 0.197865 10.75000 0.02868 0.03392 =
0.02963 -0.00789 0.00535 -0.00425
AFIX 43
H5A 2 0.268839 0.377882 0.188416 10.75000 -1.20000
AFIX 0
PART 0
PART 2
C5B 1 0.281293 0.424929 0.202763 10.25000 0.03669 0.03440 =
0.03055 -0.00556 0.00754 -0.00512
AFIX 43
H5B 2 0.220262 0.362075 0.196721 10.25000 -1.20000
AFIX 0
PART 0
PART 1
C6A 1 0.272527 0.514674 0.215116 10.75000 0.03117 0.03205 =
0.02825 -0.00398 0.00646 -0.00191
AFIX 43
H6A 2 0.190482 0.504754 0.217690 10.75000 -1.20000
AFIX 0
PART 0
PART 2
C6B 1 0.254494 0.518678 0.219207 10.25000 0.03703 0.03805 =
0.03207 -0.00823 0.00649 -0.00393
AFIX 43
H6B 2 0.175881 0.524501 0.224085 10.25000 -1.20000
AFIX 0
PART 0
PART 1
C7A 1 0.493251 0.378682 0.174973 10.75000 0.02481 0.02367 =
0.02512 -0.00237 0.00384 -0.00210
AFIX 43
H7A 2 0.573049 0.402862 0.172196 10.75000 -1.20000
AFIX 0
PART 0
PART 2
C7B 1 0.409075 0.317754 0.174967 10.25000 0.03883 0.03194 =
0.04244 -0.00527 0.00416 -0.00550
AFIX 43
H7B 2 0.356490 0.237881 0.172477 10.25000 -1.20000
AFIX 0
PART 0
PART 1
C8A 1 0.437096 0.282398 0.161207 10.75000 0.02651 0.01967 =
0.02668 -0.00257 0.00283 0.00370
AFIX 43
H8A 2 0.359935 0.251617 0.164752 10.75000 -1.20000
AFIX 0
PART 0
PART 2
C8B 1 0.494996 0.336594 0.160929 10.25000 0.03227 0.03311 =
0.02754 -0.00234 -0.00110 -0.01958
AFIX 43
H8B 2 0.554065 0.410119 0.162628 10.25000 -1.20000
AFIX 0
PART 0
C10A 1 0.607639 -0.005802 0.082839 11.00000 0.02486 0.02850 =
0.02519 -0.00322 0.00449 -0.00459
C11A 1 0.562856 0.079758 0.101996 11.00000 0.02422 0.02299 =
0.02306 0.00079 -0.00026 0.00334
C12A 1 0.606792 0.216549 0.108106 11.00000 0.02718 0.02567 =
0.03034 0.00008 -0.00128 0.00182
AFIX 43
H12A 2 0.662191 0.262962 0.099055 11.00000 -1.20000
AFIX 0
C13A 1 0.570082 0.285722 0.127384 11.00000 0.04049 0.02657 =
0.04030 -0.01141 -0.00959 0.00882
AFIX 43
H13A 2 0.601743 0.378279 0.131488 11.00000 -1.20000
AFIX 0
C14A 1 0.486988 0.220441 0.140805 11.00000 0.04556 0.04325 =
0.02302 -0.00033 0.00139 0.02435
C15A 1 0.441769 0.086399 0.134252 11.00000 0.04582 0.03260 =
0.03024 0.00750 0.01448 0.01437
AFIX 43
H15A 2 0.383678 0.041733 0.142896 11.00000 -1.20000
AFIX 0
C16A 1 0.479410 0.016137 0.115380 11.00000 0.03411 0.02771 =
0.02862 0.00288 0.00809 0.00285
AFIX 43
H16A 2 0.448080 -0.076848 0.111443 11.00000 -1.20000
AFIX 0
C20A 1 0.612420 0.042937 0.061493 11.00000 0.02586 0.02393 =
0.02713 -0.00067 0.00424 -0.00306
C21A 1 0.564206 0.185677 0.053458 11.00000 0.02888 0.02450 =
0.02658 -0.00327 0.00292 -0.00103
C22A 1 0.452554 0.236352 0.058519 11.00000 0.02810 0.02666 =
0.01924 -0.00280 0.00419 -0.00109
AFIX 43
H22A 2 0.405351 0.181461 0.068146 11.00000 -1.20000
AFIX 0
C23A 1 0.410101 0.366512 0.049563 11.00000 0.02924 0.03218 =
0.02334 -0.00447 -0.00055 0.00411
AFIX 43
H23A 2 0.333417 0.399635 0.053003 11.00000 -1.20000
AFIX 0
C24A 1 0.477633 0.449218 0.035669 11.00000 0.03905 0.02896 =
0.02817 0.00282 -0.00060 0.00053
AFIX 43
H24A 2 0.447562 0.538401 0.029618 11.00000 -1.20000
AFIX 0
C25A 1 0.588951 0.400987 0.030690 11.00000 0.04259 0.03279 =
0.03300 0.00409 0.01149 -0.00526
AFIX 43
H25A 2 0.636430 0.457885 0.021384 11.00000 -1.20000
AFIX 0
C26A 1 0.631465 0.270184 0.039207 11.00000 0.02869 0.03212 =
0.03728 -0.00351 0.01325 -0.00162
AFIX 43
H26A 2 0.707414 0.236742 0.035375 11.00000 -1.20000
AFIX 0
C31A 1 0.654067 -0.153862 0.089674 11.00000 0.03099 0.02287 =
0.02524 -0.00072 0.00947 -0.00489
C32A 1 0.622416 -0.279012 0.077338 11.00000 0.04056 0.02684 =
0.02654 -0.00314 0.00634 -0.00400
AFIX 43
H32A 2 0.566696 -0.273141 0.064580 11.00000 -1.20000
AFIX 0
C33A 1 0.672151 -0.411471 0.083685 11.00000 0.05001 0.02820 =
0.03278 -0.00569 0.00878 -0.00062
AFIX 43
H33A 2 0.649764 -0.496074 0.075277 11.00000 -1.20000
AFIX 0
C34A 1 0.753323 -0.422035 0.101960 11.00000 0.04266 0.02112 =
0.04370 0.00228 0.01338 0.00708
AFIX 43
H34A 2 0.789407 -0.512669 0.105804 11.00000 -1.20000
AFIX 0
C35A 1 0.782869 -0.297884 0.114987 11.00000 0.03151 0.03002 =
0.03512 0.00354 0.00505 0.00013
AFIX 43
H35A 2 0.837805 -0.304615 0.127853 11.00000 -1.20000
AFIX 0
C36A 1 0.731630 -0.166426 0.108971 11.00000 0.03005 0.02143 =
0.02902 -0.00130 0.00880 -0.00271
AFIX 43
H36A 2 0.749375 -0.083357 0.118082 11.00000 -1.20000
AFIX 0
C41A 1 0.668130 -0.044806 0.043553 11.00000 0.03646 0.02630 =
0.02439 0.00014 0.01006 -0.00121
C42A 1 0.787990 -0.082575 0.045120 11.00000 0.03376 0.03107 =
0.03208 0.00151 0.00923 0.00019
AFIX 43
H42A 2 0.837548 -0.053965 0.057979 11.00000 -1.20000
AFIX 0
C43A 1 0.835281 -0.161862 0.027963 11.00000 0.03928 0.02937 =
0.05357 0.00040 0.02372 0.00286
AFIX 43
H43A 2 0.917742 -0.184940 0.028880 11.00000 -1.20000
AFIX 0
C44A 1 0.763461 -0.207310 0.009616 11.00000 0.06146 0.03077 =
0.03750 -0.00595 0.02912 -0.00216
AFIX 43
H44A 2 0.795777 -0.264910 -0.001799 11.00000 -1.20000
AFIX 0
C45A 1 0.645028 -0.169655 0.007737 11.00000 0.06577 0.03196 =
0.02359 -0.00247 0.00763 -0.00277
AFIX 43
H45A 2 0.595824 -0.200912 -0.005010 11.00000 -1.20000
AFIX 0
C46A 1 0.597179 -0.086263 0.024374 11.00000 0.04033 0.03402 =
0.03031 -0.00102 0.00562 0.00338
AFIX 43
H46A 2 0.516050 -0.057270 0.022733 11.00000 -1.20000
AFIX 0
HKLF 4
REM khor3CuLT in P21/n #14
REM R1 = 0.0623 for 9143 Fo > 4sig(Fo) and 0.0744 for all 10976 data
REM 849 parameters refined using 86 restraints
END
WGHT 0.0654 7.9201
REM Highest difference peak 0.949, deepest hole -0.711, 1-sigma level 0.061
Q1 1 0.3045 0.8862 0.2026 11.00000 0.05 0.95
Q2 1 0.8050 0.2458 0.1615 11.00000 0.05 0.92
Q3 1 0.9682 0.4535 0.1632 11.00000 0.05 0.90
Q4 1 0.2456 1.1152 0.2018 11.00000 0.05 0.76
Q5 1 0.0794 1.0603 0.1906 11.00000 0.05 0.63
Q6 1 0.1155 0.8288 0.1897 11.00000 0.05 0.63
Q7 1 0.9374 0.5337 0.2403 11.00000 0.05 0.49
Q8 1 0.2356 0.7760 0.1916 11.00000 0.05 0.37
Q9 1 0.9989 0.6307 0.2237 11.00000 0.05 0.36
Q10 1 0.6926 -0.3229 0.0814 11.00000 0.05 0.34
Q11 1 1.0242 0.7198 0.2701 11.00000 0.05 0.34
Q12 1 0.6412 -0.0633 0.0722 11.00000 0.05 0.31
Q13 1 0.5942 0.0807 0.0792 11.00000 0.05 0.31
Q14 1 0.4997 0.1363 0.1397 11.00000 0.05 0.30
Q15 1 0.5461 0.2751 0.1413 11.00000 0.05 0.30
Q16 1 0.7604 0.5579 0.2250 11.00000 0.05 0.27
Q17 1 0.8309 0.4954 0.2180 11.00000 0.05 0.27
Q18 1 0.3572 0.7559 0.2453 11.00000 0.05 0.26
Q19 1 0.7992 0.4622 0.1984 11.00000 0.05 0.24
Q20 1 0.7240 -0.1579 0.0961 11.00000 0.05 0.24
;
_shelx_res_checksum 38288
_olex2_date_sample_data_collection 2018-11-06
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.558
_oxdiff_exptl_absorpt_empirical_full_min 0.671
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_preparation Luminescent
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_khor2a
_database_code_depnum_ccdc_archive 'CCDC 1917741'
loop_
_audit_author_name
_audit_author_address
'Michidmaa Khorloo'
;Hong Kong University of Science and Technology
Hong Kong
;
_audit_update_record
;
2019-05-22 deposited with the CCDC. 2019-12-11 downloaded from the CCDC.
;
_audit_creation_date 2018-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common TPE-Py
_chemical_name_systematic TPE-EP-Y
_chemical_formula_moiety 'F6 P, C34 H28 N'
_chemical_formula_sum 'C34 H28 F6 N P'
_chemical_formula_weight 595.54
_chemical_melting_point ?
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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
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'
_cell_length_a 24.8939(7)
_cell_length_b 9.1783(2)
_cell_length_c 12.5794(3)
_cell_angle_alpha 90
_cell_angle_beta 98.168(3)
_cell_angle_gamma 90
_cell_volume 2845.01(13)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 6010
_cell_measurement_temperature 100.01(10)
_cell_measurement_theta_max 73.6250
_cell_measurement_theta_min 5.1320
_shelx_estimated_absorpt_T_max 0.972
_shelx_estimated_absorpt_T_min 0.764
_exptl_absorpt_coefficient_mu 1.422
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.84224
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.390
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 1232
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.02
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0309
_diffrn_reflns_av_unetI/netI 0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.914
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max 28
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 14173
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full 66.500
_diffrn_reflns_theta_max 67.499
_diffrn_reflns_theta_min 5.386
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.01(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w 82.00 138.00 1.00 20.00 -- 106.99 -30.00 -60.00 56
2 \w -109.00 -14.00 1.00 8.00 -- -40.57 -37.00 0.00 95
3 \w -91.00 -2.00 1.00 8.00 -- -40.57 125.00-120.00 89
4 \w -67.00 36.00 1.00 8.00 -- -40.57 37.00-180.00 103
5 \w 78.00 158.00 1.00 20.00 -- 106.99 61.00 -90.00 80
6 \w 48.00 117.00 1.00 20.00 -- 106.99-125.00 -30.00 69
7 \w 31.00 138.00 1.00 20.00 -- 106.99 -30.00 90.00 107
8 \w 32.00 117.00 1.00 20.00 -- 106.99-125.00 120.00 85
9 \w 94.00 173.00 1.00 20.00 -- 106.99 125.00 90.00 79
10 \w 29.00 67.00 1.00 20.00 -- 106.99 -30.00 -60.00 38
11 \w 96.00 171.00 1.00 20.00 -- 106.99 125.00 150.00 75
12 \w 28.00 141.00 1.00 20.00 -- 106.99 -77.00 120.00 113
;
_diffrn_measurement_device 'kappa diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0309900000
_diffrn_orient_matrix_UB_12 -0.1428328000
_diffrn_orient_matrix_UB_13 -0.0298507000
_diffrn_orient_matrix_UB_21 -0.0530776000
_diffrn_orient_matrix_UB_22 0.0726909000
_diffrn_orient_matrix_UB_23 0.0221994000
_diffrn_orient_matrix_UB_31 -0.0114693000
_diffrn_orient_matrix_UB_32 0.0498615000
_diffrn_orient_matrix_UB_33 -0.1179998000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_current 0.80
_diffrn_source_power 0.040
_diffrn_source_target Cu
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage 50
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4216
_reflns_number_total 4687
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max 0.949
_refine_diff_density_min -0.426
_refine_diff_density_rms 0.103
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.019
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 389
_refine_ls_number_reflns 4687
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0932
_refine_ls_R_factor_gt 0.0869
_refine_ls_restrained_S_all 1.019
_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^)+(0.0980P)^2^+11.2920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2128
_refine_ls_wR_factor_ref 0.2163
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(P1A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.003
3. Others
Fixed Sof: P1(0.9) P1A(0.1)
4.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C15(H15),
C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33),
C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
4.b Idealised Me refined as rotating group:
C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary iterative
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.08139(14) 0.2129(3) 0.1701(2) 0.0226(6) Uani 0.9 1 d . . P A 1
P1A P 0.0814(11) 0.242(3) 0.186(2) 0.018(5) Uani 0.1 1 d . U P . .
F1 F 0.12983(12) 0.0994(3) 0.1914(2) 0.0465(7) Uani 1 1 d . . . A 1
F2 F 0.03265(11) 0.3304(3) 0.1497(3) 0.0479(8) Uani 1 1 d . . . A 1
F3 F 0.07791(13) 0.1904(4) 0.0438(2) 0.0495(8) Uani 1 1 d . . . A 1
F4 F 0.12495(11) 0.3431(3) 0.1641(3) 0.0466(7) Uani 1 1 d . . . A 1
F5 F 0.08532(11) 0.2401(4) 0.2973(2) 0.0439(7) Uani 1 1 d . . . A 1
F6 F 0.03861(12) 0.0869(3) 0.1784(2) 0.0439(7) Uani 1 1 d . . . A 1
N1 N 0.05965(14) 0.7848(4) 0.5407(3) 0.0306(8) Uani 1 1 d . . . . .
C1 C 0.0267(2) 0.7979(6) 0.6291(4) 0.0413(12) Uani 1 1 d . . . . .
H1A H -0.0119 0.7913 0.6000 0.062 Uiso 1 1 calc GR . . . .
H1B H 0.0339 0.8920 0.6651 0.062 Uiso 1 1 calc GR . . . .
H1C H 0.0361 0.7190 0.6809 0.062 Uiso 1 1 calc GR . . . .
C2 C 0.06888(17) 0.6535(5) 0.5000(4) 0.0327(10) Uani 1 1 d . . . . .
H2 H 0.0544 0.5692 0.5294 0.039 Uiso 1 1 calc R . . . .
C3 C 0.09889(18) 0.6385(5) 0.4166(4) 0.0322(10) Uani 1 1 d . . . . .
H3 H 0.1049 0.5446 0.3889 0.039 Uiso 1 1 calc R . . . .
C4 C 0.12034(16) 0.7617(5) 0.3731(3) 0.0293(9) Uani 1 1 d . . . . .
C5 C 0.10845(18) 0.8964(5) 0.4153(4) 0.0327(10) Uani 1 1 d . . . . .
H5 H 0.1213 0.9831 0.3861 0.039 Uiso 1 1 calc R . . . .
C6 C 0.07861(18) 0.9053(5) 0.4980(4) 0.0334(10) Uani 1 1 d . . . . .
H6 H 0.0711 0.9981 0.5260 0.040 Uiso 1 1 calc R . . . .
C7 C 0.15523(17) 0.7585(5) 0.2882(3) 0.0291(9) Uani 1 1 d . . . . .
H7 H 0.1594 0.8453 0.2490 0.035 Uiso 1 1 calc R . . . .
C8 C 0.18115(17) 0.6390(5) 0.2641(3) 0.0304(9) Uani 1 1 d . . . . .
H8 H 0.1745 0.5524 0.3014 0.036 Uiso 1 1 calc R . . . .
C10 C 0.33304(16) 0.5789(4) -0.0406(3) 0.0240(8) Uani 1 1 d . . . . .
C11 C 0.29371(16) 0.5971(5) 0.0380(3) 0.0251(8) Uani 1 1 d . . . . .
C12 C 0.25902(17) 0.7174(5) 0.0315(3) 0.0279(9) Uani 1 1 d . . . . .
H12 H 0.2606 0.7890 -0.0225 0.034 Uiso 1 1 calc R . . . .
C13 C 0.22202(17) 0.7325(5) 0.1043(3) 0.0273(9) Uani 1 1 d . . . . .
H13 H 0.1984 0.8143 0.0991 0.033 Uiso 1 1 calc R . . . .
C14 C 0.21921(17) 0.6287(5) 0.1851(3) 0.0293(9) Uani 1 1 d . . . . .
C15 C 0.25443(18) 0.5112(5) 0.1924(3) 0.0305(9) Uani 1 1 d . . . . .
H15 H 0.2534 0.4405 0.2473 0.037 Uiso 1 1 calc R . . . .
C16 C 0.29139(18) 0.4962(5) 0.1199(3) 0.0291(9) Uani 1 1 d . . . . .
H16 H 0.3155 0.4155 0.1264 0.035 Uiso 1 1 calc R . . . .
C20 C 0.33878(16) 0.4497(5) -0.0898(3) 0.0261(9) Uani 1 1 d . . . . .
C21 C 0.30054(17) 0.3282(4) -0.0760(3) 0.0251(8) Uani 1 1 d . . . . .
C22 C 0.24447(17) 0.3466(5) -0.0993(3) 0.0283(9) Uani 1 1 d . . . . .
H22 H 0.2301 0.4318 -0.1356 0.034 Uiso 1 1 calc R . . . .
C23 C 0.20957(17) 0.2407(5) -0.0695(4) 0.0345(10) Uani 1 1 d . . . . .
H23 H 0.1714 0.2535 -0.0855 0.041 Uiso 1 1 calc R . . . .
C24 C 0.23056(19) 0.1170(5) -0.0167(4) 0.0359(10) Uani 1 1 d . . . . .
H24 H 0.2068 0.0475 0.0077 0.043 Uiso 1 1 calc R . . . .
C25 C 0.28621(18) 0.0936(5) 0.0011(4) 0.0336(10) Uani 1 1 d . . . . .
H25 H 0.3004 0.0063 0.0348 0.040 Uiso 1 1 calc R . . . .
C26 C 0.32072(18) 0.1969(5) -0.0301(3) 0.0288(9) Uani 1 1 d . . . . .
H26 H 0.3587 0.1789 -0.0204 0.035 Uiso 1 1 calc R . . . .
C31 C 0.36572(16) 0.7118(4) -0.0579(3) 0.0239(8) Uani 1 1 d . . . . .
C32 C 0.36649(17) 0.7698(4) -0.1589(3) 0.0273(9) Uani 1 1 d . . . . .
H32 H 0.3467 0.7235 -0.2197 0.033 Uiso 1 1 calc R . . . .
C33 C 0.39614(18) 0.8958(5) -0.1723(4) 0.0307(9) Uani 1 1 d . . . . .
H33 H 0.3958 0.9358 -0.2421 0.037 Uiso 1 1 calc R . . . .
C34 C 0.42598(17) 0.9627(5) -0.0850(4) 0.0327(10) Uani 1 1 d . . . . .
H34 H 0.4470 1.0467 -0.0948 0.039 Uiso 1 1 calc R . . . .
C35 C 0.42510(17) 0.9067(5) 0.0171(4) 0.0306(9) Uani 1 1 d . . . . .
H35 H 0.4453 0.9527 0.0776 0.037 Uiso 1 1 calc R . . . .
C36 C 0.39433(17) 0.7825(5) 0.0308(4) 0.0278(9) Uani 1 1 d . . . . .
H36 H 0.3929 0.7459 0.1010 0.033 Uiso 1 1 calc R . . . .
C41 C 0.38469(17) 0.4127(4) -0.1508(3) 0.0261(9) Uani 1 1 d . . . . .
C42 C 0.37473(18) 0.3190(5) -0.2397(3) 0.0299(9) Uani 1 1 d . . . . .
H42 H 0.3387 0.2883 -0.2651 0.036 Uiso 1 1 calc R . . . .
C43 C 0.41777(19) 0.2708(5) -0.2909(3) 0.0300(9) Uani 1 1 d . . . . .
H43 H 0.4108 0.2075 -0.3510 0.036 Uiso 1 1 calc R . . . .
C44 C 0.46986(18) 0.3141(5) -0.2550(4) 0.0317(9) Uani 1 1 d . . . . .
H44 H 0.4989 0.2790 -0.2893 0.038 Uiso 1 1 calc R . . . .
C45 C 0.48022(18) 0.4088(5) -0.1690(4) 0.0346(10) Uani 1 1 d . . . . .
H45 H 0.5162 0.4411 -0.1458 0.041 Uiso 1 1 calc R . . . .
C46 C 0.43779(17) 0.4571(5) -0.1163(4) 0.0327(10) Uani 1 1 d . . . . .
H46 H 0.4452 0.5207 -0.0564 0.039 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0314(9) 0.0173(11) 0.0189(10) -0.0017(8) 0.0031(7) -0.0015(8)
P1A 0.015(6) 0.018(7) 0.022(7) -0.002(4) 0.003(4) -0.004(4)
F1 0.0477(16) 0.0426(17) 0.0525(17) 0.0144(14) 0.0191(13) 0.0145(13)
F2 0.0365(15) 0.0388(16) 0.067(2) 0.0008(15) 0.0016(13) 0.0068(13)
F3 0.0638(19) 0.0558(19) 0.0294(15) 0.0039(13) 0.0086(13) -0.0083(15)
F4 0.0384(15) 0.0395(17) 0.0618(19) 0.0039(14) 0.0073(13) -0.0102(12)
F5 0.0332(14) 0.0633(19) 0.0350(15) -0.0037(14) 0.0043(11) -0.0032(13)
F6 0.0462(15) 0.0387(16) 0.0484(16) 0.0002(13) 0.0125(12) -0.0130(13)
N1 0.0258(17) 0.041(2) 0.0246(17) 0.0044(15) 0.0030(14) 0.0035(15)
C1 0.038(2) 0.060(3) 0.028(2) 0.000(2) 0.0107(19) 0.004(2)
C2 0.031(2) 0.033(2) 0.034(2) 0.0058(19) 0.0037(18) 0.0005(18)
C3 0.036(2) 0.026(2) 0.034(2) -0.0013(18) 0.0026(18) 0.0035(18)
C4 0.0218(19) 0.037(2) 0.028(2) 0.0064(19) 0.0008(15) 0.0001(17)
C5 0.032(2) 0.027(2) 0.041(2) 0.0027(19) 0.0095(18) 0.0035(17)
C6 0.033(2) 0.032(2) 0.035(2) 0.0018(19) 0.0050(18) -0.0009(18)
C7 0.027(2) 0.028(2) 0.032(2) 0.0042(18) 0.0027(16) -0.0021(17)
C8 0.031(2) 0.030(2) 0.030(2) 0.0001(18) 0.0057(17) -0.0018(18)
C10 0.0281(19) 0.021(2) 0.0233(19) 0.0026(16) 0.0043(15) 0.0032(16)
C11 0.0241(19) 0.025(2) 0.025(2) -0.0017(16) 0.0018(15) -0.0007(16)
C12 0.028(2) 0.029(2) 0.027(2) -0.0002(17) 0.0046(16) 0.0021(16)
C13 0.026(2) 0.022(2) 0.033(2) 0.0014(17) 0.0035(16) 0.0040(16)
C14 0.028(2) 0.032(2) 0.027(2) -0.0021(18) 0.0048(16) -0.0054(17)
C15 0.042(2) 0.025(2) 0.025(2) -0.0014(17) 0.0064(17) -0.0015(18)
C16 0.038(2) 0.022(2) 0.027(2) -0.0006(17) 0.0033(17) 0.0038(17)
C20 0.028(2) 0.024(2) 0.026(2) 0.0017(16) 0.0031(16) -0.0005(16)
C21 0.035(2) 0.0176(19) 0.0228(19) -0.0012(16) 0.0047(16) -0.0032(16)
C22 0.032(2) 0.020(2) 0.033(2) -0.0023(17) 0.0028(17) -0.0020(16)
C23 0.021(2) 0.034(2) 0.048(3) -0.003(2) 0.0021(17) -0.0047(17)
C24 0.041(2) 0.028(2) 0.038(2) -0.0007(19) 0.0036(19) -0.0115(19)
C25 0.039(2) 0.022(2) 0.038(2) 0.0009(18) 0.0019(19) -0.0022(18)
C26 0.033(2) 0.021(2) 0.032(2) -0.0008(17) 0.0033(17) 0.0054(16)
C31 0.0250(19) 0.021(2) 0.0256(19) -0.0021(15) 0.0048(15) 0.0025(15)
C32 0.027(2) 0.022(2) 0.034(2) 0.0010(17) 0.0066(16) -0.0016(16)
C33 0.036(2) 0.023(2) 0.035(2) 0.0042(17) 0.0101(18) 0.0035(17)
C34 0.028(2) 0.023(2) 0.048(3) -0.0009(19) 0.0095(18) 0.0006(16)
C35 0.029(2) 0.024(2) 0.039(2) -0.0066(18) 0.0056(17) 0.0011(17)
C36 0.028(2) 0.026(2) 0.030(2) -0.0060(17) 0.0076(16) 0.0029(16)
C41 0.031(2) 0.021(2) 0.027(2) 0.0008(16) 0.0063(16) 0.0035(16)
C42 0.033(2) 0.026(2) 0.031(2) -0.0020(18) 0.0059(17) -0.0020(18)
C43 0.040(2) 0.024(2) 0.027(2) -0.0018(17) 0.0097(17) -0.0002(18)
C44 0.033(2) 0.027(2) 0.037(2) 0.0057(19) 0.0141(18) 0.0059(18)
C45 0.028(2) 0.034(2) 0.041(2) -0.003(2) 0.0053(18) 0.0046(18)
C46 0.029(2) 0.034(2) 0.034(2) -0.0022(19) 0.0009(17) 0.0040(18)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 F1 1.587(4) . ?
P1 F2 1.617(4) . ?
P1 F3 1.592(4) . ?
P1 F4 1.623(4) . ?
P1 F5 1.609(4) . ?
P1 F6 1.585(4) . ?
P1A F1 1.78(3) . ?
P1A F2 1.48(3) . ?
P1A F3 1.84(3) . ?
P1A F4 1.48(3) . ?
P1A F5 1.39(3) . ?
P1A F6 1.78(3) . ?
N1 C1 1.478(6) . ?
N1 C2 1.341(6) . ?
N1 C6 1.343(6) . ?
C2 C3 1.378(6) . ?
C3 C4 1.395(6) . ?
C4 C5 1.394(6) . ?
C4 C7 1.470(6) . ?
C5 C6 1.364(6) . ?
C7 C8 1.329(6) . ?
C8 C14 1.471(6) . ?
C10 C11 1.496(6) . ?
C10 C20 1.355(6) . ?
C10 C31 1.500(6) . ?
C11 C12 1.397(6) . ?
C11 C16 1.393(6) . ?
C12 C13 1.395(6) . ?
C13 C14 1.401(6) . ?
C14 C15 1.385(6) . ?
C15 C16 1.392(6) . ?
C20 C21 1.492(6) . ?
C20 C41 1.503(6) . ?
C21 C22 1.395(6) . ?
C21 C26 1.399(6) . ?
C22 C23 1.390(6) . ?
C23 C24 1.381(7) . ?
C24 C25 1.388(7) . ?
C25 C26 1.374(6) . ?
C31 C32 1.379(6) . ?
C31 C36 1.395(6) . ?
C32 C33 1.395(6) . ?
C33 C34 1.379(7) . ?
C34 C35 1.387(7) . ?
C35 C36 1.398(6) . ?
C41 C42 1.405(6) . ?
C41 C46 1.393(6) . ?
C42 C43 1.397(6) . ?
C43 C44 1.370(7) . ?
C44 C45 1.383(7) . ?
C45 C46 1.397(6) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 P1 F2 179.0(3) . . ?
F1 P1 F3 90.9(2) . . ?
F1 P1 F4 89.7(2) . . ?
F1 P1 F5 89.8(2) . . ?
F2 P1 F4 89.6(2) . . ?
F3 P1 F2 89.7(2) . . ?
F3 P1 F4 89.5(2) . . ?
F3 P1 F5 178.5(3) . . ?
F5 P1 F2 89.6(2) . . ?
F5 P1 F4 89.2(2) . . ?
F6 P1 F1 90.7(2) . . ?
F6 P1 F2 90.1(2) . . ?
F6 P1 F3 91.7(2) . . ?
F6 P1 F4 178.8(3) . . ?
F6 P1 F5 89.7(2) . . ?
F1 P1A F3 77.5(10) . . ?
F2 P1A F1 160.0(17) . . ?
F2 P1A F3 85.3(13) . . ?
F2 P1A F4 101.1(16) . . ?
F2 P1A F6 87.8(14) . . ?
F4 P1A F1 87.6(14) . . ?
F4 P1A F3 85.1(13) . . ?
F4 P1A F6 160.3(17) . . ?
F5 P1A F1 90.1(15) . . ?
F5 P1A F2 104.9(17) . . ?
F5 P1A F3 164.0(18) . . ?
F5 P1A F4 104.5(16) . . ?
F5 P1A F6 89.9(15) . . ?
F6 P1A F1 78.8(10) . . ?
F6 P1A F3 78.1(9) . . ?
P1 F1 P1A 9.6(9) . . ?
P1A F2 P1 11.4(9) . . ?
P1 F3 P1A 7.6(9) . . ?
P1A F4 P1 11.3(10) . . ?
P1A F5 P1 9.8(11) . . ?
P1 F6 P1A 9.5(9) . . ?
C2 N1 C1 120.2(4) . . ?
C2 N1 C6 119.9(4) . . ?
C6 N1 C1 119.8(4) . . ?
N1 C2 C3 121.4(4) . . ?
C2 C3 C4 119.8(4) . . ?
C3 C4 C7 124.6(4) . . ?
C5 C4 C3 117.1(4) . . ?
C5 C4 C7 118.3(4) . . ?
C6 C5 C4 120.8(4) . . ?
N1 C6 C5 121.0(4) . . ?
C8 C7 C4 122.5(4) . . ?
C7 C8 C14 126.0(4) . . ?
C11 C10 C31 115.1(3) . . ?
C20 C10 C11 121.4(4) . . ?
C20 C10 C31 123.4(4) . . ?
C12 C11 C10 120.5(4) . . ?
C16 C11 C10 121.0(4) . . ?
C16 C11 C12 118.6(4) . . ?
C13 C12 C11 120.0(4) . . ?
C12 C13 C14 120.9(4) . . ?
C13 C14 C8 123.3(4) . . ?
C15 C14 C8 117.9(4) . . ?
C15 C14 C13 118.8(4) . . ?
C14 C15 C16 120.3(4) . . ?
C15 C16 C11 121.3(4) . . ?
C10 C20 C21 119.3(4) . . ?
C10 C20 C41 124.6(4) . . ?
C21 C20 C41 115.8(4) . . ?
C22 C21 C20 121.4(4) . . ?
C22 C21 C26 118.7(4) . . ?
C26 C21 C20 119.6(4) . . ?
C23 C22 C21 120.3(4) . . ?
C24 C23 C22 119.8(4) . . ?
C23 C24 C25 120.4(4) . . ?
C26 C25 C24 119.8(4) . . ?
C25 C26 C21 120.7(4) . . ?
C32 C31 C10 121.8(4) . . ?
C32 C31 C36 119.0(4) . . ?
C36 C31 C10 119.2(4) . . ?
C31 C32 C33 120.5(4) . . ?
C34 C33 C32 120.5(4) . . ?
C33 C34 C35 119.7(4) . . ?
C34 C35 C36 119.8(4) . . ?
C31 C36 C35 120.5(4) . . ?
C42 C41 C20 118.9(4) . . ?
C46 C41 C20 122.1(4) . . ?
C46 C41 C42 118.7(4) . . ?
C43 C42 C41 120.0(4) . . ?
C44 C43 C42 120.6(4) . . ?
C43 C44 C45 120.2(4) . . ?
C44 C45 C46 120.1(4) . . ?
C41 C46 C45 120.4(4) . . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F1 P1 F3 P1A -134(8) . . . . ?
F1 P1 F4 P1A -125(6) . . . . ?
F1 P1 F5 P1A 134(8) . . . . ?
F1 P1 F6 P1A 125(6) . . . . ?
F1 P1A F2 P1 0.6(5) . . . . ?
F1 P1A F3 P1 41(7) . . . . ?
F1 P1A F4 P1 47(5) . . . . ?
F1 P1A F5 P1 -40(7) . . . . ?
F1 P1A F6 P1 -49(6) . . . . ?
F2 P1 F3 P1A 45(7) . . . . ?
F2 P1 F4 P1A 55(6) . . . . ?
F2 P1 F5 P1A -45(7) . . . . ?
F2 P1 F6 P1A -55(6) . . . . ?
F2 P1A F1 P1 -0.7(6) . . . . ?
F2 P1A F3 P1 -129(8) . . . . ?
F2 P1A F4 P1 -115(7) . . . . ?
F2 P1A F5 P1 127(8) . . . . ?
F2 P1A F6 P1 116(7) . . . . ?
F3 P1 F1 P1A 143(6) . . . . ?
F3 P1 F2 P1A -144(6) . . . . ?
F3 P1 F4 P1A 144(6) . . . . ?
F3 P1 F6 P1A -145(6) . . . . ?
F3 P1A F1 P1 -32(5) . . . . ?
F3 P1A F2 P1 31(5) . . . . ?
F3 P1A F4 P1 -30(5) . . . . ?
F3 P1A F5 P1 -1.4(6) . . . . ?
F3 P1A F6 P1 31(5) . . . . ?
F4 P1 F1 P1A 54(6) . . . . ?
F4 P1 F2 P1A -54(6) . . . . ?
F4 P1 F3 P1A -44(7) . . . . ?
F4 P1 F5 P1A 45(7) . . . . ?
F4 P1A F1 P1 -117(7) . . . . ?
F4 P1A F2 P1 115(7) . . . . ?
F4 P1A F3 P1 130(8) . . . . ?
F4 P1A F5 P1 -127(8) . . . . ?
F4 P1A F6 P1 -1.2(6) . . . . ?
F5 P1 F1 P1A -35(6) . . . . ?
F5 P1 F2 P1A 35(6) . . . . ?
F5 P1 F4 P1A -35(6) . . . . ?
F5 P1 F6 P1A 35(6) . . . . ?
F5 P1A F1 P1 138(7) . . . . ?
F5 P1A F2 P1 -137(7) . . . . ?
F5 P1A F3 P1 1.8(8) . . . . ?
F5 P1A F4 P1 137(7) . . . . ?
F5 P1A F6 P1 -139(7) . . . . ?
F6 P1 F1 P1A -125(6) . . . . ?
F6 P1 F2 P1A 125(6) . . . . ?
F6 P1 F3 P1A 135(8) . . . . ?
F6 P1 F5 P1A -135(8) . . . . ?
F6 P1A F1 P1 48(6) . . . . ?
F6 P1A F2 P1 -47(5) . . . . ?
F6 P1A F3 P1 -40(7) . . . . ?
F6 P1A F4 P1 1.0(5) . . . . ?
F6 P1A F5 P1 39(7) . . . . ?
N1 C2 C3 C4 0.1(6) . . . . ?
C1 N1 C2 C3 179.1(4) . . . . ?
C1 N1 C6 C5 -179.0(4) . . . . ?
C2 N1 C6 C5 -1.7(6) . . . . ?
C2 C3 C4 C5 -2.0(6) . . . . ?
C2 C3 C4 C7 176.6(4) . . . . ?
C3 C4 C5 C6 2.2(6) . . . . ?
C3 C4 C7 C8 -18.1(7) . . . . ?
C4 C5 C6 N1 -0.4(7) . . . . ?
C4 C7 C8 C14 -176.2(4) . . . . ?
C5 C4 C7 C8 160.6(4) . . . . ?
C6 N1 C2 C3 1.8(6) . . . . ?
C7 C4 C5 C6 -176.6(4) . . . . ?
C7 C8 C14 C13 -18.1(7) . . . . ?
C7 C8 C14 C15 160.9(4) . . . . ?
C8 C14 C15 C16 -179.8(4) . . . . ?
C10 C11 C12 C13 179.2(4) . . . . ?
C10 C11 C16 C15 -179.1(4) . . . . ?
C10 C20 C21 C22 54.5(6) . . . . ?
C10 C20 C21 C26 -120.0(5) . . . . ?
C10 C20 C41 C42 -147.4(4) . . . . ?
C10 C20 C41 C46 38.7(6) . . . . ?
C10 C31 C32 C33 178.3(4) . . . . ?
C10 C31 C36 C35 -179.9(4) . . . . ?
C11 C10 C20 C21 7.6(6) . . . . ?
C11 C10 C20 C41 -166.5(4) . . . . ?
C11 C10 C31 C32 -124.6(4) . . . . ?
C11 C10 C31 C36 52.6(5) . . . . ?
C11 C12 C13 C14 0.4(6) . . . . ?
C12 C11 C16 C15 1.9(6) . . . . ?
C12 C13 C14 C8 179.8(4) . . . . ?
C12 C13 C14 C15 0.9(6) . . . . ?
C13 C14 C15 C16 -0.8(6) . . . . ?
C14 C15 C16 C11 -0.6(6) . . . . ?
C16 C11 C12 C13 -1.8(6) . . . . ?
C20 C10 C11 C12 -133.4(4) . . . . ?
C20 C10 C11 C16 47.6(6) . . . . ?
C20 C10 C31 C32 56.7(6) . . . . ?
C20 C10 C31 C36 -126.0(4) . . . . ?
C20 C21 C22 C23 -169.5(4) . . . . ?
C20 C21 C26 C25 168.3(4) . . . . ?
C20 C41 C42 C43 -173.3(4) . . . . ?
C20 C41 C46 C45 173.7(4) . . . . ?
C21 C20 C41 C42 38.3(5) . . . . ?
C21 C20 C41 C46 -135.5(4) . . . . ?
C21 C22 C23 C24 0.0(7) . . . . ?
C22 C21 C26 C25 -6.3(6) . . . . ?
C22 C23 C24 C25 -3.9(7) . . . . ?
C23 C24 C25 C26 2.7(7) . . . . ?
C24 C25 C26 C21 2.5(7) . . . . ?
C26 C21 C22 C23 5.0(6) . . . . ?
C31 C10 C11 C12 47.9(5) . . . . ?
C31 C10 C11 C16 -131.1(4) . . . . ?
C31 C10 C20 C21 -173.8(4) . . . . ?
C31 C10 C20 C41 12.1(6) . . . . ?
C31 C32 C33 C34 1.3(6) . . . . ?
C32 C31 C36 C35 -2.6(6) . . . . ?
C32 C33 C34 C35 -2.0(6) . . . . ?
C33 C34 C35 C36 0.5(6) . . . . ?
C34 C35 C36 C31 1.9(6) . . . . ?
C36 C31 C32 C33 1.1(6) . . . . ?
C41 C20 C21 C22 -131.0(4) . . . . ?
C41 C20 C21 C26 54.6(5) . . . . ?
C41 C42 C43 C44 0.1(7) . . . . ?
C42 C41 C46 C45 -0.2(7) . . . . ?
C42 C43 C44 C45 -1.5(7) . . . . ?
C43 C44 C45 C46 2.0(7) . . . . ?
C44 C45 C46 C41 -1.2(7) . . . . ?
C46 C41 C42 C43 0.7(6) . . . . ?
_shelx_res_file
;
khor2a.res created by SHELXL-2014/7
TITL khor2a in P2(1)/c 100K
CELL 1.54184 24.893871 9.178269 12.579357 90 98.1675 90
ZERR 4 0.000728 0.000227 0.000305 0 0.0025 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H F N P
UNIT 136 112 24 4 4
ISOR 0.005 0.003 P1A
L.S. 10
PLAN 20
SIZE 0.02 0.08 0.2
TEMP -173
CONF
fmap 2
acta 133
OMIT 0 135
OMIT -5 1 2
OMIT 5 4 9
OMIT 0 3 2
OMIT -3 1 9
OMIT -6 1 2
OMIT 4 4 2
OMIT -14 4 2
OMIT -6 0 2
OMIT 3 5 7
OMIT -13 2 7
OMIT -7 0 2
OMIT 15 2 2
OMIT -8 0 2
OMIT -18 4 7
OMIT -10 4 7
OMIT -3 4 5
OMIT -4 3 9
OMIT -4 7 9
OMIT -9 0 2
OMIT 5 6 9
OMIT -8 5 7
OMIT -8 1 2
OMIT -16 4 7
OMIT -5 7 2
OMIT -22 3 9
OMIT 1 1 9
OMIT -1 8 9
OMIT 2 2 5
OMIT -16 2 9
OMIT -2 3 2
OMIT -9 7 7
OMIT -9 1 2
OMIT -19 3 7
OMIT 0 9 2
OMIT 8 3 7
OMIT -6 3 7
OMIT -9 1 14
OMIT 7 5 7
OMIT 11 4 2
OMIT -14 3 5
OMIT 1 1 0
OMIT -8 6 9
OMIT 5 4 2
OMIT 2 4 9
OMIT -3 8 7
OMIT -13 0 2
OMIT 6 1 2
OMIT 0 6 2
OMIT -4 8 11
OMIT -3 2 9
OMIT 2 1 0
OMIT 2 0 0
OMIT 3 1 0
OMIT -12 1 2
OMIT 5 5 7
OMIT -7 8 5
OMIT 6 5 5
OMIT 14 6 7
OMIT 0 1 2
OMIT -3 5 9
OMIT 3 6 7
OMIT 2 3 11
OMIT 1 10 7
OMIT 0 1 14
OMIT -1 4 11
OMIT 12 1 2
OMIT -11 1 14
OMIT 4 4 7
OMIT 8 9 2
OMIT -1 2 9
OMIT 5 5 11
OMIT -13 6 9
OMIT 13 1 7
OMIT 4 2 9
OMIT -10 7 2
OMIT 1 8 7
OMIT -5 2 11
OMIT -6 1 7
OMIT 5 2 11
OMIT 11 5 7
OMIT -3 1 13
OMIT 9 3 7
OMIT -8 7 5
OMIT 17 0 2
OMIT -7 6 5
OMIT -19 5 7
OMIT 7 4 11
OMIT -7 9 7
OMIT 2 3 9
OMIT 8 6 7
OMIT -10 6 7
OMIT 17 1 7
OMIT -3 0 4
OMIT 10 5 7
OMIT 6 3 14
OMIT -20 6 7
OMIT -24 1 7
OMIT -8 3 2
OMIT 7 3 7
OMIT -11 6 11
OMIT -9 6 4
OMIT -17 2 7
OMIT 2 4 7
OMIT 9 1 2
OMIT -1 8 5
OMIT 2 7 9
OMIT 1 6 2
OMIT -1 1 7
OMIT -8 1 9
OMIT -16 6 7
OMIT -5 7 9
OMIT 3 4 2
OMIT -5 9 5
OMIT -8 0 14
OMIT 1 3 9
OMIT 10 4 7
OMIT 11 2 2
OMIT 14 1 9
OMIT -11 5 9
OMIT 11 1 7
OMIT 9 3 2
OMIT 0 6 9
OMIT -14 2 14
OMIT 6 1 9
OMIT 8 5 2
OMIT -12 3 2
OMIT -16 5 9
OMIT 0 6 5
OMIT 5 2 0
OMIT -15 3 7
OMIT -18 2 7
OMIT -3 3 14
OMIT 3 1 11
OMIT -13 6 7
OMIT 6 5 7
OMIT -9 1 9
OMIT -12 5 7
OMIT 1 9 5
OMIT -11 4 7
OMIT -16 7 9
OMIT -15 2 14
OMIT 13 5 2
OMIT -10 8 7
OMIT -11 1 7
OMIT -9 2 14
OMIT 2 1 4
OMIT 9 4 2
OMIT 6 3 2
OMIT 5 1 11
OMIT -3 7 9
OMIT 15 4 9
OMIT -5 3 12
OMIT -1 4 9
OMIT 18 3 7
OMIT -4 1 1
OMIT -2 10 2
OMIT 25 4 2
OMIT 22 0 2
OMIT -10 5 5
OMIT 5 3 7
OMIT 12 3 7
OMIT 4 10 5
OMIT 4 5 2
OMIT 8 7 9
OMIT 14 8 7
OMIT 17 4 2
OMIT -5 8 2
OMIT 3 4 7
OMIT -10 6 5
OMIT -2 6 10
OMIT 4 3 0
OMIT -6 2 13
OMIT -6 10 2
OMIT -6 2 2
OMIT 2 2 2
OMIT -9 4 14
OMIT 17 2 2
OMIT 11 8 2
OMIT 18 2 9
OMIT 0 1 7
OMIT -22 5 7
OMIT -14 6 5
OMIT -9 7 9
OMIT -15 6 7
OMIT -1 4 12
OMIT -3 7 5
OMIT 2 6 9
OMIT 16 1 2
OMIT 22 4 2
OMIT 8 5 9
OMIT -10 8 5
OMIT -5 9 2
OMIT -3 0 2
OMIT -11 4 4
OMIT 6 6 9
OMIT -19 7 7
OMIT -25 1 7
OMIT -19 2 7
OMIT -3 2 4
OMIT -8 2 13
OMIT -9 6 7
OMIT 7 6 9
OMIT -8 7 3
OMIT -11 10 4
OMIT -4 2 5
OMIT -4 9 9
OMIT -18 4 9
OMIT -13 1 9
OMIT 1 4 9
OMIT 20 3 9
OMIT 24 3 2
OMIT -6 3 4
OMIT -3 6 7
OMIT 9 0 2
OMIT 18 2 2
OMIT -9 3 11
OMIT -1 5 7
OMIT -4 8 2
OMIT -23 1 9
OMIT -20 0 2
OMIT -15 4 5
OMIT 10 6 7
OMIT -18 1 11
OMIT -10 6 2
OMIT -3 7 3
OMIT -19 2 11
OMIT -6 1 14
OMIT -13 8 5
OMIT 1 7 5
OMIT 7 8 7
OMIT -7 2 2
OMIT -15 1 2
OMIT -26 3 7
OMIT -3 10 2
OMIT 15 7 2
OMIT 23 1 2
OMIT 12 6 2
OMIT 4 1 0
OMIT -9 1 4
OMIT -19 3 2
OMIT -6 5 2
OMIT -6 3 5
OMIT -5 9 3
OMIT 1 1 2
OMIT 3 6 11
OMIT 24 1 2
OMIT -12 5 5
OMIT 8 6 11
OMIT -4 2 2
OMIT -11 3 9
OMIT -12 9 7
OMIT 14 3 9
OMIT 6 2 0
OMIT -8 8 7
OMIT -1 4 2
OMIT 14 2 2
OMIT -18 5 7
OMIT -5 1 14
OMIT 12 5 7
OMIT 15 0 2
OMIT -1 6 11
OMIT 0 1 9
OMIT 8 4 2
OMIT 4 2 11
OMIT -12 2 9
OMIT 10 7 7
OMIT 8 3 2
OMIT -11 5 12
OMIT 7 4 0
OMIT 4 3 7
OMIT -6 4 4
OMIT 2 0 4
OMIT 2 1 2
OMIT 2 10 5
OMIT -8 7 2
OMIT -6 6 5
OMIT -8 5 11
OMIT -2 8 9
OMIT 14 7 5
OMIT 0 4 3
OMIT -13 4 9
OMIT -7 8 9
OMIT -13 8 7
OMIT 5 11 2
OMIT 8 3 9
OMIT 12 3 2
OMIT 4 1 11
OMIT 13 7 9
OMIT 12 5 2
OMIT 0 10 2
OMIT 7 0 4
OMIT -8 9 2
OMIT 0 5 5
OMIT 1 8 2
OMIT -10 7 9
OMIT -3 8 5
OMIT -5 2 9
OMIT -27 2 2
OMIT 19 1 2
OMIT -6 8 7
OMIT 0 6 4
OMIT 15 6 7
OMIT 1 10 5
OMIT 16 0 2
OMIT -22 1 5
OMIT 2 7 2
OMIT -27 2 7
OMIT -12 5 2
OMIT 8 2 2
OMIT -8 4 2
OMIT 4 0 12
OMIT -8 6 5
OMIT 10 2 2
OMIT -2 3 13
OMIT 7 6 2
OMIT 1 6 5
OMIT -21 5 9
OMIT 6 5 1
OMIT -1 1 4
OMIT 2 3 0
OMIT -12 4 5
OMIT -8 5 2
OMIT -5 2 1
OMIT -9 9 5
OMIT -4 5 5
OMIT 5 3 11
OMIT 1 9 1
OMIT -7 2 7
OMIT 10 3 0
OMIT 12 2 0
OMIT -2 7 2
OMIT -10 5 2
OMIT -1 2 2
OMIT -21 4 9
OMIT -1 5 2
OMIT -1 5 11
OMIT 2 2 0
OMIT -20 3 9
OMIT 15 3 5
OMIT -11 7 9
OMIT -8 2 3
OMIT -9 1 10
OMIT -15 5 5
OMIT -10 2 2
OMIT -21 7 2
OMIT 2 6 7
OMIT -12 8 3
OMIT 2 1 9
OMIT -6 1 11
OMIT 3 0 4
OMIT -17 3 9
OMIT -5 3 4
OMIT -9 3 4
OMIT 13 3 2
OMIT -12 4 4
OMIT 3 7 4
OMIT 6 1 4
OMIT 2 4 2
OMIT -15 3 2
OMIT -2 7 3
OMIT -3 8 1
OMIT -3 4 4
OMIT -5 4 5
OMIT -13 1 4
OMIT 0 4 4
OMIT -14 1 2
OMIT 19 7 5
OMIT -11 1 4
OMIT -5 3 5
OMIT 5 4 5
OMIT -12 7 4
OMIT 1 3 10
OMIT -7 7 11
OMIT -2 5 2
OMIT -9 5 3
OMIT 0 0 12
OMIT -9 7 3
OMIT 10 5 2
OMIT 2 4 12
OMIT 0 10 3
OMIT -13 5 11
OMIT -4 1 2
OMIT -11 7 4
OMIT -3 10 4
OMIT 8 4 5
OMIT -3 1 12
OMIT -4 3 4
OMIT 11 0 0
OMIT 10 4 1
OMIT -6 1 5
OMIT 4 2 2
OMIT 27 1 0
OMIT -1 10 1
OMIT -1 7 5
OMIT -5 7 3
OMIT -6 0 12
OMIT 0 7 1
OMIT -20 6 5
OMIT 3 4 3
OMIT -7 1 12
OMIT -17 6 5
OMIT -7 7 2
OMIT -3 3 4
OMIT 0 2 0
OMIT 3 1 12
OMIT -9 2 7
OMIT -23 2 2
OMIT 5 8 5
OMIT 8 4 7
OMIT 1 2 0
OMIT -6 3 2
OMIT 4 5 5
OMIT 3 4 11
OMIT 12 1 0
OMIT -21 2 2
OMIT -1 8 2
OMIT -2 5 10
OMIT 9 5 3
OMIT 1 2 2
OMIT -7 5 2
OMIT 5 1 0
OMIT 0 1 1
OMIT 4 3 2
OMIT -6 8 1
OMIT 22 2 5
OMIT 27 0 0
OMIT -1 6 9
OMIT -16 5 3
OMIT -5 7 5
OMIT 3 3 9
OMIT 5 0 0
OMIT -3 1 4
OMIT 4 9 4
OMIT 4 6 2
OMIT -10 1 4
REM
REM
REM
WGHT 0.098000 11.292000
FVAR 3.64853
PART 1
P1 5 0.081390 0.212860 0.170080 10.90000 0.03141 0.01734 =
0.01885 -0.00171 0.00308 -0.00150
PART 0
P1A 5 0.081445 0.242469 0.186089 10.10000 0.01520 0.01770 =
0.02191 -0.00236 0.00265 -0.00418
PART 1
F1 3 0.129828 0.099365 0.191372 11.00000 0.04774 0.04264 =
0.05246 0.01436 0.01914 0.01450
F2 3 0.032647 0.330428 0.149716 11.00000 0.03646 0.03884 =
0.06675 0.00081 0.00161 0.00678
F3 3 0.077914 0.190357 0.043775 11.00000 0.06376 0.05583 =
0.02938 0.00387 0.00858 -0.00826
F4 3 0.124948 0.343146 0.164073 11.00000 0.03844 0.03947 =
0.06181 0.00386 0.00727 -0.01016
F5 3 0.085321 0.240092 0.297328 11.00000 0.03323 0.06333 =
0.03503 -0.00373 0.00433 -0.00318
F6 3 0.038610 0.086876 0.178393 11.00000 0.04617 0.03868 =
0.04837 0.00016 0.01245 -0.01304
PART 0
N1 4 0.059652 0.784796 0.540667 11.00000 0.02584 0.04130 =
0.02460 0.00441 0.00297 0.00348
C1 1 0.026677 0.797868 0.629088 11.00000 0.03819 0.05953 =
0.02792 -0.00045 0.01074 0.00443
AFIX 137
H1A 2 -0.011907 0.791314 0.599967 11.00000 -1.50000
H1B 2 0.033935 0.891986 0.665060 11.00000 -1.50000
H1C 2 0.036139 0.718972 0.680860 11.00000 -1.50000
AFIX 0
C2 1 0.068884 0.653545 0.500044 11.00000 0.03134 0.03302 =
0.03357 0.00583 0.00374 0.00051
AFIX 43
H2 2 0.054447 0.569167 0.529351 11.00000 -1.20000
AFIX 0
C3 1 0.098888 0.638534 0.416644 11.00000 0.03612 0.02592 =
0.03395 -0.00133 0.00262 0.00351
AFIX 43
H3 2 0.104934 0.544617 0.388892 11.00000 -1.20000
AFIX 0
C4 1 0.120342 0.761685 0.373135 11.00000 0.02184 0.03698 =
0.02841 0.00644 0.00078 0.00007
C5 1 0.108448 0.896409 0.415323 11.00000 0.03198 0.02672 =
0.04055 0.00267 0.00949 0.00350
AFIX 43
H5 2 0.121270 0.983058 0.386133 11.00000 -1.20000
AFIX 0
C6 1 0.078606 0.905261 0.498047 11.00000 0.03330 0.03158 =
0.03533 0.00179 0.00503 -0.00089
AFIX 43
H6 2 0.071111 0.998085 0.525954 11.00000 -1.20000
AFIX 0
C7 1 0.155225 0.758548 0.288220 11.00000 0.02723 0.02795 =
0.03182 0.00419 0.00274 -0.00207
AFIX 43
H7 2 0.159409 0.845287 0.249012 11.00000 -1.20000
AFIX 0
C8 1 0.181149 0.639048 0.264150 11.00000 0.03104 0.03016 =
0.03039 0.00013 0.00573 -0.00183
AFIX 43
H8 2 0.174493 0.552375 0.301446 11.00000 -1.20000
AFIX 0
C10 1 0.333039 0.578880 -0.040573 11.00000 0.02808 0.02086 =
0.02332 0.00256 0.00428 0.00322
C11 1 0.293714 0.597069 0.037993 11.00000 0.02411 0.02538 =
0.02537 -0.00168 0.00180 -0.00074
C12 1 0.259025 0.717385 0.031532 11.00000 0.02814 0.02851 =
0.02738 -0.00023 0.00463 0.00205
AFIX 43
H12 2 0.260640 0.788969 -0.022469 11.00000 -1.20000
AFIX 0
C13 1 0.222017 0.732481 0.104324 11.00000 0.02620 0.02241 =
0.03305 0.00143 0.00345 0.00402
AFIX 43
H13 2 0.198394 0.814257 0.099099 11.00000 -1.20000
AFIX 0
C14 1 0.219206 0.628680 0.185053 11.00000 0.02838 0.03222 =
0.02739 -0.00209 0.00476 -0.00545
C15 1 0.254428 0.511154 0.192449 11.00000 0.04244 0.02490 =
0.02470 -0.00140 0.00635 -0.00145
AFIX 43
H15 2 0.253351 0.440461 0.247268 11.00000 -1.20000
AFIX 0
C16 1 0.291393 0.496166 0.119923 11.00000 0.03807 0.02203 =
0.02692 -0.00061 0.00329 0.00379
AFIX 43
H16 2 0.315537 0.415472 0.126424 11.00000 -1.20000
AFIX 0
C20 1 0.338783 0.449697 -0.089794 11.00000 0.02799 0.02440 =
0.02568 0.00170 0.00313 -0.00049
C21 1 0.300541 0.328242 -0.075963 11.00000 0.03516 0.01760 =
0.02281 -0.00123 0.00473 -0.00320
C22 1 0.244474 0.346593 -0.099266 11.00000 0.03208 0.01972 =
0.03261 -0.00226 0.00276 -0.00195
AFIX 43
H22 2 0.230093 0.431809 -0.135618 11.00000 -1.20000
AFIX 0
C23 1 0.209568 0.240731 -0.069522 11.00000 0.02095 0.03415 =
0.04753 -0.00336 0.00208 -0.00474
AFIX 43
H23 2 0.171402 0.253457 -0.085500 11.00000 -1.20000
AFIX 0
C24 1 0.230565 0.117004 -0.016671 11.00000 0.04076 0.02807 =
0.03825 -0.00066 0.00361 -0.01153
AFIX 43
H24 2 0.206792 0.047489 0.007667 11.00000 -1.20000
AFIX 0
C25 1 0.286212 0.093578 0.001116 11.00000 0.03895 0.02235 =
0.03845 0.00090 0.00194 -0.00218
AFIX 43
H25 2 0.300387 0.006343 0.034785 11.00000 -1.20000
AFIX 0
C26 1 0.320722 0.196865 -0.030095 11.00000 0.03323 0.02103 =
0.03182 -0.00079 0.00327 0.00541
AFIX 43
H26 2 0.358687 0.178898 -0.020433 11.00000 -1.20000
AFIX 0
C31 1 0.365723 0.711836 -0.057927 11.00000 0.02505 0.02136 =
0.02558 -0.00214 0.00478 0.00251
C32 1 0.366493 0.769805 -0.158876 11.00000 0.02664 0.02166 =
0.03429 0.00102 0.00659 -0.00158
AFIX 43
H32 2 0.346674 0.723550 -0.219739 11.00000 -1.20000
AFIX 0
C33 1 0.396144 0.895820 -0.172309 11.00000 0.03626 0.02262 =
0.03455 0.00421 0.01007 0.00355
AFIX 43
H33 2 0.395777 0.935845 -0.242054 11.00000 -1.20000
AFIX 0
C34 1 0.425985 0.962686 -0.085018 11.00000 0.02832 0.02287 =
0.04796 -0.00087 0.00952 0.00063
AFIX 43
H34 2 0.447042 1.046672 -0.094811 11.00000 -1.20000
AFIX 0
C35 1 0.425096 0.906701 0.017114 11.00000 0.02908 0.02434 =
0.03855 -0.00657 0.00564 0.00113
AFIX 43
H35 2 0.445350 0.952651 0.077629 11.00000 -1.20000
AFIX 0
C36 1 0.394325 0.782502 0.030774 11.00000 0.02771 0.02636 =
0.03034 -0.00597 0.00757 0.00293
AFIX 43
H36 2 0.392871 0.745926 0.100956 11.00000 -1.20000
AFIX 0
C41 1 0.384688 0.412697 -0.150839 11.00000 0.03082 0.02123 =
0.02675 0.00078 0.00627 0.00346
C42 1 0.374729 0.318957 -0.239717 11.00000 0.03319 0.02583 =
0.03114 -0.00203 0.00590 -0.00200
AFIX 43
H42 2 0.338737 0.288287 -0.265059 11.00000 -1.20000
AFIX 0
C43 1 0.417767 0.270807 -0.290866 11.00000 0.04026 0.02432 =
0.02679 -0.00178 0.00971 -0.00021
AFIX 43
H43 2 0.410841 0.207523 -0.351013 11.00000 -1.20000
AFIX 0
C44 1 0.469863 0.314097 -0.255004 11.00000 0.03332 0.02719 =
0.03725 0.00569 0.01407 0.00590
AFIX 43
H44 2 0.498941 0.278972 -0.289280 11.00000 -1.20000
AFIX 0
C45 1 0.480221 0.408800 -0.169028 11.00000 0.02815 0.03433 =
0.04131 -0.00284 0.00531 0.00460
AFIX 43
H45 2 0.516240 0.441054 -0.145810 11.00000 -1.20000
AFIX 0
C46 1 0.437786 0.457118 -0.116258 11.00000 0.02914 0.03443 =
0.03353 -0.00220 0.00090 0.00398
AFIX 43
H46 2 0.445208 0.520704 -0.056383 11.00000 -1.20000
AFIX 0
HKLF 4
REM khor2a in P2(1)/c 100K
REM R1 = 0.0869 for 4216 Fo > 4sig(Fo) and 0.0932 for all 4687 data
REM 389 parameters refined using 6 restraints
END
WGHT 0.1228 7.2867
REM Highest difference peak 0.949, deepest hole -0.426, 1-sigma level 0.103
Q1 1 0.0825 0.2819 0.0975 11.00000 0.05 0.95
Q2 1 0.0828 0.2758 0.2219 11.00000 0.05 0.82
Q3 1 0.0793 0.2725 -0.0303 11.00000 0.05 0.61
Q4 1 0.0836 0.2397 0.3806 11.00000 0.05 0.53
Q5 1 0.4187 0.5861 -0.1023 11.00000 0.05 0.44
Q6 1 0.3876 1.0905 -0.1293 11.00000 0.05 0.44
Q7 1 0.4704 0.1706 -0.2759 11.00000 0.05 0.43
Q8 1 0.1280 0.1442 0.1103 11.00000 0.05 0.41
Q9 1 0.4361 1.0425 -0.1341 11.00000 0.05 0.39
Q10 1 0.1235 0.4151 0.2469 11.00000 0.05 0.38
Q11 1 0.2516 0.9856 0.1638 11.00000 0.05 0.38
Q12 1 0.4278 0.5720 -0.0160 11.00000 0.05 0.37
Q13 1 0.1184 0.7616 0.2996 11.00000 0.05 0.36
Q14 1 0.3981 0.7079 -0.0432 11.00000 0.05 0.36
Q15 1 0.2474 0.1430 -0.1042 11.00000 0.05 0.36
Q16 1 0.0470 0.4137 0.1910 11.00000 0.05 0.35
Q17 1 0.3682 0.7707 -0.0881 11.00000 0.05 0.35
Q18 1 0.3679 0.7766 -0.0196 11.00000 0.05 0.35
Q19 1 0.3193 0.2850 -0.0252 11.00000 0.05 0.35
Q20 1 0.1174 0.1987 0.1739 11.00000 0.05 0.34
;
_shelx_res_checksum 14968
_olex2_date_sample_data_collection 2018-10-25
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.164
_oxdiff_exptl_absorpt_empirical_full_min 0.773
_exptl_crystal_preparation Luminescent