# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020
#######################################################################
#
# 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.
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data_2-NO2radical
_database_code_depnum_ccdc_archive 'CCDC 2004974'
loop_
_audit_author_name
_audit_author_address
'thomas l gianetti'
;University of Arizona
United States of America
;
_audit_update_record
;
2020-05-20 deposited with the CCDC. 2020-09-14 downloaded from the CCDC.
;
_audit_creation_date 2019-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common 2-NO2radical
_chemical_name_systematic 2-NO2radical
_chemical_formula_moiety 'C31 H38 N5 O4'
_chemical_formula_sum 'C31 H38 N5 O4'
_chemical_formula_weight 544.66
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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 triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.834(7)
_cell_length_b 11.010(7)
_cell_length_c 13.357(9)
_cell_angle_alpha 71.977(17)
_cell_angle_beta 84.217(17)
_cell_angle_gamma 64.762(17)
_cell_volume 1369.6(16)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 3993
_cell_measurement_temperature 100
_cell_measurement_theta_max 25.49
_cell_measurement_theta_min 2.28
_shelx_estimated_absorpt_T_max 0.993
_shelx_estimated_absorpt_T_min 0.957
_exptl_absorpt_coefficient_mu 0.089
_exptl_absorpt_correction_T_max 0.7452
_exptl_absorpt_correction_T_min 0.6277
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0757 before and 0.0448 after correction. The Ratio of minimum to maximum transmission is 0.8423. The \l/2 correction factor is 0.00150.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'metallic dark gray'
_exptl_crystal_colour_lustre metallic
_exptl_crystal_colour_modifier dark
_exptl_crystal_colour_primary gray
_exptl_crystal_density_diffrn 1.321
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 582
_exptl_crystal_preparation ?
_exptl_crystal_size_max 0.5
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.08
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0323
_diffrn_reflns_av_unetI/netI 0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 12298
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.545
_diffrn_reflns_theta_min 1.604
_diffrn_ambient_temperature 100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3329
_reflns_number_total 5025
_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 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_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 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.260
_refine_diff_density_min -0.294
_refine_diff_density_rms 0.056
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.022
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 367
_refine_ls_number_reflns 5025
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0929
_refine_ls_R_factor_gt 0.0528
_refine_ls_restrained_S_all 1.022
_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^)+(0.0625P)^2^+1.1428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1223
_refine_ls_wR_factor_ref 0.1487
_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.a Secondary CH2 refined with riding coordinates:
C00K(H00A,H00B), C00Q(H00C,H00D), C00S(H00E,H00F), C00T(H00G,H00H), C00X(H00I,
H00J), C00Y(H00K,H00M)
2.b Aromatic/amide H refined with riding coordinates:
C00L(H00L), C00N(H00N), C00O(H00O), C00P(H00P), C00R(H00R), C00U(H00U),
C00V(H00V), C00W(H00W)
2.c Idealised Me refined as rotating group:
C00Z(H00Q,H00S,H00T), C010(H01A,H01B,H01C), C011(H01D,H01E,H01F), C012(H01G,
H01H,H01I), C013(H01J,H01K,H01L), C014(H01M,H01N,H01O)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_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
O001 O 0.35755(18) 0.72620(18) 0.00308(12) 0.0269(4) Uani 1 1 d . . . . .
O002 O 0.52279(17) 0.80091(18) 0.09446(13) 0.0269(4) Uani 1 1 d . . . . .
O003 O -0.15677(17) 1.08037(18) 0.31801(13) 0.0276(4) Uani 1 1 d . . . . .
O004 O -0.14414(18) 0.9851(2) 0.48643(13) 0.0314(5) Uani 1 1 d . . . . .
N005 N -0.0968(2) 0.9875(2) 0.39885(15) 0.0222(5) Uani 1 1 d . . . . .
N006 N 0.3652(2) 0.5108(2) 0.36619(15) 0.0215(5) Uani 1 1 d . . . . .
N007 N 0.0949(2) 1.0048(2) 0.22232(15) 0.0211(5) Uani 1 1 d . . . . .
N008 N 0.3995(2) 0.1266(2) 0.60386(16) 0.0261(5) Uani 1 1 d . . . . .
N009 N 0.0592(2) 1.4140(3) 0.2279(2) 0.0376(6) Uani 1 1 d . . . . .
C00A C 0.2236(2) 0.7570(2) 0.29483(18) 0.0200(5) Uani 1 1 d . . . . .
C00B C 0.3053(2) 0.7589(3) 0.20453(18) 0.0197(5) Uani 1 1 d . . . . .
C00C C 0.2406(2) 0.8700(3) 0.11024(18) 0.0203(5) Uani 1 1 d . . . . .
C00D C 0.0308(2) 0.8731(2) 0.39009(18) 0.0210(5) Uani 1 1 d . . . . .
C00E C 0.1366(2) 0.9952(3) 0.12060(18) 0.0207(5) Uani 1 1 d . . . . .
C00F C 0.2544(2) 0.6297(3) 0.37681(18) 0.0211(5) Uani 1 1 d . . . . .
C00G C 0.2687(2) 0.8571(3) 0.00745(18) 0.0220(5) Uani 1 1 d . . . . .
C00H C 0.1128(2) 0.8816(2) 0.30165(17) 0.0194(5) Uani 1 1 d . . . . .
C00I C 0.4703(3) 0.5240(3) 0.29991(18) 0.0226(5) Uani 1 1 d . . . . .
C00J C 0.4415(2) 0.6515(3) 0.21910(18) 0.0215(5) Uani 1 1 d . . . . .
C00K C 0.0683(2) 1.1338(3) 0.24717(19) 0.0230(6) Uani 1 1 d . . . . .
H00A H 0.044289 1.122712 0.321975 0.028 Uiso 1 1 calc R . . . .
H00B H -0.010458 1.212598 0.203195 0.028 Uiso 1 1 calc R . . . .
C00L C 0.0646(2) 0.7477(3) 0.47092(18) 0.0228(6) Uani 1 1 d . . . . .
H00L H 0.010255 0.745358 0.531309 0.027 Uiso 1 1 calc R . . . .
C00M C 0.5520(3) 0.6697(3) 0.16188(19) 0.0241(6) Uani 1 1 d . . . . .
C00N C 0.6013(3) 0.4153(3) 0.3154(2) 0.0263(6) Uani 1 1 d . . . . .
H00N H 0.618516 0.327519 0.366874 0.032 Uiso 1 1 calc R . . . .
C00O C 0.2043(3) 0.9688(3) -0.07927(19) 0.0250(6) Uani 1 1 d . . . . .
H00O H 0.226053 0.959896 -0.148109 0.030 Uiso 1 1 calc R . . . .
C00P C 0.0712(3) 1.1085(3) 0.03281(19) 0.0241(6) Uani 1 1 d . . . . .
H00P H 0.002656 1.194100 0.041042 0.029 Uiso 1 1 calc R . . . .
C00Q C 0.5069(3) 0.1737(3) 0.59669(19) 0.0250(6) Uani 1 1 d . . . . .
H00C H 0.583412 0.120102 0.558428 0.030 Uiso 1 1 calc R . . . .
H00D H 0.541568 0.152896 0.668649 0.030 Uiso 1 1 calc R . . . .
C00R C 0.1748(3) 0.6274(3) 0.46532(19) 0.0238(6) Uani 1 1 d . . . . .
H00R H 0.196678 0.542818 0.521586 0.029 Uiso 1 1 calc R . . . .
C00S C 0.3846(3) 0.3718(3) 0.43671(18) 0.0237(6) Uani 1 1 d . . . . .
H00E H 0.435926 0.300752 0.399636 0.028 Uiso 1 1 calc R . . . .
H00F H 0.293964 0.370076 0.452127 0.028 Uiso 1 1 calc R . . . .
C00T C 0.4604(3) 0.3299(3) 0.54081(19) 0.0254(6) Uani 1 1 d . . . . .
H00G H 0.540807 0.352620 0.527162 0.030 Uiso 1 1 calc R . . . .
H00H H 0.399565 0.384446 0.586723 0.030 Uiso 1 1 calc R . . . .
C00U C 0.1076(3) 1.0943(3) -0.06584(19) 0.0262(6) Uani 1 1 d . . . . .
H00U H 0.065677 1.172076 -0.126076 0.031 Uiso 1 1 calc R . . . .
C00V C 0.6818(3) 0.5629(3) 0.1796(2) 0.0275(6) Uani 1 1 d . . . . .
H00V H 0.755275 0.576017 0.139751 0.033 Uiso 1 1 calc R . . . .
C00W C 0.7046(3) 0.4365(3) 0.2556(2) 0.0295(6) Uani 1 1 d . . . . .
H00W H 0.793904 0.362740 0.266539 0.035 Uiso 1 1 calc R . . . .
C00X C 0.1913(3) 1.1681(3) 0.2277(2) 0.0293(6) Uani 1 1 d . . . . .
H00I H 0.204781 1.195647 0.150925 0.035 Uiso 1 1 calc R . . . .
H00J H 0.273344 1.082603 0.260858 0.035 Uiso 1 1 calc R . . . .
C00Y C 0.1784(3) 1.2852(3) 0.2704(2) 0.0312(6) Uani 1 1 d . . . . .
H00K H 0.173658 1.254358 0.348109 0.037 Uiso 1 1 calc R . . . .
H00M H 0.261000 1.303769 0.253543 0.037 Uiso 1 1 calc R . . . .
C00Z C 0.4551(3) -0.0257(3) 0.6436(2) 0.0330(6) Uani 1 1 d . . . . .
H00Q H 0.528663 -0.066564 0.598818 0.049 Uiso 1 1 calc GR . . . .
H00S H 0.382806 -0.056654 0.642906 0.049 Uiso 1 1 calc GR . . . .
H00T H 0.491229 -0.056609 0.715869 0.049 Uiso 1 1 calc GR . . . .
C010 C 0.2928(3) 0.1877(3) 0.6709(2) 0.0347(7) Uani 1 1 d . . . . .
H01A H 0.331969 0.162819 0.741312 0.052 Uiso 1 1 calc GR . . . .
H01B H 0.223237 0.151572 0.676050 0.052 Uiso 1 1 calc GR . . . .
H01C H 0.250971 0.290247 0.640864 0.052 Uiso 1 1 calc GR . . . .
C011 C 0.6162(3) 0.8143(3) 0.0140(2) 0.0367(7) Uani 1 1 d . . . . .
H01D H 0.574067 0.906326 -0.038827 0.055 Uiso 1 1 calc GR . . . .
H01E H 0.640063 0.739950 -0.019505 0.055 Uiso 1 1 calc GR . . . .
H01F H 0.698878 0.805986 0.044700 0.055 Uiso 1 1 calc GR . . . .
C012 C 0.3824(3) 0.7048(3) -0.0980(2) 0.0397(7) Uani 1 1 d . . . . .
H01G H 0.422322 0.767479 -0.142067 0.060 Uiso 1 1 calc GR . . . .
H01H H 0.296211 0.725374 -0.131122 0.060 Uiso 1 1 calc GR . . . .
H01I H 0.445922 0.606916 -0.090592 0.060 Uiso 1 1 calc GR . . . .
C013 C 0.0350(3) 1.5145(3) 0.2849(3) 0.0448(8) Uani 1 1 d . . . . .
H01J H 0.027793 1.471350 0.360022 0.067 Uiso 1 1 calc GR . . . .
H01K H -0.050154 1.597580 0.257986 0.067 Uiso 1 1 calc GR . . . .
H01L H 0.111036 1.542494 0.275050 0.067 Uiso 1 1 calc GR . . . .
C014 C 0.0750(4) 1.4786(4) 0.1190(3) 0.0663(12) Uani 1 1 d . . . . .
H01M H 0.156052 1.498200 0.112281 0.099 Uiso 1 1 calc GR . . . .
H01N H -0.005946 1.566723 0.092385 0.099 Uiso 1 1 calc GR . . . .
H01O H 0.085579 1.414902 0.078004 0.099 Uiso 1 1 calc GR . . . .
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
O001 0.0357(10) 0.0271(10) 0.0171(9) -0.0113(7) 0.0016(7) -0.0095(8)
O002 0.0272(9) 0.0279(10) 0.0253(9) -0.0088(8) 0.0080(7) -0.0119(8)
O003 0.0243(9) 0.0279(10) 0.0243(9) -0.0052(8) -0.0012(7) -0.0064(8)
O004 0.0304(10) 0.0391(11) 0.0216(9) -0.0133(8) 0.0066(8) -0.0098(9)
N005 0.0210(10) 0.0259(12) 0.0215(11) -0.0101(9) 0.0017(9) -0.0094(9)
N006 0.0238(11) 0.0189(11) 0.0196(10) -0.0066(8) 0.0005(8) -0.0062(9)
N007 0.0229(11) 0.0216(11) 0.0185(10) -0.0074(9) 0.0012(8) -0.0080(9)
N008 0.0284(12) 0.0222(12) 0.0280(11) -0.0077(9) -0.0010(9) -0.0101(9)
N009 0.0318(13) 0.0348(14) 0.0499(15) -0.0192(12) -0.0025(11) -0.0117(11)
C00A 0.0227(12) 0.0216(13) 0.0167(12) -0.0086(10) -0.0002(10) -0.0080(10)
C00B 0.0229(12) 0.0236(13) 0.0158(11) -0.0089(10) 0.0009(9) -0.0105(10)
C00C 0.0223(12) 0.0235(13) 0.0176(12) -0.0067(10) 0.0001(10) -0.0112(10)
C00D 0.0220(12) 0.0210(13) 0.0201(12) -0.0095(10) -0.0010(10) -0.0062(10)
C00E 0.0221(12) 0.0251(13) 0.0184(12) -0.0069(10) 0.0009(10) -0.0127(11)
C00F 0.0243(13) 0.0221(13) 0.0165(12) -0.0075(10) -0.0025(10) -0.0076(10)
C00G 0.0251(13) 0.0255(14) 0.0189(12) -0.0084(10) 0.0017(10) -0.0126(11)
C00H 0.0221(12) 0.0220(13) 0.0155(12) -0.0072(10) -0.0035(9) -0.0085(10)
C00I 0.0268(13) 0.0245(14) 0.0180(12) -0.0106(10) 0.0003(10) -0.0088(11)
C00J 0.0248(13) 0.0240(13) 0.0168(12) -0.0105(10) 0.0000(10) -0.0080(10)
C00K 0.0249(13) 0.0209(13) 0.0213(12) -0.0078(10) 0.0027(10) -0.0073(10)
C00L 0.0266(13) 0.0271(14) 0.0152(12) -0.0066(10) 0.0026(10) -0.0119(11)
C00M 0.0266(13) 0.0287(14) 0.0209(12) -0.0124(11) 0.0023(10) -0.0119(11)
C00N 0.0300(14) 0.0222(14) 0.0228(13) -0.0103(11) -0.0022(11) -0.0041(11)
C00O 0.0292(14) 0.0339(15) 0.0154(12) -0.0075(11) 0.0011(10) -0.0161(12)
C00P 0.0244(13) 0.0241(14) 0.0227(13) -0.0058(11) 0.0002(10) -0.0096(11)
C00Q 0.0258(13) 0.0271(14) 0.0202(12) -0.0056(11) -0.0030(10) -0.0095(11)
C00R 0.0276(13) 0.0238(14) 0.0183(12) -0.0048(10) 0.0011(10) -0.0102(11)
C00S 0.0277(13) 0.0193(13) 0.0221(13) -0.0062(10) -0.0013(10) -0.0075(11)
C00T 0.0303(14) 0.0224(14) 0.0215(13) -0.0061(11) -0.0025(11) -0.0087(11)
C00U 0.0284(14) 0.0284(14) 0.0203(12) -0.0020(11) -0.0029(10) -0.0133(11)
C00V 0.0233(13) 0.0345(16) 0.0281(14) -0.0163(12) 0.0058(11) -0.0114(12)
C00W 0.0260(14) 0.0317(15) 0.0298(14) -0.0177(12) -0.0015(11) -0.0046(11)
C00X 0.0257(14) 0.0312(15) 0.0352(15) -0.0144(12) 0.0042(11) -0.0134(12)
C00Y 0.0319(15) 0.0309(15) 0.0330(15) -0.0123(12) 0.0000(12) -0.0130(12)
C00Z 0.0357(15) 0.0263(15) 0.0380(16) -0.0067(12) -0.0042(12) -0.0146(12)
C010 0.0362(16) 0.0344(16) 0.0351(16) -0.0121(13) 0.0069(12) -0.0161(13)
C011 0.0387(16) 0.0367(17) 0.0370(16) -0.0129(13) 0.0148(13) -0.0195(13)
C012 0.0587(19) 0.0378(17) 0.0197(14) -0.0149(12) 0.0047(13) -0.0136(15)
C013 0.0492(19) 0.0358(18) 0.053(2) -0.0221(15) 0.0100(15) -0.0167(15)
C014 0.087(3) 0.045(2) 0.046(2) -0.0154(17) -0.0160(19) -0.0023(19)
_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
O001 C00G 1.366(3) . ?
O001 C012 1.422(3) . ?
O002 C00M 1.364(3) . ?
O002 C011 1.418(3) . ?
O003 N005 1.235(3) . ?
O004 N005 1.226(3) . ?
N005 C00D 1.444(3) . ?
N006 C00F 1.384(3) . ?
N006 C00I 1.400(3) . ?
N006 C00S 1.465(3) . ?
N007 C00E 1.409(3) . ?
N007 C00H 1.388(3) . ?
N007 C00K 1.461(3) . ?
N008 C00Q 1.447(3) . ?
N008 C00Z 1.452(3) . ?
N008 C010 1.447(3) . ?
N009 C00Y 1.445(4) . ?
N009 C013 1.452(4) . ?
N009 C014 1.437(4) . ?
C00A C00B 1.423(3) . ?
C00A C00F 1.414(3) . ?
C00A C00H 1.408(3) . ?
C00B C00C 1.438(3) . ?
C00B C00J 1.428(3) . ?
C00C C00E 1.397(3) . ?
C00C C00G 1.413(3) . ?
C00D C00H 1.409(3) . ?
C00D C00L 1.390(3) . ?
C00E C00P 1.393(3) . ?
C00F C00R 1.391(3) . ?
C00G C00O 1.375(3) . ?
C00I C00J 1.410(3) . ?
C00I C00N 1.395(3) . ?
C00J C00M 1.409(3) . ?
C00K H00A 0.9900 . ?
C00K H00B 0.9900 . ?
C00K C00X 1.512(4) . ?
C00L H00L 0.9500 . ?
C00L C00R 1.372(3) . ?
C00M C00V 1.379(4) . ?
C00N H00N 0.9500 . ?
C00N C00W 1.368(4) . ?
C00O H00O 0.9500 . ?
C00O C00U 1.386(4) . ?
C00P H00P 0.9500 . ?
C00P C00U 1.374(4) . ?
C00Q H00C 0.9900 . ?
C00Q H00D 0.9900 . ?
C00Q C00T 1.520(4) . ?
C00R H00R 0.9500 . ?
C00S H00E 0.9900 . ?
C00S H00F 0.9900 . ?
C00S C00T 1.527(3) . ?
C00T H00G 0.9900 . ?
C00T H00H 0.9900 . ?
C00U H00U 0.9500 . ?
C00V H00V 0.9500 . ?
C00V C00W 1.382(4) . ?
C00W H00W 0.9500 . ?
C00X H00I 0.9900 . ?
C00X H00J 0.9900 . ?
C00X C00Y 1.514(4) . ?
C00Y H00K 0.9900 . ?
C00Y H00M 0.9900 . ?
C00Z H00Q 0.9800 . ?
C00Z H00S 0.9800 . ?
C00Z H00T 0.9800 . ?
C010 H01A 0.9800 . ?
C010 H01B 0.9800 . ?
C010 H01C 0.9800 . ?
C011 H01D 0.9800 . ?
C011 H01E 0.9800 . ?
C011 H01F 0.9800 . ?
C012 H01G 0.9800 . ?
C012 H01H 0.9800 . ?
C012 H01I 0.9800 . ?
C013 H01J 0.9800 . ?
C013 H01K 0.9800 . ?
C013 H01L 0.9800 . ?
C014 H01M 0.9800 . ?
C014 H01N 0.9800 . ?
C014 H01O 0.9800 . ?
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
C00G O001 C012 117.3(2) . . ?
C00M O002 C011 117.2(2) . . ?
O003 N005 C00D 119.11(19) . . ?
O004 N005 O003 122.5(2) . . ?
O004 N005 C00D 118.3(2) . . ?
C00F N006 C00I 120.0(2) . . ?
C00F N006 C00S 120.2(2) . . ?
C00I N006 C00S 119.05(19) . . ?
C00E N007 C00K 118.98(19) . . ?
C00H N007 C00E 118.1(2) . . ?
C00H N007 C00K 121.0(2) . . ?
C00Q N008 C00Z 110.3(2) . . ?
C010 N008 C00Q 111.4(2) . . ?
C010 N008 C00Z 109.8(2) . . ?
C00Y N009 C013 111.3(2) . . ?
C014 N009 C00Y 111.0(2) . . ?
C014 N009 C013 107.9(3) . . ?
C00F C00A C00B 119.6(2) . . ?
C00H C00A C00B 119.7(2) . . ?
C00H C00A C00F 120.6(2) . . ?
C00A C00B C00C 115.7(2) . . ?
C00A C00B C00J 116.1(2) . . ?
C00J C00B C00C 128.2(2) . . ?
C00E C00C C00B 118.3(2) . . ?
C00E C00C C00G 117.6(2) . . ?
C00G C00C C00B 124.0(2) . . ?
C00H C00D N005 123.0(2) . . ?
C00L C00D N005 116.1(2) . . ?
C00L C00D C00H 120.7(2) . . ?
C00C C00E N007 118.8(2) . . ?
C00P C00E N007 119.7(2) . . ?
C00P C00E C00C 121.5(2) . . ?
N006 C00F C00A 118.1(2) . . ?
N006 C00F C00R 122.1(2) . . ?
C00R C00F C00A 119.8(2) . . ?
O001 C00G C00C 114.9(2) . . ?
O001 C00G C00O 124.2(2) . . ?
C00O C00G C00C 120.8(2) . . ?
N007 C00H C00A 117.5(2) . . ?
N007 C00H C00D 124.7(2) . . ?
C00D C00H C00A 117.7(2) . . ?
N006 C00I C00J 118.3(2) . . ?
C00N C00I N006 120.8(2) . . ?
C00N C00I C00J 120.9(2) . . ?
C00I C00J C00B 119.0(2) . . ?
C00M C00J C00B 123.3(2) . . ?
C00M C00J C00I 117.5(2) . . ?
N007 C00K H00A 109.4 . . ?
N007 C00K H00B 109.4 . . ?
N007 C00K C00X 111.3(2) . . ?
H00A C00K H00B 108.0 . . ?
C00X C00K H00A 109.4 . . ?
C00X C00K H00B 109.4 . . ?
C00D C00L H00L 119.3 . . ?
C00R C00L C00D 121.4(2) . . ?
C00R C00L H00L 119.3 . . ?
O002 C00M C00J 115.5(2) . . ?
O002 C00M C00V 123.4(2) . . ?
C00V C00M C00J 121.0(2) . . ?
C00I C00N H00N 120.4 . . ?
C00W C00N C00I 119.3(2) . . ?
C00W C00N H00N 120.4 . . ?
C00G C00O H00O 120.1 . . ?
C00G C00O C00U 119.7(2) . . ?
C00U C00O H00O 120.1 . . ?
C00E C00P H00P 120.6 . . ?
C00U C00P C00E 118.8(2) . . ?
C00U C00P H00P 120.6 . . ?
N008 C00Q H00C 108.9 . . ?
N008 C00Q H00D 108.9 . . ?
N008 C00Q C00T 113.2(2) . . ?
H00C C00Q H00D 107.8 . . ?
C00T C00Q H00C 108.9 . . ?
C00T C00Q H00D 108.9 . . ?
C00F C00R H00R 120.2 . . ?
C00L C00R C00F 119.7(2) . . ?
C00L C00R H00R 120.2 . . ?
N006 C00S H00E 108.6 . . ?
N006 C00S H00F 108.6 . . ?
N006 C00S C00T 114.5(2) . . ?
H00E C00S H00F 107.6 . . ?
C00T C00S H00E 108.6 . . ?
C00T C00S H00F 108.6 . . ?
C00Q C00T C00S 111.0(2) . . ?
C00Q C00T H00G 109.4 . . ?
C00Q C00T H00H 109.4 . . ?
C00S C00T H00G 109.4 . . ?
C00S C00T H00H 109.4 . . ?
H00G C00T H00H 108.0 . . ?
C00O C00U H00U 119.3 . . ?
C00P C00U C00O 121.3(2) . . ?
C00P C00U H00U 119.3 . . ?
C00M C00V H00V 120.2 . . ?
C00M C00V C00W 119.7(2) . . ?
C00W C00V H00V 120.2 . . ?
C00N C00W C00V 121.5(2) . . ?
C00N C00W H00W 119.3 . . ?
C00V C00W H00W 119.3 . . ?
C00K C00X H00I 108.9 . . ?
C00K C00X H00J 108.9 . . ?
C00K C00X C00Y 113.3(2) . . ?
H00I C00X H00J 107.7 . . ?
C00Y C00X H00I 108.9 . . ?
C00Y C00X H00J 108.9 . . ?
N009 C00Y C00X 112.7(2) . . ?
N009 C00Y H00K 109.0 . . ?
N009 C00Y H00M 109.0 . . ?
C00X C00Y H00K 109.0 . . ?
C00X C00Y H00M 109.0 . . ?
H00K C00Y H00M 107.8 . . ?
N008 C00Z H00Q 109.5 . . ?
N008 C00Z H00S 109.5 . . ?
N008 C00Z H00T 109.5 . . ?
H00Q C00Z H00S 109.5 . . ?
H00Q C00Z H00T 109.5 . . ?
H00S C00Z H00T 109.5 . . ?
N008 C010 H01A 109.5 . . ?
N008 C010 H01B 109.5 . . ?
N008 C010 H01C 109.5 . . ?
H01A C010 H01B 109.5 . . ?
H01A C010 H01C 109.5 . . ?
H01B C010 H01C 109.5 . . ?
O002 C011 H01D 109.5 . . ?
O002 C011 H01E 109.5 . . ?
O002 C011 H01F 109.5 . . ?
H01D C011 H01E 109.5 . . ?
H01D C011 H01F 109.5 . . ?
H01E C011 H01F 109.5 . . ?
O001 C012 H01G 109.5 . . ?
O001 C012 H01H 109.5 . . ?
O001 C012 H01I 109.5 . . ?
H01G C012 H01H 109.5 . . ?
H01G C012 H01I 109.5 . . ?
H01H C012 H01I 109.5 . . ?
N009 C013 H01J 109.5 . . ?
N009 C013 H01K 109.5 . . ?
N009 C013 H01L 109.5 . . ?
H01J C013 H01K 109.5 . . ?
H01J C013 H01L 109.5 . . ?
H01K C013 H01L 109.5 . . ?
N009 C014 H01M 109.5 . . ?
N009 C014 H01N 109.5 . . ?
N009 C014 H01O 109.5 . . ?
H01M C014 H01N 109.5 . . ?
H01M C014 H01O 109.5 . . ?
H01N C014 H01O 109.5 . . ?
_shelx_res_file
;
TITL mo_tlg99_0m_a.res in P-1
mo_tlg99_0m.res
created by SHELXL-2018/3 at 14:11:15 on 30-Oct-2019
REM Old TITL mo_tlg99_0m in P-1
REM SHELXT solution in P-1
REM R1 0.159, Rweak 0.002, Alpha 0.027, Orientation as input
REM Formula found by SHELXT: C33 N3 O4
CELL 0.71073 10.8343 11.01 13.3566 71.977 84.217 64.762
ZERR 2 0.0071 0.0073 0.0087 0.017 0.017 0.017
LATT 1
SFAC C H N O
UNIT 62 76 10 8
L.S. 15
PLAN 20
SIZE 0.08 0.2 0.5
TEMP -173.15
BOND $H
list 4
fmap 2 53
acta
REM
REM
REM
WGHT 0.062500 1.142800
FVAR 0.58057
O001 4 0.357548 0.726203 0.003079 11.00000 0.03573 0.02709 =
0.01715 -0.01127 0.00156 -0.00945
O002 4 0.522788 0.800907 0.094458 11.00000 0.02716 0.02788 =
0.02525 -0.00884 0.00795 -0.01187
O003 4 -0.156766 1.080371 0.318012 11.00000 0.02432 0.02794 =
0.02432 -0.00520 -0.00123 -0.00644
O004 4 -0.144138 0.985143 0.486433 11.00000 0.03035 0.03906 =
0.02164 -0.01327 0.00655 -0.00983
N005 3 -0.096793 0.987455 0.398847 11.00000 0.02101 0.02586 =
0.02146 -0.01009 0.00171 -0.00945
N006 3 0.365155 0.510782 0.366189 11.00000 0.02383 0.01893 =
0.01957 -0.00658 0.00053 -0.00623
N007 3 0.094928 1.004791 0.222320 11.00000 0.02290 0.02160 =
0.01848 -0.00736 0.00117 -0.00800
N008 3 0.399525 0.126616 0.603857 11.00000 0.02839 0.02217 =
0.02796 -0.00772 -0.00100 -0.01009
N009 3 0.059164 1.413976 0.227856 11.00000 0.03177 0.03479 =
0.04986 -0.01918 -0.00249 -0.01167
C00A 1 0.223591 0.756956 0.294834 11.00000 0.02268 0.02162 =
0.01671 -0.00856 -0.00020 -0.00796
C00B 1 0.305345 0.758908 0.204528 11.00000 0.02286 0.02359 =
0.01580 -0.00886 0.00088 -0.01054
C00C 1 0.240556 0.869998 0.110241 11.00000 0.02231 0.02354 =
0.01758 -0.00666 0.00008 -0.01124
C00D 1 0.030811 0.873139 0.390094 11.00000 0.02197 0.02105 =
0.02008 -0.00949 -0.00104 -0.00624
C00E 1 0.136622 0.995247 0.120603 11.00000 0.02210 0.02508 =
0.01842 -0.00694 0.00091 -0.01266
C00F 1 0.254357 0.629745 0.376808 11.00000 0.02431 0.02213 =
0.01654 -0.00751 -0.00253 -0.00759
C00G 1 0.268694 0.857113 0.007452 11.00000 0.02515 0.02546 =
0.01891 -0.00838 0.00168 -0.01261
C00H 1 0.112779 0.881624 0.301652 11.00000 0.02209 0.02204 =
0.01554 -0.00724 -0.00346 -0.00851
C00I 1 0.470300 0.524041 0.299915 11.00000 0.02680 0.02446 =
0.01796 -0.01060 0.00026 -0.00878
C00J 1 0.441476 0.651465 0.219097 11.00000 0.02480 0.02395 =
0.01684 -0.01052 0.00003 -0.00802
C00K 1 0.068300 1.133804 0.247169 11.00000 0.02491 0.02087 =
0.02134 -0.00780 0.00267 -0.00728
AFIX 23
H00A 2 0.044289 1.122712 0.321975 11.00000 -1.20000
H00B 2 -0.010458 1.212598 0.203195 11.00000 -1.20000
AFIX 0
C00L 1 0.064611 0.747744 0.470918 11.00000 0.02662 0.02711 =
0.01524 -0.00662 0.00259 -0.01190
AFIX 43
H00L 2 0.010255 0.745358 0.531309 11.00000 -1.20000
AFIX 0
C00M 1 0.552038 0.669708 0.161883 11.00000 0.02660 0.02874 =
0.02086 -0.01242 0.00226 -0.01190
C00N 1 0.601257 0.415304 0.315390 11.00000 0.02998 0.02216 =
0.02278 -0.01028 -0.00222 -0.00413
AFIX 43
H00N 2 0.618516 0.327519 0.366874 11.00000 -1.20000
AFIX 0
C00O 1 0.204339 0.968753 -0.079273 11.00000 0.02919 0.03389 =
0.01536 -0.00754 0.00113 -0.01608
AFIX 43
H00O 2 0.226053 0.959896 -0.148109 11.00000 -1.20000
AFIX 0
C00P 1 0.071226 1.108523 0.032810 11.00000 0.02437 0.02410 =
0.02268 -0.00582 0.00021 -0.00958
AFIX 43
H00P 2 0.002656 1.194100 0.041042 11.00000 -1.20000
AFIX 0
C00Q 1 0.506946 0.173694 0.596691 11.00000 0.02580 0.02713 =
0.02020 -0.00561 -0.00300 -0.00952
AFIX 23
H00C 2 0.583412 0.120102 0.558428 11.00000 -1.20000
H00D 2 0.541568 0.152896 0.668649 11.00000 -1.20000
AFIX 0
C00R 1 0.174794 0.627378 0.465318 11.00000 0.02757 0.02384 =
0.01830 -0.00481 0.00107 -0.01024
AFIX 43
H00R 2 0.196678 0.542818 0.521586 11.00000 -1.20000
AFIX 0
C00S 1 0.384603 0.371832 0.436712 11.00000 0.02771 0.01927 =
0.02207 -0.00620 -0.00134 -0.00754
AFIX 23
H00E 2 0.435926 0.300752 0.399636 11.00000 -1.20000
H00F 2 0.293964 0.370076 0.452127 11.00000 -1.20000
AFIX 0
C00T 1 0.460411 0.329899 0.540812 11.00000 0.03029 0.02240 =
0.02148 -0.00613 -0.00253 -0.00868
AFIX 23
H00G 2 0.540807 0.352620 0.527162 11.00000 -1.20000
H00H 2 0.399565 0.384446 0.586723 11.00000 -1.20000
AFIX 0
C00U 1 0.107624 1.094306 -0.065843 11.00000 0.02838 0.02839 =
0.02030 -0.00200 -0.00286 -0.01335
AFIX 43
H00U 2 0.065677 1.172076 -0.126076 11.00000 -1.20000
AFIX 0
C00V 1 0.681837 0.562855 0.179589 11.00000 0.02329 0.03449 =
0.02808 -0.01632 0.00578 -0.01140
AFIX 43
H00V 2 0.755275 0.576017 0.139751 11.00000 -1.20000
AFIX 0
C00W 1 0.704568 0.436506 0.255583 11.00000 0.02602 0.03173 =
0.02975 -0.01765 -0.00155 -0.00461
AFIX 43
H00W 2 0.793904 0.362740 0.266539 11.00000 -1.20000
AFIX 0
C00X 1 0.191327 1.168130 0.227709 11.00000 0.02568 0.03122 =
0.03522 -0.01438 0.00417 -0.01338
AFIX 23
H00I 2 0.204781 1.195647 0.150925 11.00000 -1.20000
H00J 2 0.273344 1.082603 0.260858 11.00000 -1.20000
AFIX 0
C00Y 1 0.178391 1.285242 0.270448 11.00000 0.03185 0.03093 =
0.03300 -0.01233 0.00001 -0.01301
AFIX 23
H00K 2 0.173658 1.254358 0.348109 11.00000 -1.20000
H00M 2 0.261000 1.303769 0.253543 11.00000 -1.20000
AFIX 0
C00Z 1 0.455070 -0.025682 0.643593 11.00000 0.03569 0.02632 =
0.03801 -0.00674 -0.00425 -0.01462
AFIX 137
H00Q 2 0.528663 -0.066564 0.598818 11.00000 -1.50000
H00S 2 0.382806 -0.056654 0.642906 11.00000 -1.50000
H00T 2 0.491229 -0.056609 0.715869 11.00000 -1.50000
AFIX 0
C010 1 0.292820 0.187743 0.670930 11.00000 0.03619 0.03436 =
0.03513 -0.01206 0.00694 -0.01609
AFIX 137
H01A 2 0.331969 0.162819 0.741312 11.00000 -1.50000
H01B 2 0.223237 0.151572 0.676050 11.00000 -1.50000
H01C 2 0.250971 0.290247 0.640864 11.00000 -1.50000
AFIX 0
C011 1 0.616157 0.814328 0.013995 11.00000 0.03865 0.03674 =
0.03705 -0.01288 0.01476 -0.01946
AFIX 137
H01D 2 0.574067 0.906326 -0.038827 11.00000 -1.50000
H01E 2 0.640063 0.739950 -0.019505 11.00000 -1.50000
H01F 2 0.698878 0.805986 0.044700 11.00000 -1.50000
AFIX 0
C012 1 0.382433 0.704834 -0.098027 11.00000 0.05870 0.03778 =
0.01968 -0.01490 0.00468 -0.01363
AFIX 137
H01G 2 0.422322 0.767479 -0.142067 11.00000 -1.50000
H01H 2 0.296211 0.725374 -0.131122 11.00000 -1.50000
H01I 2 0.445922 0.606916 -0.090592 11.00000 -1.50000
AFIX 0
C013 1 0.034996 1.514519 0.284860 11.00000 0.04922 0.03576 =
0.05320 -0.02207 0.01002 -0.01672
AFIX 137
H01J 2 0.027793 1.471350 0.360022 11.00000 -1.50000
H01K 2 -0.050154 1.597580 0.257986 11.00000 -1.50000
H01L 2 0.111036 1.542494 0.275050 11.00000 -1.50000
AFIX 0
C014 1 0.074968 1.478583 0.118982 11.00000 0.08658 0.04456 =
0.04599 -0.01538 -0.01600 -0.00226
AFIX 137
H01M 2 0.156052 1.498200 0.112281 11.00000 -1.50000
H01N 2 -0.005946 1.566723 0.092385 11.00000 -1.50000
H01O 2 0.085579 1.414902 0.078004 11.00000 -1.50000
AFIX 0
HKLF 4
REM mo_tlg99_0m_a.res in P-1
REM wR2 = 0.1487, GooF = S = 1.022, Restrained GooF = 1.022 for all data
REM R1 = 0.0528 for 3329 Fo > 4sig(Fo) and 0.0929 for all 5025 data
REM 367 parameters refined using 0 restraints
END
WGHT 0.0594 1.2000
REM Highest difference peak 0.260, deepest hole -0.294, 1-sigma level 0.056
Q1 1 0.1581 1.5162 0.1248 11.00000 0.05 0.26
Q2 1 0.1798 1.4179 0.2064 11.00000 0.05 0.25
Q3 1 0.2428 1.3954 0.1808 11.00000 0.05 0.22
Q4 1 0.7154 0.6745 0.0021 11.00000 0.05 0.22
Q5 1 0.0627 0.8834 0.3420 11.00000 0.05 0.22
Q6 1 0.2597 0.7613 0.2639 11.00000 0.05 0.22
Q7 1 0.2654 0.8753 0.0571 11.00000 0.05 0.22
Q8 1 -0.0020 0.8526 0.3544 11.00000 0.05 0.22
Q9 1 0.4256 0.3614 0.4827 11.00000 0.05 0.22
Q10 1 0.2855 0.8803 0.1430 11.00000 0.05 0.22
Q11 1 0.2215 0.8470 0.0614 11.00000 0.05 0.21
Q12 1 -0.1131 1.0785 0.2548 11.00000 0.05 0.20
Q13 1 0.1272 1.1161 -0.0102 11.00000 0.05 0.20
Q14 1 0.2517 0.7736 0.1583 11.00000 0.05 0.20
Q15 1 0.1854 0.7441 0.2776 11.00000 0.05 0.20
Q16 1 0.3432 0.1559 0.5340 11.00000 0.05 0.20
Q17 1 0.4597 0.6210 0.2745 11.00000 0.05 0.20
Q18 1 0.4045 0.6614 0.1974 11.00000 0.05 0.19
Q19 1 -0.2175 1.0997 0.4951 11.00000 0.05 0.19
Q20 1 0.4957 0.6480 0.1678 11.00000 0.05 0.19
;
_shelx_res_checksum 5166
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene/hexanes'
_chemical_properties_physical Air-sensitive
#######################################################################
#
# 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_2-Hradical
_database_code_depnum_ccdc_archive 'CCDC 2004977'
loop_
_audit_author_name
_audit_author_address
'thomas l gianetti'
;University of Arizona
United States of America
;
_audit_update_record
;
2020-05-20 deposited with the CCDC. 2020-09-14 downloaded from the CCDC.
;
_audit_creation_date 2019-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common 2-Hradical
_chemical_name_systematic 2-Hradical
_chemical_formula_moiety 'C30.95 H38.88 N4 O2, 0.33(H2 O)'
_chemical_formula_sum 'C30.95 H39.55 N4 O2.33'
_chemical_formula_weight 505.00
_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 0.0148 0.0070 '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'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 '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 orthorhombic
_space_group_IT_number 61
_space_group_name_H-M_alt 'P b c a'
_space_group_name_Hall '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
_cell_length_a 20.1829(5)
_cell_length_b 10.7314(3)
_cell_length_c 25.5707(7)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 5538.4(3)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 9884
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 73.08
_cell_measurement_theta_min 3.56
_shelx_estimated_absorpt_T_max 0.981
_shelx_estimated_absorpt_T_min 0.955
_exptl_absorpt_coefficient_mu 0.391
_exptl_absorpt_correction_T_max 0.7537
_exptl_absorpt_correction_T_min 0.6302
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1038 before and 0.0593 after correction. The Ratio of minimum to maximum transmission is 0.8361. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'metallic dark violet'
_exptl_crystal_colour_lustre metallic
_exptl_crystal_colour_modifier dark
_exptl_crystal_colour_primary violet
_exptl_crystal_density_diffrn 1.211
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 2176
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.05
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0549
_diffrn_reflns_av_unetI/netI 0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_h_min -27
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 31
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_number 45766
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full 53.594
_diffrn_reflns_theta_max 73.269
_diffrn_reflns_theta_min 3.560
_diffrn_ambient_temperature 100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type GaK\a
_diffrn_radiation_wavelength 1.34138
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5594
_reflns_number_total 7238
_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 'SAINT V8.40A (?, 2016)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.40A (?, 2016)'
_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 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.535
_refine_diff_density_min -0.246
_refine_diff_density_rms 0.050
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.095
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 414
_refine_ls_number_reflns 7238
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0906
_refine_ls_R_factor_gt 0.0669
_refine_ls_restrained_S_all 1.109
_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^)+(0.0528P)^2^+3.1410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1402
_refine_ls_wR_factor_ref 0.1505
_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, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
C3AA-N0AB
1.47 with sigma of 0.01
N0AA-C4 \\sim N0AB-C1AA
with sigma of 0.02
N0AA-C6 \\sim N0AB-C6A
with sigma of 0.02
C3-C4 \\sim C4AA-C1AA
with sigma of 0.02
N0AA-C3 \\sim N0AB-C4AA
with sigma of 0.04
C4-C6 \\sim C1AA-C6A
with sigma of 0.04
3. Others
Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=1-FVAR(1)
Fixed Sof: N0AA(0.6667) C3(0.6667) H3A(0.6667) H3B(0.6667) C4(0.6667)
H4A(0.6667) C6(0.6667) H6A(0.6667) H6B(0.6667) H6C(0.6667) C4AA(0.33333)
H4AD(0.33333) H4AE(0.33333) C1AA(0.33333) H1AA(0.33333) H1AB(0.33333)
N0AB(0.33333) C6A(0.33333) H6AA(0.33333) H6AB(0.33333) H6AC(0.33333)
O2A(0.33333) H2AA(0.33333) H2AB(0.33333) H3AC(0.6667) H3AD(0.6667)
H3AE(0.6667) H3AF(0.33333) H3AG(0.33333) H3AH(0.33333) H4B(0.6667)
C0AA(0.33333) H0AA(0.33333) H0AB(0.33333) C2(0.6667) H2A(0.6667) H2B(0.6667)
4.a Free rotating group:
O2A(H2AA,H2AB)
4.b Secondary CH2 refined with riding coordinates:
C00I(H00C,H00E), C3A(H3AA,H3AB), C3(H3A,H3B), C4AA(H4AD,H4AE), C1AA(H1AA,
H1AB), C0AA(H0AA,H0AB), C2(H2A,H2B)
4.c Aromatic/amide H refined with riding coordinates:
C00A(H00A), C00B(H00B), C00D(H00D), C00L(H00L), C00M(H00M), C00N(H00N),
C00O(H00O), C00Q(H00Q), C00R(H00R)
4.d Idealised Me refined as rotating group:
C00K(H00F,H00G,H00H), C00S(H00K,H00P,H00S), C4A(H4AA,H4AB,H4AC), C6(H6A,H6B,
H6C), C1(H1A,H1B,H1C), C6A(H6AA,H6AB,H6AC), C3AA(H3AC,H3AD,H3AE), C3AA(H3AF,
H3AG,H3AH)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_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
O001 O 0.45057(5) 0.69694(10) 0.24546(5) 0.0259(3) Uani 1 1 d . . . . .
O002 O 0.48079(5) 0.52500(11) 0.32277(5) 0.0303(3) Uani 1 1 d . . . . .
N003 N 0.30077(7) 0.35716(13) 0.22486(6) 0.0290(3) Uani 1 1 d . . . . .
N004 N 0.26211(7) 0.67505(14) 0.35348(6) 0.0325(3) Uani 1 1 d . . . . .
C006 C 0.38231(7) 0.51901(14) 0.23939(7) 0.0218(3) Uani 1 1 d . . . . .
C007 C 0.43592(7) 0.59010(13) 0.21894(7) 0.0220(3) Uani 1 1 d . . . . .
C008 C 0.35822(7) 0.41990(14) 0.20826(7) 0.0244(3) Uani 1 1 d . . . . .
C009 C 0.37464(8) 0.61189(15) 0.33316(7) 0.0255(3) Uani 1 1 d . . . . .
C00A C 0.46905(8) 0.55368(15) 0.17422(7) 0.0275(4) Uani 1 1 d . . . . .
H00A H 0.506428 0.599244 0.162211 0.033 Uiso 1 1 calc R . . . .
C00B C 0.39167(8) 0.38416(15) 0.16286(7) 0.0275(4) Uani 1 1 d . . . . .
H00B H 0.376410 0.315134 0.142960 0.033 Uiso 1 1 calc R . . . .
C00C C 0.44192(8) 0.60796(15) 0.34944(7) 0.0274(4) Uani 1 1 d . . . . .
C00D C 0.44705(9) 0.44972(16) 0.14705(7) 0.0300(4) Uani 1 1 d . . . . .
H00D H 0.470610 0.423009 0.116906 0.036 Uiso 1 1 calc R . . . .
C00E C 0.33005(8) 0.68021(15) 0.36472(7) 0.0294(4) Uani 1 1 d . . . . .
C00F C 0.27986(7) 0.51370(15) 0.28989(7) 0.0277(4) Uani 1 1 d . . . . .
C00G C 0.23657(8) 0.57818(16) 0.32336(8) 0.0313(4) Uani 1 1 d . . . . .
C00H C 0.25565(8) 0.41783(16) 0.25772(7) 0.0295(4) Uani 1 1 d . . . . .
C00I C 0.28010(9) 0.24444(16) 0.19710(8) 0.0331(4) Uani 1 1 d . . . . .
H00C H 0.251192 0.194810 0.220432 0.040 Uiso 1 1 calc R . . . .
H00E H 0.319881 0.193708 0.189363 0.040 Uiso 1 1 calc R . . . .
C00J C 0.34871(8) 0.54805(16) 0.28774(8) 0.0309(4) Uani 1 1 d . . . . .
C00K C 0.51037(8) 0.75927(16) 0.23176(8) 0.0327(4) Uani 1 1 d . . . . .
H00F H 0.507389 0.789065 0.195608 0.049 Uiso 1 1 calc GR . . . .
H00G H 0.547702 0.701381 0.234981 0.049 Uiso 1 1 calc GR . . . .
H00H H 0.517181 0.830257 0.255259 0.049 Uiso 1 1 calc GR . . . .
C00L C 0.46477(9) 0.68065(18) 0.38996(8) 0.0349(4) Uani 1 1 d . . . . .
H00L H 0.510381 0.679945 0.399146 0.042 Uiso 1 1 calc R . . . .
C00M C 0.14701(8) 0.44762(19) 0.29404(9) 0.0418(5) Uani 1 1 d . . . . .
H00M H 0.101721 0.423931 0.295995 0.050 Uiso 1 1 calc R . . . .
C00N C 0.18863(8) 0.38387(17) 0.26066(8) 0.0359(4) Uani 1 1 d . . . . .
H00N H 0.172048 0.317523 0.239829 0.043 Uiso 1 1 calc R . . . .
C00O C 0.35370(10) 0.75343(18) 0.40568(8) 0.0385(4) Uani 1 1 d . . . . .
H00O H 0.323772 0.802375 0.425689 0.046 Uiso 1 1 calc R . . . .
C00P C 0.24310(10) 0.26904(18) 0.14599(9) 0.0381(5) Uani 1 1 d . . . . .
C00Q C 0.42034(10) 0.7550(2) 0.41724(8) 0.0412(5) Uani 1 1 d . . . . .
H00Q H 0.436165 0.807836 0.444317 0.049 Uiso 1 1 calc R . . . .
C00R C 0.16931(8) 0.54497(18) 0.32472(9) 0.0399(5) Uani 1 1 d . . . . .
H00R H 0.139338 0.589125 0.346566 0.048 Uiso 1 1 calc R . . . .
C00S C 0.54995(8) 0.52762(19) 0.33333(9) 0.0398(5) Uani 1 1 d . . . . .
H00K H 0.572693 0.468214 0.310414 0.060 Uiso 1 1 calc GR . . . .
H00P H 0.557715 0.504765 0.369927 0.060 Uiso 1 1 calc GR . . . .
H00S H 0.567111 0.611671 0.326928 0.060 Uiso 1 1 calc GR . . . .
C3A C 0.22893(13) 0.1473(2) 0.11790(9) 0.0538(8) Uani 0.977(5) 1 d . . P A 2
H3AA H 0.268654 0.093448 0.119950 0.065 Uiso 0.977(5) 1 calc R . P A 2
H3AB H 0.192268 0.103853 0.136029 0.065 Uiso 0.977(5) 1 calc R . P A 2
C4A C 0.20500(17) 0.0446(2) 0.03740(11) 0.0737(11) Uani 0.977(5) 1 d . . P A 2
H4AA H 0.246896 -0.001032 0.040404 0.111 Uiso 0.977(5) 1 calc GR . P A 2
H4AB H 0.194477 0.057508 0.000386 0.111 Uiso 0.977(5) 1 calc GR . P A 2
H4AC H 0.169498 -0.003633 0.053956 0.111 Uiso 0.977(5) 1 calc GR . P A 2
N1 N 0.21114(9) 0.16453(16) 0.06330(7) 0.0415(4) Uani 1 1 d . . . . .
N0AA N 0.08061(12) 0.7482(3) 0.44001(13) 0.0432(7) Uani 0.6667 1 d D . P B 1
C3 C 0.20086(16) 0.7095(3) 0.44032(14) 0.0378(7) Uani 0.6667 1 d D . P B 1
H3A H 0.188888 0.620274 0.437808 0.045 Uiso 0.6667 1 calc R . P B 1
H3B H 0.239880 0.716650 0.463593 0.045 Uiso 0.6667 1 calc R . P B 1
C4 C 0.14348(16) 0.7811(3) 0.46392(14) 0.0447(8) Uani 0.6667 1 d D . P B 1
H4A H 0.1514(17) 0.878(3) 0.4518(14) 0.054 Uiso 0.6667 1 d R . P C 1
C6 C 0.0308(2) 0.8457(4) 0.4488(2) 0.0697(15) Uani 0.6667 1 d D . P B 1
H6A H 0.021886 0.853224 0.486299 0.105 Uiso 0.6667 1 calc GR . P B 1
H6B H -0.010235 0.823583 0.430448 0.105 Uiso 0.6667 1 calc GR . P B 1
H6C H 0.047400 0.925329 0.435352 0.105 Uiso 0.6667 1 calc GR . P B 1
C1 C 0.14995(13) 0.2327(3) 0.05895(10) 0.0759(9) Uani 1 1 d . . . . .
H1A H 0.114574 0.186805 0.076776 0.114 Uiso 1 1 calc GR . . . .
H1B H 0.138501 0.242876 0.021945 0.114 Uiso 1 1 calc GR . . . .
H1C H 0.155118 0.314904 0.075153 0.114 Uiso 1 1 calc GR . . . .
C4AA C 0.1760(2) 0.7317(5) 0.4176(2) 0.0253(11) Uani 0.3333 1 d D . P B 2
H4AD H 0.165118 0.641771 0.418304 0.030 Uiso 0.3333 1 calc R . P B 2
H4AE H 0.205463 0.750245 0.447522 0.030 Uiso 0.3333 1 calc R . P B 2
C1AA C 0.1137(2) 0.8073(5) 0.42167(19) 0.0241(10) Uani 0.3333 1 d D . P B 2
H1AA H 0.125615 0.896785 0.420248 0.029 Uiso 0.3333 1 calc R . P B 2
H1AB H 0.085531 0.789100 0.390931 0.029 Uiso 0.3333 1 calc R . P B 2
N0AB N 0.0742(2) 0.7845(4) 0.47009(19) 0.0257(10) Uani 0.3333 1 d D . P B 2
C6A C 0.0211(4) 0.8789(8) 0.4740(3) 0.049(2) Uani 0.3333 1 d D . P B 2
H6AA H -0.006860 0.875089 0.442698 0.074 Uiso 0.3333 1 calc GR . P B 2
H6AB H 0.040805 0.962011 0.476914 0.074 Uiso 0.3333 1 calc GR . P B 2
H6AC H -0.006013 0.862040 0.505039 0.074 Uiso 0.3333 1 calc GR . P B 2
H00I H 0.2687(10) 0.3225(18) 0.1243(8) 0.029(5) Uiso 1 1 d . . . . .
H00J H 0.2022(13) 0.314(2) 0.1525(10) 0.055(7) Uiso 1 1 d . . . . .
O2A O 0.1441(2) 0.8210(5) 0.56548(16) 0.0412(10) Uani 0.3333 1 d . . P D 2
H2AA H 0.126980 0.832420 0.534644 0.062 Uiso 0.3333 1 d G . P D 2
H2AB H 0.186636 0.817459 0.559939 0.062 Uiso 0.3333 1 d G . P D 2
C3AA C 0.05279(11) 0.6410(2) 0.46414(11) 0.0589(7) Uani 1 1 d D . . . .
H3AC H 0.083954 0.571300 0.461399 0.088 Uiso 0.6667 1 calc GR . P B 1
H3AD H 0.011234 0.619107 0.446571 0.088 Uiso 0.6667 1 calc GR . P B 1
H3AE H 0.043982 0.658720 0.501091 0.088 Uiso 0.6667 1 calc GR . P B 1
H3AF H 0.019318 0.633440 0.436556 0.088 Uiso 0.3333 1 calc GR . P B 2
H3AG H 0.034303 0.611225 0.497301 0.088 Uiso 0.3333 1 calc GR . P B 2
H3AH H 0.091654 0.590870 0.454937 0.088 Uiso 0.3333 1 calc GR . P B 2
H4B H 0.1399(16) 0.763(3) 0.5058(14) 0.042(9) Uiso 0.6667 1 d . . P E 1
C0AA C 0.2107(6) 0.7640(14) 0.3666(4) 0.030(2) Uani 0.3333 1 d . . P B 2
H0AA H 0.177635 0.766312 0.338013 0.036 Uiso 0.3333 1 calc R . P B 2
H0AB H 0.230550 0.848064 0.369583 0.036 Uiso 0.3333 1 calc R . P B 2
C2 C 0.2191(3) 0.7586(7) 0.3855(2) 0.0333(12) Uani 0.6667 1 d . . P B 1
H2A H 0.177635 0.774133 0.365924 0.040 Uiso 0.6667 1 calc R . P B 1
H2B H 0.241978 0.839647 0.389616 0.040 Uiso 0.6667 1 calc R . P B 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O001 0.0181(5) 0.0211(5) 0.0384(7) -0.0030(5) 0.0028(5) -0.0041(4)
O002 0.0166(5) 0.0319(6) 0.0425(8) -0.0049(5) -0.0015(5) 0.0018(4)
N003 0.0228(7) 0.0254(7) 0.0387(9) 0.0022(6) -0.0054(6) -0.0087(5)
N004 0.0204(7) 0.0312(7) 0.0459(10) 0.0035(7) 0.0089(6) 0.0024(5)
C006 0.0148(6) 0.0201(7) 0.0305(9) 0.0022(6) -0.0037(6) 0.0008(5)
C007 0.0166(6) 0.0187(7) 0.0307(9) 0.0013(6) -0.0038(6) 0.0008(5)
C008 0.0200(7) 0.0199(7) 0.0332(10) 0.0055(6) -0.0057(7) -0.0016(5)
C009 0.0194(7) 0.0250(8) 0.0322(9) 0.0014(7) 0.0034(7) -0.0024(6)
C00A 0.0228(7) 0.0265(8) 0.0330(10) 0.0024(7) 0.0011(7) -0.0030(6)
C00B 0.0278(8) 0.0219(7) 0.0329(10) -0.0002(7) -0.0056(7) -0.0014(6)
C00C 0.0196(7) 0.0280(8) 0.0347(10) -0.0001(7) 0.0034(7) -0.0023(6)
C00D 0.0301(8) 0.0287(8) 0.0312(10) -0.0012(7) 0.0000(7) 0.0002(6)
C00E 0.0234(8) 0.0277(8) 0.0370(10) 0.0029(7) 0.0077(7) -0.0001(6)
C00F 0.0155(7) 0.0293(8) 0.0385(10) 0.0077(7) -0.0015(7) -0.0028(6)
C00G 0.0181(7) 0.0304(8) 0.0455(11) 0.0117(8) 0.0030(7) 0.0007(6)
C00H 0.0200(7) 0.0288(8) 0.0397(10) 0.0087(7) -0.0046(7) -0.0048(6)
C00I 0.0311(8) 0.0263(8) 0.0419(11) 0.0052(8) -0.0105(8) -0.0102(7)
C00J 0.0185(7) 0.0335(9) 0.0406(11) -0.0026(8) 0.0023(7) -0.0058(6)
C00K 0.0237(8) 0.0270(8) 0.0473(12) -0.0041(8) 0.0040(8) -0.0085(6)
C00L 0.0274(8) 0.0437(10) 0.0337(10) -0.0021(8) -0.0010(8) -0.0062(7)
C00M 0.0158(7) 0.0463(11) 0.0634(14) 0.0164(10) -0.0013(8) -0.0053(7)
C00N 0.0204(8) 0.0355(9) 0.0516(12) 0.0115(8) -0.0081(8) -0.0098(7)
C00O 0.0377(10) 0.0394(10) 0.0385(11) -0.0072(9) 0.0123(9) -0.0004(8)
C00P 0.0359(10) 0.0332(9) 0.0452(12) 0.0089(9) -0.0148(9) -0.0121(8)
C00Q 0.0404(10) 0.0487(11) 0.0344(11) -0.0119(9) 0.0044(9) -0.0100(9)
C00R 0.0172(7) 0.0386(10) 0.0641(14) 0.0125(9) 0.0052(8) 0.0010(7)
C00S 0.0165(7) 0.0485(11) 0.0545(13) -0.0003(10) -0.0009(8) -0.0004(7)
C3A 0.0766(17) 0.0386(12) 0.0461(14) 0.0114(10) -0.0293(12) -0.0295(11)
C4A 0.123(3) 0.0512(15) 0.0465(16) 0.0031(12) -0.0282(16) -0.0322(16)
N1 0.0436(9) 0.0446(9) 0.0363(10) 0.0063(7) -0.0054(8) -0.0137(7)
N0AA 0.0273(12) 0.0491(16) 0.0534(19) 0.0142(15) 0.0114(13) 0.0107(11)
C3 0.0281(14) 0.0433(17) 0.042(2) -0.0021(14) 0.0075(14) -0.0032(12)
C4 0.0415(17) 0.0464(18) 0.046(2) -0.0089(15) 0.0146(15) -0.0072(13)
C6 0.050(2) 0.055(3) 0.104(4) 0.034(3) 0.027(3) 0.0219(19)
C1 0.0508(14) 0.139(3) 0.0382(14) -0.0115(16) -0.0159(12) 0.0096(16)
C4AA 0.018(2) 0.031(3) 0.027(3) 0.010(2) -0.003(2) 0.0062(19)
C1AA 0.016(2) 0.037(3) 0.019(3) 0.013(2) 0.0070(19) 0.0077(18)
N0AB 0.024(2) 0.033(2) 0.020(2) 0.0016(19) 0.0151(19) 0.0120(17)
C6A 0.047(4) 0.059(5) 0.042(4) 0.007(3) 0.018(3) 0.038(3)
O2A 0.031(2) 0.067(3) 0.025(2) 0.001(2) -0.0016(16) 0.001(2)
C3AA 0.0363(11) 0.0714(16) 0.0690(17) 0.0258(13) -0.0043(11) -0.0151(11)
C0AA 0.026(4) 0.030(3) 0.034(6) 0.003(5) 0.004(4) 0.005(3)
C2 0.0217(19) 0.0314(18) 0.047(4) 0.000(3) 0.005(2) 0.0036(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
O001 C007 1.3644(18) . ?
O001 C00K 1.4236(18) . ?
O002 C00C 1.369(2) . ?
O002 C00S 1.4221(19) . ?
N003 C008 1.406(2) . ?
N003 C00H 1.400(2) . ?
N003 C00I 1.463(2) . ?
N004 C00E 1.402(2) . ?
N004 C00G 1.393(2) . ?
N004 C0AA 1.449(14) . ?
N004 C2 1.493(7) . ?
C006 C007 1.424(2) . ?
C006 C008 1.415(2) . ?
C006 C00J 1.444(2) . ?
C007 C00A 1.381(2) . ?
C008 C00B 1.397(2) . ?
C009 C00C 1.421(2) . ?
C009 C00E 1.414(2) . ?
C009 C00J 1.446(2) . ?
C00A C00D 1.387(2) . ?
C00B C00D 1.381(2) . ?
C00C C00L 1.377(3) . ?
C00E C00O 1.394(3) . ?
C00F C00G 1.405(2) . ?
C00F C00H 1.405(2) . ?
C00F C00J 1.439(2) . ?
C00G C00R 1.404(2) . ?
C00H C00N 1.403(2) . ?
C00I C00P 1.528(3) . ?
C00L C00Q 1.388(3) . ?
C00M C00N 1.379(3) . ?
C00M C00R 1.382(3) . ?
C00O C00Q 1.377(3) . ?
C00P C3A 1.518(3) . ?
C3A N1 1.453(3) . ?
C4A N1 1.453(3) . ?
N1 C1 1.440(3) . ?
N0AA C4 1.452(4) . ?
N0AA C6 1.468(5) . ?
N0AA C3AA 1.421(3) . ?
C3 C4 1.515(4) . ?
C3 C2 1.542(6) . ?
C4AA C1AA 1.500(6) . ?
C4AA C0AA 1.520(13) . ?
C1AA N0AB 1.493(6) . ?
N0AB C6A 1.479(7) . ?
N0AB C3AA 1.607(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
C007 O001 C00K 117.14(13) . . ?
C00C O002 C00S 117.07(14) . . ?
C008 N003 C00I 118.97(15) . . ?
C00H N003 C008 119.66(14) . . ?
C00H N003 C00I 119.36(14) . . ?
C00E N004 C0AA 128.8(5) . . ?
C00E N004 C2 115.6(3) . . ?
C00G N004 C00E 120.32(14) . . ?
C00G N004 C0AA 110.8(5) . . ?
C00G N004 C2 122.5(3) . . ?
C007 C006 C00J 123.77(14) . . ?
C008 C006 C007 117.22(15) . . ?
C008 C006 C00J 118.86(14) . . ?
O001 C007 C006 115.62(14) . . ?
O001 C007 C00A 122.99(14) . . ?
C00A C007 C006 121.36(14) . . ?
N003 C008 C006 118.25(15) . . ?
C00B C008 N003 121.20(15) . . ?
C00B C008 C006 120.54(14) . . ?
C00C C009 C00J 124.54(15) . . ?
C00E C009 C00C 117.16(16) . . ?
C00E C009 C00J 118.27(15) . . ?
C007 C00A C00D 119.16(15) . . ?
C00D C00B C008 119.64(15) . . ?
O002 C00C C009 114.90(15) . . ?
O002 C00C C00L 123.48(15) . . ?
C00L C00C C009 121.60(16) . . ?
C00B C00D C00A 121.47(17) . . ?
N004 C00E C009 119.01(16) . . ?
C00O C00E N004 120.75(16) . . ?
C00O C00E C009 120.22(16) . . ?
C00G C00F C00J 119.84(16) . . ?
C00H C00F C00G 120.07(15) . . ?
C00H C00F C00J 120.07(16) . . ?
N004 C00G C00F 118.32(14) . . ?
N004 C00G C00R 122.26(17) . . ?
C00R C00G C00F 119.42(18) . . ?
N003 C00H C00F 117.77(14) . . ?
N003 C00H C00N 122.59(16) . . ?
C00N C00H C00F 119.61(17) . . ?
N003 C00I C00P 114.29(14) . . ?
C006 C00J C009 128.29(14) . . ?
C00F C00J C006 115.53(15) . . ?
C00F C00J C009 116.12(16) . . ?
C00C C00L C00Q 119.18(17) . . ?
C00N C00M C00R 121.87(16) . . ?
C00M C00N C00H 119.44(18) . . ?
C00Q C00O C00E 120.18(17) . . ?
C3A C00P C00I 110.37(16) . . ?
C00O C00Q C00L 121.05(18) . . ?
C00M C00R C00G 119.53(18) . . ?
N1 C3A C00P 113.07(17) . . ?
C4A N1 C3A 110.27(18) . . ?
C1 N1 C3A 110.5(2) . . ?
C1 N1 C4A 110.0(2) . . ?
C4 N0AA C6 111.2(3) . . ?
C3AA N0AA C4 111.0(3) . . ?
C3AA N0AA C6 103.9(3) . . ?
C4 C3 C2 111.8(4) . . ?
N0AA C4 C3 112.2(3) . . ?
C1AA C4AA C0AA 108.8(6) . . ?
N0AB C1AA C4AA 114.6(4) . . ?
C1AA N0AB C3AA 102.9(4) . . ?
C6A N0AB C1AA 109.4(4) . . ?
C6A N0AB C3AA 117.8(5) . . ?
N004 C0AA C4AA 112.2(8) . . ?
N004 C2 C3 115.6(4) . . ?
_shelx_res_file
;
TITL 20191017_gianetti_1_0ma_a.res in Pbca
20191017_gianetti_1_0ma.res
created by SHELXL-2018/3 at 14:06:27 on 30-Oct-2019
REM Old TITL 20191017_gianetti_1_0ma_a.res in Pbca
REM SHELXT solution in Pbca: R1 0.210, Rweak 0.021, Alpha 0.040
REM 0.669 for 634 systematic absences, Orientation as input
REM Formula found by SHELXT: C33 N3 O2
CELL 1.34138 20.1829 10.7314 25.5707 90 90 90
ZERR 8 0.0005 0.0003 0.0007 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N O
DISP C 0.0148 0.007 57.7277
DISP H -0 0 0.6481
DISP N 0.0253 0.0136 110.4733
DISP O 0.0412 0.025 193.8859
UNIT 247.63 316.4 32 18.67
DFIX 1.47 0.01 C3AA N0AB
SADI N0AA C4 N0AB C1AA
SADI N0AA C6 N0AB C6A
SADI C3 C4 C4AA C1AA
SADI 0.04 N0AA C3 N0AB C4AA
SADI 0.04 C4 C6 C1AA C6A
L.S. 20 0 0
PLAN 20
SIZE 0.12 0.1 0.05
TEMP -173.15
FREE H4b O2A
BOND
list 4
fmap 2 53
acta
REM
REM
REM
WGHT 0.052800 3.141000
FVAR 0.34114 0.02344
O001 4 0.450569 0.696937 0.245455 11.00000 0.01808 0.02109 =
0.03840 -0.00304 0.00276 -0.00409
O002 4 0.480786 0.524999 0.322769 11.00000 0.01660 0.03189 =
0.04253 -0.00490 -0.00149 0.00182
N003 3 0.300771 0.357162 0.224863 11.00000 0.02276 0.02541 =
0.03869 0.00220 -0.00541 -0.00868
N004 3 0.262114 0.675051 0.353479 11.00000 0.02040 0.03117 =
0.04586 0.00346 0.00891 0.00236
C006 1 0.382306 0.519007 0.239391 11.00000 0.01477 0.02009 =
0.03050 0.00215 -0.00370 0.00083
C007 1 0.435924 0.590102 0.218939 11.00000 0.01664 0.01871 =
0.03070 0.00129 -0.00384 0.00082
C008 1 0.358217 0.419904 0.208258 11.00000 0.01997 0.01994 =
0.03321 0.00545 -0.00567 -0.00159
C009 1 0.374640 0.611886 0.333159 11.00000 0.01944 0.02499 =
0.03219 0.00144 0.00341 -0.00240
C00A 1 0.469050 0.553676 0.174218 11.00000 0.02281 0.02654 =
0.03304 0.00244 0.00106 -0.00304
AFIX 43
H00A 2 0.506428 0.599244 0.162211 11.00000 -1.20000
AFIX 0
C00B 1 0.391667 0.384160 0.162861 11.00000 0.02777 0.02190 =
0.03288 -0.00017 -0.00558 -0.00137
AFIX 43
H00B 2 0.376410 0.315134 0.142960 11.00000 -1.20000
AFIX 0
C00C 1 0.441919 0.607956 0.349442 11.00000 0.01956 0.02797 =
0.03467 -0.00008 0.00344 -0.00231
C00D 1 0.447054 0.449716 0.147055 11.00000 0.03006 0.02867 =
0.03121 -0.00121 0.00001 0.00022
AFIX 43
H00D 2 0.470610 0.423009 0.116906 11.00000 -1.20000
AFIX 0
C00E 1 0.330051 0.680209 0.364721 11.00000 0.02341 0.02774 =
0.03701 0.00286 0.00774 -0.00009
C00F 1 0.279856 0.513695 0.289889 11.00000 0.01549 0.02926 =
0.03848 0.00771 -0.00152 -0.00276
C00G 1 0.236574 0.578177 0.323363 11.00000 0.01809 0.03037 =
0.04550 0.01165 0.00300 0.00066
C00H 1 0.255653 0.417825 0.257723 11.00000 0.02002 0.02884 =
0.03972 0.00870 -0.00457 -0.00475
C00I 1 0.280102 0.244439 0.197100 11.00000 0.03109 0.02632 =
0.04187 0.00519 -0.01047 -0.01024
AFIX 23
H00C 2 0.251192 0.194810 0.220432 11.00000 -1.20000
H00E 2 0.319881 0.193708 0.189363 11.00000 -1.20000
AFIX 0
C00J 1 0.348707 0.548046 0.287741 11.00000 0.01847 0.03352 =
0.04062 -0.00256 0.00229 -0.00581
C00K 1 0.510369 0.759266 0.231759 11.00000 0.02372 0.02700 =
0.04734 -0.00409 0.00405 -0.00849
AFIX 137
H00F 2 0.507389 0.789065 0.195608 11.00000 -1.50000
H00G 2 0.547702 0.701381 0.234981 11.00000 -1.50000
H00H 2 0.517181 0.830257 0.255259 11.00000 -1.50000
AFIX 0
C00L 1 0.464773 0.680652 0.389963 11.00000 0.02737 0.04371 =
0.03373 -0.00212 -0.00099 -0.00621
AFIX 43
H00L 2 0.510381 0.679945 0.399146 11.00000 -1.20000
AFIX 0
C00M 1 0.147006 0.447621 0.294038 11.00000 0.01576 0.04629 =
0.06343 0.01641 -0.00134 -0.00529
AFIX 43
H00M 2 0.101721 0.423931 0.295995 11.00000 -1.20000
AFIX 0
C00N 1 0.188625 0.383867 0.260658 11.00000 0.02042 0.03554 =
0.05160 0.01146 -0.00809 -0.00977
AFIX 43
H00N 2 0.172048 0.317523 0.239829 11.00000 -1.20000
AFIX 0
C00O 1 0.353703 0.753427 0.405685 11.00000 0.03770 0.03943 =
0.03846 -0.00722 0.01225 -0.00044
AFIX 43
H00O 2 0.323772 0.802375 0.425689 11.00000 -1.20000
AFIX 0
C00P 1 0.243104 0.269043 0.145987 11.00000 0.03592 0.03319 =
0.04522 0.00887 -0.01485 -0.01214
C00Q 1 0.420345 0.755015 0.417245 11.00000 0.04037 0.04873 =
0.03441 -0.01187 0.00437 -0.00998
AFIX 43
H00Q 2 0.436165 0.807836 0.444317 11.00000 -1.20000
AFIX 0
C00R 1 0.169307 0.544975 0.324716 11.00000 0.01716 0.03861 =
0.06407 0.01247 0.00515 0.00098
AFIX 43
H00R 2 0.139338 0.589125 0.346566 11.00000 -1.20000
AFIX 0
C00S 1 0.549952 0.527615 0.333330 11.00000 0.01648 0.04849 =
0.05451 -0.00035 -0.00087 -0.00037
AFIX 137
H00K 2 0.572693 0.468214 0.310414 11.00000 -1.50000
H00P 2 0.557715 0.504765 0.369927 11.00000 -1.50000
H00S 2 0.567111 0.611671 0.326928 11.00000 -1.50000
AFIX 0
PART 2
C3A 1 0.228928 0.147340 0.117902 -21.00000 0.07659 0.03865 =
0.04609 0.01140 -0.02928 -0.02946
AFIX 23
H3AA 2 0.268654 0.093448 0.119950 -21.00000 -1.20000
H3AB 2 0.192268 0.103853 0.136029 -21.00000 -1.20000
AFIX 0
C4A 1 0.205004 0.044584 0.037405 -21.00000 0.12337 0.05124 =
0.04649 0.00312 -0.02820 -0.03222
AFIX 137
H4AA 2 0.246896 -0.001032 0.040404 -21.00000 -1.50000
H4AB 2 0.194477 0.057508 0.000386 -21.00000 -1.50000
H4AC 2 0.169498 -0.003633 0.053956 -21.00000 -1.50000
AFIX 0
PART 0
N1 3 0.211141 0.164529 0.063299 11.00000 0.04358 0.04464 =
0.03631 0.00629 -0.00536 -0.01368
PART 1
N0AA 3 0.080610 0.748230 0.440008 10.66670 0.02726 0.04905 =
0.05341 0.01419 0.01135 0.01073
C3 1 0.200860 0.709535 0.440323 10.66670 0.02814 0.04333 =
0.04206 -0.00208 0.00746 -0.00321
AFIX 23
H3A 2 0.188888 0.620274 0.437808 10.66670 -1.20000
H3B 2 0.239880 0.716650 0.463593 10.66670 -1.20000
AFIX 0
C4 1 0.143476 0.781089 0.463916 10.66670 0.04155 0.04641 =
0.04618 -0.00893 0.01459 -0.00720
H4A 2 0.151397 0.877977 0.451807 10.66670 -1.20000
C6 1 0.030772 0.845694 0.448754 10.66670 0.04979 0.05510 =
0.10425 0.03402 0.02675 0.02192
AFIX 137
H6A 2 0.021886 0.853224 0.486299 10.66670 -1.50000
H6B 2 -0.010235 0.823583 0.430448 10.66670 -1.50000
H6C 2 0.047400 0.925329 0.435352 10.66670 -1.50000
AFIX 0
PART 0
C1 1 0.149947 0.232724 0.058946 11.00000 0.05083 0.13859 =
0.03823 -0.01149 -0.01585 0.00963
AFIX 137
H1A 2 0.114574 0.186805 0.076776 11.00000 -1.50000
H1B 2 0.138501 0.242876 0.021945 11.00000 -1.50000
H1C 2 0.155118 0.314904 0.075153 11.00000 -1.50000
AFIX 0
PART 2
C4AA 1 0.175987 0.731714 0.417569 10.33333 0.01770 0.03144 =
0.02689 0.01045 -0.00342 0.00618
AFIX 23
H4AD 2 0.165118 0.641771 0.418304 10.33333 -1.20000
H4AE 2 0.205463 0.750245 0.447522 10.33333 -1.20000
AFIX 0
C1AA 1 0.113727 0.807346 0.421672 10.33333 0.01642 0.03696 =
0.01888 0.01269 0.00696 0.00774
AFIX 23
H1AA 2 0.125615 0.896785 0.420248 10.33333 -1.20000
H1AB 2 0.085531 0.789100 0.390931 10.33333 -1.20000
AFIX 0
N0AB 3 0.074234 0.784507 0.470086 10.33333 0.02358 0.03323 =
0.02039 0.00163 0.01506 0.01200
C6A 1 0.021056 0.878871 0.474016 10.33333 0.04699 0.05862 =
0.04217 0.00704 0.01821 0.03756
AFIX 137
H6AA 2 -0.006860 0.875089 0.442698 10.33333 -1.50000
H6AB 2 0.040805 0.962011 0.476914 10.33333 -1.50000
H6AC 2 -0.006013 0.862040 0.505039 10.33333 -1.50000
AFIX 0
PART 0
H00I 2 0.268739 0.322451 0.124340 11.00000 0.02892
H00J 2 0.202239 0.313524 0.152546 11.00000 0.05530
PART 2
AFIX 6
O2A 4 0.144135 0.820982 0.565475 10.33333 0.03126 0.06727 =
0.02495 0.00066 -0.00163 0.00150
H2AA 2 0.126980 0.832420 0.534644 10.33333 -1.50000
H2AB 2 0.186636 0.817459 0.559939 10.33333 -1.50000
AFIX 0
PART 0
C3AA 1 0.052785 0.641018 0.464140 11.00000 0.03626 0.07137 =
0.06897 0.02582 -0.00431 -0.01512
PART 1
AFIX 137
H3AC 2 0.083954 0.571300 0.461399 10.66670 -1.50000
H3AD 2 0.011234 0.619107 0.446571 10.66670 -1.50000
H3AE 2 0.043982 0.658720 0.501091 10.66670 -1.50000
AFIX 137
PART 0
PART 2
H3AF 2 0.019318 0.633440 0.436556 10.33333 -1.50000
H3AG 2 0.034303 0.611225 0.497301 10.33333 -1.50000
H3AH 2 0.091654 0.590870 0.454937 10.33333 -1.50000
AFIX 0
PART 0
PART 1
H4B 2 0.139864 0.762559 0.505833 10.66670 0.04192
PART 0
PART 2
C0AA 1 0.210697 0.764005 0.366597 10.33333 0.02552 0.02975 =
0.03393 0.00332 0.00376 0.00475
AFIX 23
H0AA 2 0.177635 0.766312 0.338013 10.33333 -1.20000
H0AB 2 0.230550 0.848064 0.369583 10.33333 -1.20000
AFIX 0
PART 0
PART 1
C2 1 0.219129 0.758600 0.385515 10.66670 0.02171 0.03145 =
0.04681 -0.00014 0.00523 0.00359
AFIX 23
H2A 2 0.177635 0.774133 0.365924 10.66670 -1.20000
H2B 2 0.241978 0.839647 0.389616 10.66670 -1.20000
AFIX 0
HKLF 4
REM 20191017_gianetti_1_0ma_a.res in Pbca
REM wR2 = 0.1505, GooF = S = 1.095, Restrained GooF = 1.109 for all data
REM R1 = 0.0669 for 5594 Fo > 4sig(Fo) and 0.0906 for all 7238 data
REM 414 parameters refined using 6 restraints
END
WGHT 0.0528 3.1406
REM Highest difference peak 0.535, deepest hole -0.246, 1-sigma level 0.050
Q1 1 0.3592 0.4846 0.3008 11.00000 0.05 0.54
Q2 1 0.2221 0.0752 0.1371 11.00000 0.05 0.23
Q3 1 0.3763 0.4671 0.2227 11.00000 0.05 0.20
Q4 1 0.2013 0.5683 0.3258 11.00000 0.05 0.18
Q5 1 0.2384 -0.1568 0.0415 11.00000 0.05 0.16
Q6 1 0.2622 0.4826 0.2615 11.00000 0.05 0.16
Q7 1 0.4013 0.5631 0.2222 11.00000 0.05 0.16
Q8 1 0.2205 0.4210 0.2479 11.00000 0.05 0.16
Q9 1 0.0195 0.5945 0.4387 11.00000 0.05 0.16
Q10 1 0.3156 0.5246 0.2846 11.00000 0.05 0.15
Q11 1 0.4799 0.9431 0.2735 11.00000 0.05 0.15
Q12 1 0.2982 0.2757 0.0967 11.00000 0.05 0.15
Q13 1 0.1354 0.8986 0.3157 11.00000 0.05 0.15
Q14 1 0.4203 0.4189 0.1586 11.00000 0.05 0.15
Q15 1 0.2206 0.4446 0.1838 11.00000 0.05 0.15
Q16 1 0.1644 0.3015 -0.0006 11.00000 0.05 0.15
Q17 1 0.5004 0.8407 0.2737 11.00000 0.05 0.14
Q18 1 0.1655 0.3527 0.0563 11.00000 0.05 0.14
Q19 1 0.4159 0.5397 0.2396 11.00000 0.05 0.14
Q20 1 0.4824 0.8072 0.4722 11.00000 0.05 0.14
;
_shelx_res_checksum 38980
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/hexanes'
_chemical_properties_physical Air-sensitive
#######################################################################
#
# 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_2-NO2cation
_database_code_depnum_ccdc_archive 'CCDC 2004975'
loop_
_audit_author_name
_audit_author_address
'thomas l gianetti'
;University of Arizona
United States of America
;
_audit_update_record
;
2020-05-20 deposited with the CCDC. 2020-09-14 downloaded from the CCDC.
;
_audit_creation_date 2019-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common 2-NO2cation
_chemical_name_systematic 2-NO2cation
_chemical_formula_moiety 'B F4, C31 H38 N5 O4'
_chemical_formula_sum 'C31 H39 B F4 N5 O4'
_chemical_formula_weight 632.48
_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 0.0148 0.0070 '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'
B B 0.0070 0.0029 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0583 0.0400 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 '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 15
_space_group_name_H-M_alt 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 22.4230(7)
_cell_length_b 11.1591(4)
_cell_length_c 26.6457(11)
_cell_angle_alpha 90
_cell_angle_beta 113.7260(10)
_cell_angle_gamma 90
_cell_volume 6103.8(4)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 9744
_cell_measurement_temperature 100.0
_cell_measurement_theta_max 73.18
_cell_measurement_theta_min 3.92
_shelx_estimated_absorpt_T_max 0.977
_shelx_estimated_absorpt_T_min 0.955
_exptl_absorpt_coefficient_mu 0.582
_exptl_absorpt_correction_T_max 0.7537
_exptl_absorpt_correction_T_min 0.6401
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0834 before and 0.0551 after correction. The Ratio of minimum to maximum transmission is 0.8493. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'metallic dark red'
_exptl_crystal_colour_lustre metallic
_exptl_crystal_colour_modifier dark
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.377
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 2664
_exptl_crystal_preparation ?
_exptl_crystal_recrystallization_method 'from acetonitrile ether layering'
_exptl_crystal_size_max 0.08
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.04
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0371
_diffrn_reflns_av_unetI/netI 0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max 31
_diffrn_reflns_limit_h_min -32
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 36
_diffrn_reflns_limit_l_min -38
_diffrn_reflns_number 72727
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full 53.594
_diffrn_reflns_theta_max 73.298
_diffrn_reflns_theta_min 3.923
_diffrn_ambient_temperature 100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type GaK\a
_diffrn_radiation_wavelength 1.34138
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 8589
_reflns_number_total 9160
_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 'SAINT V8.40A (?, 2016)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.40A (?, 2016)'
_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 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.337
_refine_diff_density_min -0.271
_refine_diff_density_rms 0.047
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.965
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 412
_refine_ls_number_reflns 9160
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0427
_refine_ls_R_factor_gt 0.0405
_refine_ls_restrained_S_all 0.965
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+5.1492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1094
_refine_ls_wR_factor_ref 0.1114
_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.a Secondary CH2 refined with riding coordinates:
C00Q(H00A,H00B), C00S(H00C,H00D), C00X(H00F,H00G), C00Z(H00H,H00I), C011(H01A,
H01B), C012(H01C,H01D)
2.b Aromatic/amide H refined with riding coordinates:
C00E(H00E), C00R(H00R), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W),
C00Y(H00Y), C010(H010)
2.c Idealised Me refined as rotating group:
C013(H01E,H01F,H01G), C014(H01H,H01I,H01J), C015(H01K,H01L,H01M), C016(H01N,
H01O,H01P), C017(H01Q,H01R,H01S), C018(H01T,H01U,H01V)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_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
F001 F 0.66233(4) 0.75770(7) 0.70744(3) 0.03669(16) Uani 1 1 d . . . . .
F002 F 0.57018(3) 0.66857(7) 0.64678(3) 0.03785(17) Uani 1 1 d . . . . .
F003 F 0.65648(4) 0.55488(7) 0.70006(3) 0.03868(17) Uani 1 1 d . . . . .
O004 O 0.51603(3) 0.69601(6) 0.34371(3) 0.02178(14) Uani 1 1 d . . . . .
F005 F 0.59597(4) 0.65305(7) 0.73796(3) 0.04144(19) Uani 1 1 d . . . . .
O006 O 0.60976(3) 0.53395(6) 0.38709(3) 0.02270(14) Uani 1 1 d . . . . .
O007 O 0.84918(3) 0.98418(7) 0.45305(3) 0.02603(15) Uani 1 1 d . . . . .
O008 O 0.84755(4) 1.14203(7) 0.50028(3) 0.02932(17) Uani 1 1 d . . . . .
N009 N 0.71979(3) 0.90160(7) 0.39329(3) 0.01498(13) Uani 1 1 d . . . . .
N00A N 0.63062(3) 0.82701(7) 0.52719(3) 0.01507(13) Uani 1 1 d . . . . .
N00B N 0.82419(4) 1.04632(7) 0.47764(3) 0.01947(15) Uani 1 1 d . . . . .
N00C N 0.67057(4) 1.08374(7) 0.63564(3) 0.02205(16) Uani 1 1 d . . . . .
N00D N 0.59365(4) 1.03687(8) 0.36532(4) 0.02542(17) Uani 1 1 d . . . . .
C00E C 0.71365(4) 0.97932(8) 0.54548(3) 0.01641(15) Uani 1 1 d . . . . .
H00E H 0.709801 1.001928 0.578420 0.020 Uiso 1 1 calc R . . . .
C00F C 0.58024(4) 0.73727(7) 0.43672(4) 0.01563(15) Uani 1 1 d . . . . .
C00G C 0.67780(4) 0.85831(7) 0.46141(3) 0.01296(14) Uani 1 1 d . . . . .
C00H C 0.67356(4) 0.88863(7) 0.51189(3) 0.01364(14) Uani 1 1 d . . . . .
C00I C 0.72346(4) 0.91976(7) 0.44525(3) 0.01343(14) Uani 1 1 d . . . . .
C00J C 0.69415(4) 0.79472(8) 0.36650(3) 0.01580(15) Uani 1 1 d . . . . .
C00K C 0.63564(4) 0.77159(7) 0.42624(3) 0.01380(14) Uani 1 1 d . . . . .
C00L C 0.58190(4) 0.75663(8) 0.49004(4) 0.01634(15) Uani 1 1 d . . . . .
C00M C 0.65428(4) 0.72341(8) 0.38451(3) 0.01540(15) Uani 1 1 d . . . . .
C00N C 0.76565(4) 1.00263(8) 0.48230(3) 0.01575(15) Uani 1 1 d . . . . .
C00O C 0.63790(4) 0.60583(8) 0.36192(4) 0.01866(16) Uani 1 1 d . . . . .
C00P C 0.52251(4) 0.68431(8) 0.39618(4) 0.01893(16) Uani 1 1 d . . . . .
C00Q C 0.63443(4) 0.83860(8) 0.58397(3) 0.01811(16) Uani 1 1 d . . . . .
H00A H 0.679137 0.863472 0.608377 0.022 Uiso 1 1 calc R . . . .
H00B H 0.626424 0.759043 0.596502 0.022 Uiso 1 1 calc R . . . .
C00R C 0.75823(4) 1.03454(8) 0.53008(3) 0.01703(15) Uani 1 1 d . . . . .
H00R H 0.784837 1.096293 0.552578 0.020 Uiso 1 1 calc R . . . .
C00S C 0.73113(5) 1.00087(8) 0.36101(4) 0.01988(17) Uani 1 1 d . . . . .
H00C H 0.760922 0.973033 0.344313 0.024 Uiso 1 1 calc R . . . .
H00D H 0.752434 1.068436 0.385844 0.024 Uiso 1 1 calc R . . . .
C00T C 0.47670(4) 0.63160(9) 0.41143(4) 0.02394(19) Uani 1 1 d . . . . .
H00T H 0.440410 0.590637 0.385168 0.029 Uiso 1 1 calc R . . . .
C00U C 0.65465(5) 0.56862(9) 0.31987(4) 0.02271(18) Uani 1 1 d . . . . .
H00U H 0.642820 0.490876 0.304544 0.027 Uiso 1 1 calc R . . . .
C00V C 0.53423(4) 0.70315(9) 0.50494(4) 0.02179(17) Uani 1 1 d . . . . .
H00V H 0.536520 0.711119 0.541163 0.026 Uiso 1 1 calc R . . . .
C00W C 0.70924(4) 0.75769(9) 0.32243(4) 0.01966(16) Uani 1 1 d . . . . .
H00W H 0.732863 0.808749 0.308457 0.024 Uiso 1 1 calc R . . . .
C00X C 0.58602(5) 0.92856(9) 0.58982(4) 0.02169(17) Uani 1 1 d . . . . .
H00F H 0.543690 0.918410 0.558189 0.026 Uiso 1 1 calc R . . . .
H00G H 0.579248 0.908347 0.623324 0.026 Uiso 1 1 calc R . . . .
C00Y C 0.68911(5) 0.64606(9) 0.30000(4) 0.02243(18) Uani 1 1 d . . . . .
H00Y H 0.698929 0.620924 0.270112 0.027 Uiso 1 1 calc R . . . .
C00Z C 0.66750(5) 1.04460(9) 0.31577(4) 0.02354(18) Uani 1 1 d . . . . .
H00H H 0.677806 1.096898 0.290323 0.028 Uiso 1 1 calc R . . . .
H00I H 0.642842 0.974703 0.294664 0.028 Uiso 1 1 calc R . . . .
C010 C 0.48444(5) 0.63931(9) 0.46610(5) 0.02522(19) Uani 1 1 d . . . . .
H010 H 0.454166 0.598923 0.476849 0.030 Uiso 1 1 calc R . . . .
C011 C 0.60574(5) 1.06043(9) 0.59304(4) 0.02316(18) Uani 1 1 d . . . . .
H01A H 0.604913 1.085535 0.557130 0.028 Uiso 1 1 calc R . . . .
H01B H 0.573402 1.109546 0.600441 0.028 Uiso 1 1 calc R . . . .
C012 C 0.62488(5) 1.11376(9) 0.33830(4) 0.02389(18) Uani 1 1 d . . . . .
H01C H 0.652011 1.174181 0.364897 0.029 Uiso 1 1 calc R . . . .
H01D H 0.590716 1.157089 0.307797 0.029 Uiso 1 1 calc R . . . .
C013 C 0.45646(5) 0.65559(11) 0.30134(5) 0.0302(2) Uani 1 1 d . . . . .
H01E H 0.456180 0.676089 0.265485 0.045 Uiso 1 1 calc GR . . . .
H01F H 0.419549 0.694492 0.305536 0.045 Uiso 1 1 calc GR . . . .
H01G H 0.452867 0.568505 0.303995 0.045 Uiso 1 1 calc GR . . . .
C014 C 0.58087(6) 0.42463(9) 0.36001(5) 0.0329(2) Uani 1 1 d . . . . .
H01H H 0.551223 0.441934 0.322074 0.049 Uiso 1 1 calc GR . . . .
H01I H 0.556481 0.387286 0.379234 0.049 Uiso 1 1 calc GR . . . .
H01J H 0.615140 0.369894 0.360213 0.049 Uiso 1 1 calc GR . . . .
C015 C 0.67423(6) 1.06082(10) 0.69073(4) 0.0292(2) Uani 1 1 d . . . . .
H01K H 0.642236 1.110864 0.697389 0.044 Uiso 1 1 calc GR . . . .
H01L H 0.718060 1.080080 0.717710 0.044 Uiso 1 1 calc GR . . . .
H01M H 0.664845 0.976138 0.694077 0.044 Uiso 1 1 calc GR . . . .
C016 C 0.69159(6) 1.20593(10) 0.63179(5) 0.0319(2) Uani 1 1 d . . . . .
H01N H 0.689478 1.219944 0.594807 0.048 Uiso 1 1 calc GR . . . .
H01O H 0.736462 1.217104 0.658628 0.048 Uiso 1 1 calc GR . . . .
H01P H 0.662925 1.262778 0.639360 0.048 Uiso 1 1 calc GR . . . .
C017 C 0.57872(6) 1.10297(12) 0.40611(5) 0.0361(3) Uani 1 1 d . . . . .
H01Q H 0.618520 1.140576 0.432416 0.054 Uiso 1 1 calc GR . . . .
H01R H 0.561342 1.047719 0.425484 0.054 Uiso 1 1 calc GR . . . .
H01S H 0.546282 1.164990 0.387820 0.054 Uiso 1 1 calc GR . . . .
C018 C 0.53445(6) 0.98339(11) 0.32561(6) 0.0400(3) Uani 1 1 d . . . . .
H01T H 0.503803 1.046824 0.305771 0.060 Uiso 1 1 calc GR . . . .
H01U H 0.514637 0.932397 0.344667 0.060 Uiso 1 1 calc GR . . . .
H01V H 0.544935 0.934852 0.299597 0.060 Uiso 1 1 calc GR . . . .
B019 B 0.62127(6) 0.65915(10) 0.69835(5) 0.0237(2) Uani 1 1 d . . . . .
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
F001 0.0424(4) 0.0315(3) 0.0357(4) -0.0010(3) 0.0152(3) -0.0111(3)
F002 0.0308(3) 0.0483(4) 0.0316(3) 0.0114(3) 0.0095(3) -0.0080(3)
F003 0.0470(4) 0.0305(3) 0.0488(4) 0.0065(3) 0.0300(4) 0.0109(3)
O004 0.0141(3) 0.0233(3) 0.0225(3) -0.0047(2) 0.0017(2) -0.0040(2)
F005 0.0627(5) 0.0388(4) 0.0415(4) 0.0169(3) 0.0404(4) 0.0154(3)
O006 0.0217(3) 0.0135(3) 0.0301(3) -0.0042(2) 0.0075(3) -0.0035(2)
O007 0.0176(3) 0.0299(4) 0.0357(4) -0.0052(3) 0.0161(3) -0.0038(3)
O008 0.0295(4) 0.0302(4) 0.0330(4) -0.0104(3) 0.0176(3) -0.0183(3)
N009 0.0151(3) 0.0166(3) 0.0152(3) -0.0010(2) 0.0082(2) -0.0013(2)
N00A 0.0133(3) 0.0175(3) 0.0162(3) 0.0020(2) 0.0078(2) -0.0018(2)
N00B 0.0151(3) 0.0232(4) 0.0215(3) -0.0017(3) 0.0089(3) -0.0064(3)
N00C 0.0280(4) 0.0200(4) 0.0217(4) 0.0005(3) 0.0137(3) 0.0001(3)
N00D 0.0227(4) 0.0246(4) 0.0300(4) 0.0071(3) 0.0117(3) 0.0044(3)
C00E 0.0146(3) 0.0210(4) 0.0137(3) -0.0017(3) 0.0057(3) -0.0032(3)
C00F 0.0117(3) 0.0140(3) 0.0206(4) 0.0001(3) 0.0058(3) -0.0017(3)
C00G 0.0104(3) 0.0142(3) 0.0144(3) 0.0003(3) 0.0051(3) -0.0010(3)
C00H 0.0109(3) 0.0164(3) 0.0144(3) 0.0016(3) 0.0058(3) -0.0009(3)
C00I 0.0114(3) 0.0151(3) 0.0149(3) -0.0001(3) 0.0064(3) -0.0006(3)
C00J 0.0132(3) 0.0175(4) 0.0158(3) -0.0020(3) 0.0048(3) 0.0019(3)
C00K 0.0111(3) 0.0133(3) 0.0157(3) 0.0003(3) 0.0041(3) -0.0001(3)
C00L 0.0128(3) 0.0155(3) 0.0216(4) 0.0025(3) 0.0078(3) -0.0013(3)
C00M 0.0127(3) 0.0152(3) 0.0169(3) -0.0023(3) 0.0045(3) 0.0005(3)
C00N 0.0120(3) 0.0186(4) 0.0176(4) -0.0009(3) 0.0071(3) -0.0042(3)
C00O 0.0145(3) 0.0157(4) 0.0211(4) -0.0029(3) 0.0022(3) 0.0012(3)
C00P 0.0131(3) 0.0156(4) 0.0251(4) -0.0015(3) 0.0046(3) -0.0014(3)
C00Q 0.0191(4) 0.0219(4) 0.0164(4) 0.0044(3) 0.0103(3) 0.0008(3)
C00R 0.0146(3) 0.0199(4) 0.0159(3) -0.0026(3) 0.0053(3) -0.0044(3)
C00S 0.0244(4) 0.0200(4) 0.0208(4) 0.0010(3) 0.0148(3) -0.0023(3)
C00T 0.0134(3) 0.0195(4) 0.0361(5) -0.0013(4) 0.0070(3) -0.0050(3)
C00U 0.0194(4) 0.0204(4) 0.0216(4) -0.0072(3) 0.0012(3) 0.0040(3)
C00V 0.0182(4) 0.0212(4) 0.0296(4) 0.0041(3) 0.0135(3) -0.0033(3)
C00W 0.0179(4) 0.0245(4) 0.0170(4) -0.0025(3) 0.0075(3) 0.0037(3)
C00X 0.0210(4) 0.0250(4) 0.0240(4) 0.0016(3) 0.0143(3) 0.0007(3)
C00Y 0.0202(4) 0.0266(4) 0.0171(4) -0.0057(3) 0.0040(3) 0.0071(3)
C00Z 0.0327(5) 0.0216(4) 0.0182(4) 0.0026(3) 0.0122(4) 0.0018(4)
C010 0.0167(4) 0.0215(4) 0.0395(5) 0.0046(4) 0.0134(4) -0.0041(3)
C011 0.0249(4) 0.0233(4) 0.0249(4) 0.0046(3) 0.0138(4) 0.0041(3)
C012 0.0281(4) 0.0190(4) 0.0254(4) 0.0033(3) 0.0116(4) 0.0022(3)
C013 0.0156(4) 0.0374(6) 0.0292(5) -0.0110(4) 0.0003(3) -0.0051(4)
C014 0.0313(5) 0.0177(4) 0.0431(6) -0.0095(4) 0.0082(4) -0.0078(4)
C015 0.0410(6) 0.0287(5) 0.0223(4) -0.0015(4) 0.0174(4) 0.0015(4)
C016 0.0392(6) 0.0230(5) 0.0383(6) -0.0005(4) 0.0207(5) -0.0041(4)
C017 0.0334(5) 0.0424(6) 0.0408(6) 0.0089(5) 0.0237(5) 0.0123(5)
C018 0.0273(5) 0.0286(5) 0.0560(8) 0.0047(5) 0.0082(5) -0.0013(4)
B019 0.0294(5) 0.0226(5) 0.0240(5) 0.0057(4) 0.0157(4) 0.0007(4)
_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
F001 B019 1.3915(13) . ?
F002 B019 1.3946(13) . ?
F003 B019 1.3964(13) . ?
O004 C00P 1.3525(12) . ?
O004 C013 1.4313(11) . ?
F005 B019 1.3864(12) . ?
O006 C00O 1.3534(12) . ?
O006 C014 1.4325(12) . ?
O007 N00B 1.2327(11) . ?
O008 N00B 1.2348(11) . ?
N009 C00I 1.3685(10) . ?
N009 C00J 1.3901(11) . ?
N009 C00S 1.4858(11) . ?
N00A C00H 1.3719(10) . ?
N00A C00L 1.3856(11) . ?
N00A C00Q 1.4864(11) . ?
N00B C00N 1.4517(10) . ?
N00C C011 1.4635(13) . ?
N00C C015 1.4595(12) . ?
N00C C016 1.4596(13) . ?
N00D C012 1.4665(13) . ?
N00D C017 1.4596(15) . ?
N00D C018 1.4518(15) . ?
C00E C00H 1.4091(11) . ?
C00E C00R 1.3701(11) . ?
C00F C00K 1.4307(11) . ?
C00F C00L 1.4227(12) . ?
C00F C00P 1.4374(11) . ?
C00G C00H 1.4266(11) . ?
C00G C00I 1.4350(10) . ?
C00G C00K 1.4126(11) . ?
C00I C00N 1.4047(11) . ?
C00J C00M 1.4171(12) . ?
C00J C00W 1.4085(12) . ?
C00K C00M 1.4403(11) . ?
C00L C00V 1.4134(11) . ?
C00M C00O 1.4285(12) . ?
C00N C00R 1.3948(11) . ?
C00O C00U 1.3813(13) . ?
C00P C00T 1.3791(13) . ?
C00Q C00X 1.5319(13) . ?
C00S C00Z 1.5306(14) . ?
C00T C010 1.3987(16) . ?
C00U C00Y 1.3976(15) . ?
C00V C010 1.3767(14) . ?
C00W C00Y 1.3768(13) . ?
C00X C011 1.5290(14) . ?
C00Z C012 1.5266(14) . ?
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
C00P O004 C013 117.59(8) . . ?
C00O O006 C014 117.50(8) . . ?
C00I N009 C00J 119.39(7) . . ?
C00I N009 C00S 121.37(7) . . ?
C00J N009 C00S 118.30(7) . . ?
C00H N00A C00L 121.18(7) . . ?
C00H N00A C00Q 119.94(7) . . ?
C00L N00A C00Q 118.84(7) . . ?
O007 N00B O008 123.50(8) . . ?
O007 N00B C00N 118.47(8) . . ?
O008 N00B C00N 117.98(8) . . ?
C015 N00C C011 112.65(8) . . ?
C015 N00C C016 110.19(9) . . ?
C016 N00C C011 111.08(8) . . ?
C017 N00D C012 111.58(9) . . ?
C018 N00D C012 111.10(9) . . ?
C018 N00D C017 109.51(10) . . ?
C00R C00E C00H 119.24(8) . . ?
C00K C00F C00P 123.61(8) . . ?
C00L C00F C00K 118.58(7) . . ?
C00L C00F C00P 117.82(7) . . ?
C00H C00G C00I 119.72(7) . . ?
C00K C00G C00H 120.49(7) . . ?
C00K C00G C00I 119.74(7) . . ?
N00A C00H C00E 121.05(7) . . ?
N00A C00H C00G 118.82(7) . . ?
C00E C00H C00G 120.12(7) . . ?
N009 C00I C00G 118.24(7) . . ?
N009 C00I C00N 123.91(7) . . ?
C00N C00I C00G 117.62(7) . . ?
N009 C00J C00M 119.66(7) . . ?
N009 C00J C00W 119.44(8) . . ?
C00W C00J C00M 120.89(8) . . ?
C00F C00K C00M 126.53(7) . . ?
C00G C00K C00F 117.11(7) . . ?
C00G C00K C00M 116.32(7) . . ?
N00A C00L C00F 119.72(7) . . ?
N00A C00L C00V 120.44(8) . . ?
C00V C00L C00F 119.83(8) . . ?
C00J C00M C00K 118.06(7) . . ?
C00J C00M C00O 117.61(8) . . ?
C00O C00M C00K 124.25(8) . . ?
C00I C00N N00B 122.50(7) . . ?
C00R C00N N00B 115.87(7) . . ?
C00R C00N C00I 121.04(7) . . ?
O006 C00O C00M 115.32(8) . . ?
O006 C00O C00U 123.84(8) . . ?
C00U C00O C00M 120.68(9) . . ?
O004 C00P C00F 115.27(8) . . ?
O004 C00P C00T 124.23(8) . . ?
C00T C00P C00F 120.42(9) . . ?
N00A C00Q C00X 114.06(7) . . ?
C00E C00R C00N 121.86(8) . . ?
N009 C00S C00Z 111.79(7) . . ?
C00P C00T C010 119.05(9) . . ?
C00O C00U C00Y 119.58(8) . . ?
C010 C00V C00L 118.92(9) . . ?
C00Y C00W C00J 118.72(9) . . ?
C011 C00X C00Q 115.82(7) . . ?
C00W C00Y C00U 121.99(8) . . ?
C012 C00Z C00S 112.59(8) . . ?
C00V C010 C00T 122.55(9) . . ?
N00C C011 C00X 112.91(8) . . ?
N00D C012 C00Z 113.28(8) . . ?
F001 B019 F002 109.61(8) . . ?
F001 B019 F003 109.10(9) . . ?
F002 B019 F003 108.94(9) . . ?
F005 B019 F001 110.55(9) . . ?
F005 B019 F002 109.15(9) . . ?
F005 B019 F003 109.47(8) . . ?
_shelx_res_file
;
TITL 20191121_gianetti_01_0ma_a.res in C2/c
20191121_gianetti_01_0ma.res
created by SHELXL-2018/3 at 12:03:51 on 22-Nov-2019
REM Old TITL 20191121_gianetti_01_0ma in C2/c
REM SHELXT solution in C2/c: R1 0.151, Rweak 0.005, Alpha 0.030
REM 0.971 for 335 systematic absences, Orientation as input
REM Formula found by SHELXT: C34 N3 O8
CELL 1.34138 22.423 11.1591 26.6457 90 113.726 90
ZERR 8 0.0007 0.0004 0.0011 0 0.001 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H B F N O
DISP C 0.0148 0.007 57.7277
DISP H -0 0 0.6481
DISP N 0.0253 0.0136 110.4733
DISP O 0.0412 0.025 193.8859
UNIT 248 312 8 32 40 32
L.S. 20
PLAN 20
SIZE 0.08 0.07 0.04
TEMP -173.15
BOND
list 4
fmap 2 53
ACTA
REM
REM
REM
WGHT 0.061000 5.149199
FVAR 0.29366
F001 4 0.662331 0.757699 0.707438 11.00000 0.04235 0.03150 =
0.03571 -0.00101 0.01519 -0.01107
F002 4 0.570180 0.668574 0.646783 11.00000 0.03080 0.04828 =
0.03155 0.01140 0.00950 -0.00797
F003 4 0.656478 0.554881 0.700062 11.00000 0.04703 0.03050 =
0.04884 0.00654 0.03002 0.01089
O004 6 0.516025 0.696010 0.343711 11.00000 0.01407 0.02333 =
0.02250 -0.00468 0.00167 -0.00400
F005 4 0.595969 0.653045 0.737956 11.00000 0.06269 0.03880 =
0.04151 0.01687 0.04041 0.01540
O006 6 0.609760 0.533951 0.387088 11.00000 0.02169 0.01351 =
0.03014 -0.00421 0.00753 -0.00353
O007 6 0.849177 0.984179 0.453052 11.00000 0.01765 0.02994 =
0.03566 -0.00516 0.01608 -0.00382
O008 6 0.847549 1.142033 0.500276 11.00000 0.02951 0.03017 =
0.03304 -0.01043 0.01755 -0.01829
N009 5 0.719786 0.901602 0.393292 11.00000 0.01513 0.01662 =
0.01523 -0.00104 0.00822 -0.00126
N00A 5 0.630623 0.827010 0.527189 11.00000 0.01328 0.01749 =
0.01622 0.00199 0.00780 -0.00184
N00B 5 0.824190 1.046316 0.477641 11.00000 0.01511 0.02323 =
0.02154 -0.00168 0.00892 -0.00642
N00C 5 0.670574 1.083743 0.635637 11.00000 0.02800 0.02003 =
0.02169 0.00054 0.01371 0.00013
N00D 5 0.593654 1.036868 0.365319 11.00000 0.02275 0.02463 =
0.02995 0.00706 0.01171 0.00437
C00E 1 0.713646 0.979325 0.545477 11.00000 0.01461 0.02101 =
0.01365 -0.00173 0.00575 -0.00325
AFIX 43
H00E 2 0.709801 1.001928 0.578420 11.00000 -1.20000
AFIX 0
C00F 1 0.580238 0.737271 0.436719 11.00000 0.01165 0.01397 =
0.02060 0.00011 0.00579 -0.00170
C00G 1 0.677796 0.858305 0.461415 11.00000 0.01043 0.01420 =
0.01438 0.00028 0.00511 -0.00097
C00H 1 0.673565 0.888631 0.511890 11.00000 0.01087 0.01642 =
0.01435 0.00157 0.00582 -0.00092
C00I 1 0.723460 0.919759 0.445249 11.00000 0.01137 0.01511 =
0.01490 -0.00009 0.00643 -0.00057
C00J 1 0.694152 0.794721 0.366501 11.00000 0.01316 0.01750 =
0.01579 -0.00196 0.00482 0.00191
C00K 1 0.635641 0.771587 0.426242 11.00000 0.01110 0.01333 =
0.01571 0.00033 0.00407 -0.00007
C00L 1 0.581899 0.756634 0.490038 11.00000 0.01278 0.01553 =
0.02157 0.00250 0.00781 -0.00128
C00M 1 0.654278 0.723406 0.384506 11.00000 0.01273 0.01518 =
0.01688 -0.00227 0.00448 0.00053
C00N 1 0.765646 1.002631 0.482303 11.00000 0.01204 0.01864 =
0.01764 -0.00092 0.00709 -0.00415
C00O 1 0.637902 0.605833 0.361923 11.00000 0.01448 0.01573 =
0.02105 -0.00289 0.00225 0.00120
C00P 1 0.522513 0.684310 0.396183 11.00000 0.01311 0.01563 =
0.02511 -0.00147 0.00463 -0.00145
C00Q 1 0.634433 0.838601 0.583974 11.00000 0.01905 0.02193 =
0.01641 0.00439 0.01032 0.00082
AFIX 23
H00A 2 0.679137 0.863472 0.608377 11.00000 -1.20000
H00B 2 0.626424 0.759043 0.596502 11.00000 -1.20000
AFIX 0
C00R 1 0.758227 1.034536 0.530079 11.00000 0.01455 0.01990 =
0.01589 -0.00265 0.00533 -0.00444
AFIX 43
H00R 2 0.784837 1.096293 0.552578 11.00000 -1.20000
AFIX 0
C00S 1 0.731127 1.000873 0.361012 11.00000 0.02439 0.02000 =
0.02076 0.00096 0.01482 -0.00227
AFIX 23
H00C 2 0.760922 0.973033 0.344313 11.00000 -1.20000
H00D 2 0.752434 1.068436 0.385844 11.00000 -1.20000
AFIX 0
C00T 1 0.476703 0.631597 0.411426 11.00000 0.01338 0.01950 =
0.03609 -0.00129 0.00701 -0.00496
AFIX 43
H00T 2 0.440410 0.590637 0.385168 11.00000 -1.20000
AFIX 0
C00U 1 0.654649 0.568618 0.319866 11.00000 0.01941 0.02039 =
0.02160 -0.00720 0.00123 0.00404
AFIX 43
H00U 2 0.642820 0.490876 0.304544 11.00000 -1.20000
AFIX 0
C00V 1 0.534235 0.703146 0.504937 11.00000 0.01824 0.02116 =
0.02964 0.00409 0.01345 -0.00326
AFIX 43
H00V 2 0.536520 0.711119 0.541163 11.00000 -1.20000
AFIX 0
C00W 1 0.709244 0.757689 0.322432 11.00000 0.01794 0.02452 =
0.01696 -0.00248 0.00746 0.00368
AFIX 43
H00W 2 0.732863 0.808749 0.308457 11.00000 -1.20000
AFIX 0
C00X 1 0.586015 0.928558 0.589815 11.00000 0.02104 0.02500 =
0.02400 0.00162 0.01426 0.00071
AFIX 23
H00F 2 0.543690 0.918410 0.558189 11.00000 -1.20000
H00G 2 0.579248 0.908347 0.623324 11.00000 -1.20000
AFIX 0
C00Y 1 0.689106 0.646061 0.299998 11.00000 0.02021 0.02661 =
0.01707 -0.00571 0.00396 0.00709
AFIX 43
H00Y 2 0.698929 0.620924 0.270112 11.00000 -1.20000
AFIX 0
C00Z 1 0.667498 1.044595 0.315774 11.00000 0.03270 0.02157 =
0.01820 0.00261 0.01218 0.00179
AFIX 23
H00H 2 0.677806 1.096898 0.290323 11.00000 -1.20000
H00I 2 0.642842 0.974703 0.294664 11.00000 -1.20000
AFIX 0
C010 1 0.484443 0.639306 0.466099 11.00000 0.01669 0.02150 =
0.03946 0.00462 0.01338 -0.00411
AFIX 43
H010 2 0.454166 0.598923 0.476849 11.00000 -1.20000
AFIX 0
C011 1 0.605735 1.060425 0.593038 11.00000 0.02488 0.02331 =
0.02492 0.00458 0.01379 0.00414
AFIX 23
H01A 2 0.604913 1.085535 0.557130 11.00000 -1.20000
H01B 2 0.573402 1.109546 0.600441 11.00000 -1.20000
AFIX 0
C012 1 0.624879 1.113759 0.338297 11.00000 0.02806 0.01898 =
0.02542 0.00332 0.01157 0.00222
AFIX 23
H01C 2 0.652011 1.174181 0.364897 11.00000 -1.20000
H01D 2 0.590716 1.157089 0.307797 11.00000 -1.20000
AFIX 0
C013 1 0.456460 0.655588 0.301342 11.00000 0.01558 0.03736 =
0.02924 -0.01095 0.00030 -0.00511
AFIX 137
H01E 2 0.456180 0.676089 0.265485 11.00000 -1.50000
H01F 2 0.419549 0.694492 0.305536 11.00000 -1.50000
H01G 2 0.452867 0.568505 0.303995 11.00000 -1.50000
AFIX 0
C014 1 0.580869 0.424633 0.360014 11.00000 0.03132 0.01773 =
0.04308 -0.00945 0.00821 -0.00780
AFIX 137
H01H 2 0.551223 0.441934 0.322074 11.00000 -1.50000
H01I 2 0.556481 0.387286 0.379234 11.00000 -1.50000
H01J 2 0.615140 0.369894 0.360213 11.00000 -1.50000
AFIX 0
C015 1 0.674229 1.060824 0.690728 11.00000 0.04104 0.02866 =
0.02232 -0.00146 0.01736 0.00153
AFIX 137
H01K 2 0.642236 1.110864 0.697389 11.00000 -1.50000
H01L 2 0.718060 1.080080 0.717710 11.00000 -1.50000
H01M 2 0.664845 0.976138 0.694077 11.00000 -1.50000
AFIX 0
C016 1 0.691586 1.205930 0.631792 11.00000 0.03919 0.02303 =
0.03831 -0.00046 0.02073 -0.00405
AFIX 137
H01N 2 0.689478 1.219944 0.594807 11.00000 -1.50000
H01O 2 0.736462 1.217104 0.658628 11.00000 -1.50000
H01P 2 0.662925 1.262778 0.639360 11.00000 -1.50000
AFIX 0
C017 1 0.578723 1.102968 0.406111 11.00000 0.03337 0.04243 =
0.04082 0.00887 0.02368 0.01228
AFIX 137
H01Q 2 0.618520 1.140576 0.432416 11.00000 -1.50000
H01R 2 0.561342 1.047719 0.425484 11.00000 -1.50000
H01S 2 0.546282 1.164990 0.387820 11.00000 -1.50000
AFIX 0
C018 1 0.534447 0.983391 0.325613 11.00000 0.02728 0.02861 =
0.05604 0.00472 0.00824 -0.00135
AFIX 137
H01T 2 0.503803 1.046824 0.305771 11.00000 -1.50000
H01U 2 0.514637 0.932397 0.344667 11.00000 -1.50000
H01V 2 0.544935 0.934852 0.299597 11.00000 -1.50000
AFIX 0
B019 3 0.621275 0.659145 0.698349 11.00000 0.02940 0.02260 =
0.02398 0.00569 0.01572 0.00070
HKLF 4
REM 20191121_gianetti_01_0ma_a.res in C2/c
REM wR2 = 0.1114, GooF = S = 0.965, Restrained GooF = 0.965 for all data
REM R1 = 0.0405 for 8589 Fo > 4sig(Fo) and 0.0427 for all 9160 data
REM 412 parameters refined using 0 restraints
END
WGHT 0.0525 4.7538
REM Highest difference peak 0.337, deepest hole -0.271, 1-sigma level 0.047
Q1 1 0.6571 0.8193 0.4428 11.00000 0.05 0.34
Q2 1 0.6803 0.7526 0.3791 11.00000 0.05 0.34
Q3 1 0.7021 0.6997 0.3190 11.00000 0.05 0.32
Q4 1 0.6411 0.7422 0.4004 11.00000 0.05 0.32
Q5 1 0.7424 0.9676 0.4600 11.00000 0.05 0.32
Q6 1 0.7029 0.8773 0.4577 11.00000 0.05 0.32
Q7 1 0.7392 1.0030 0.5403 11.00000 0.05 0.31
Q8 1 0.5601 0.7039 0.4188 11.00000 0.05 0.31
Q9 1 0.6382 0.6728 0.7601 11.00000 0.05 0.30
Q10 1 0.7032 0.8539 0.3802 11.00000 0.05 0.29
Q11 1 0.6993 1.0220 0.3391 11.00000 0.05 0.29
Q12 1 0.5612 0.7266 0.4991 11.00000 0.05 0.27
Q13 1 0.6546 0.8561 0.5197 11.00000 0.05 0.27
Q14 1 0.6176 0.7446 0.4397 11.00000 0.05 0.27
Q15 1 0.6515 0.6593 0.3818 11.00000 0.05 0.27
Q16 1 0.7582 1.0186 0.5010 11.00000 0.05 0.26
Q17 1 0.6453 0.5796 0.3376 11.00000 0.05 0.26
Q18 1 0.5794 0.7406 0.4600 11.00000 0.05 0.26
Q19 1 0.6986 0.7777 0.3408 11.00000 0.05 0.25
Q20 1 0.6813 0.6012 0.3182 11.00000 0.05 0.25
;
_shelx_res_checksum 95414
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# 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_2-Hcation
_database_code_depnum_ccdc_archive 'CCDC 2004976'
loop_
_audit_author_name
_audit_author_address
'thomas l gianetti'
;University of Arizona
United States of America
;
_audit_update_record
;
2020-05-20 deposited with the CCDC. 2020-09-14 downloaded from the CCDC.
;
_audit_creation_date 2019-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_systematic 2-Hcation
_chemical_formula_moiety 'C1 H2 Cl2, B F4, C31 H39 N4 O2'
_chemical_formula_sum 'C32 H41 B Cl2 F4 N4 O2'
_chemical_formula_weight 671.43
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
B 0.00141 0.00067 2.05450 1.33260 1.09790 0.70680 23.21850 1.02100 60.34980
0.14030 -0.193200007081
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
F 0.01794 0.01033 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150
26.14760 0.277599990368
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z
_symmetry_Int_Tables_number 2
_cell_length_a 11.5110(3)
_cell_length_b 12.4254(3)
_cell_length_c 13.1831(3)
_cell_angle_alpha 85.1060(18)
_cell_angle_beta 78.778(2)
_cell_angle_gamma 64.945(3)
_cell_volume 1675.45(8)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 12735
_cell_measurement_temperature 100.01(10)
_cell_measurement_theta_max 30.3260
_cell_measurement_theta_min 3.1460
_exptl_absorpt_coefficient_mu 0.251
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.94936
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb 1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour 'metallic dark violet'
_exptl_crystal_colour_lustre metallic
_exptl_crystal_colour_modifier dark
_exptl_crystal_colour_primary violet
_exptl_crystal_density_diffrn 1.3308
_exptl_crystal_description block
_exptl_crystal_F_000 704.9552
_exptl_crystal_recrystallization_method DCM/Hexane
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.2
_diffrn_reflns_av_R_equivalents 0.0227
_diffrn_reflns_av_unetI/netI 0.0230
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 35035
_diffrn_reflns_theta_full 26.3714
_diffrn_reflns_theta_max 26.37
_diffrn_reflns_theta_min 3.15
_diffrn_ambient_temperature 100
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9985
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -46.00 35.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -21.7904 38.0000 -60.0000 81
#__ type_ start__ end____ width___ exp.time_
2 omega -24.00 2.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -21.7904 -99.0000 -60.0000 26
#__ type_ start__ end____ width___ exp.time_
3 omega 14.00 40.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -21.7904 38.0000 -90.0000 26
#__ type_ start__ end____ width___ exp.time_
4 omega -19.00 20.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -21.7904 -99.0000 150.0000 39
#__ type_ start__ end____ width___ exp.time_
5 omega -21.00 13.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -21.7904 -99.0000 -90.0000 34
#__ type_ start__ end____ width___ exp.time_
6 omega -49.00 -9.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 22.4154 -38.0000 -150.0000 40
#__ type_ start__ end____ width___ exp.time_
7 omega -3.00 90.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 22.4154 71.0000 133.0000 93
#__ type_ start__ end____ width___ exp.time_
8 omega -44.00 49.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 22.4154 -71.0000 2.0000 93
#__ type_ start__ end____ width___ exp.time_
9 omega -98.00 -34.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -21.7904 -179.0000 30.0000 64
#__ type_ start__ end____ width___ exp.time_
10 omega 1.00 91.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 22.4154 57.0000 30.0000 90
#__ type_ start__ end____ width___ exp.time_
11 omega -3.00 95.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 22.4154 38.0000 -150.0000 98
#__ type_ start__ end____ width___ exp.time_
12 omega -25.00 64.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 22.4154 -99.0000 -120.0000 89
#__ type_ start__ end____ width___ exp.time_
13 omega -25.00 38.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 22.4154 -99.0000 90.0000 63
#__ type_ start__ end____ width___ exp.time_
14 omega 1.00 91.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 22.4154 57.0000 -60.0000 90
;
_diffrn_measurement_device_type 'Xcalibur, Sapphire3'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_reflns_Friedel_coverage 0.0
_reflns_limit_h_max 14
_reflns_limit_h_min -13
_reflns_limit_k_max 15
_reflns_limit_k_min -15
_reflns_limit_l_max 16
_reflns_limit_l_min 0
_reflns_number_gt 6350
_reflns_number_total 6857
_reflns_threshold_expression I>=2u(I)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb 1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb 1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb 1 2013,16:14:44)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.3598
_refine_diff_density_min -0.2530
_refine_diff_density_rms 0.0538
_refine_ls_d_res_high 0.8000
_refine_ls_d_res_low 6.4655
_refine_ls_goodness_of_fit_ref 1.0699
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_constraints 67
_refine_ls_number_parameters 440
_refine_ls_number_reflns 6857
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0507
_refine_ls_R_factor_gt 0.0459
_refine_ls_restrained_S_all 1.0699
_refine_ls_shift/su_max 0.0009
_refine_ls_shift/su_mean 0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+1.2295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1033
_refine_ls_wR_factor_ref 0.1060
_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. Others
Sof(Cl2A)=Sof(C19A)=Sof(H19c)=Sof(H19d)=Sof(Cl1A)=1-FVAR(1)
Sof(Cl2)=Sof(Cl1)=Sof(C19)=Sof(H19a)=Sof(H19b)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
C00U(H00a,H00b), C00V(H00c,H00d), C00W(H00e,H00f), C00Z(H00g,H00i), C012(H01g,
H01h), C013(H01i,H01j), C19(H19a,H19b), C19A(H19c,H19d)
3.b Aromatic/amide H refined with riding coordinates:
C00H(H00H), C00N(H00N), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S),
C00T(H00T), C00X(H00X), C00Y(H00Y)
3.c Idealised Me refined as rotating group:
C010(H01a,H01b,H01c), C011(H01d,H01e,H01f), C014(H01k,H01l,H01m), C015(H01n,
H01o,H01p), C016(H01q,H01r,H01s), C018(H01t,H01u,H01v)
;
_atom_sites_solution_primary dual
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_refinement_flags_posn
_atom_site_disorder_group
Cl2 Cl 0.6481(7) 0.0801(7) 0.0532(6) 0.0643(14) Uani 0.458(15) . 1
Cl1 Cl 0.8937(5) -0.1394(2) 0.0022(2) 0.0542(11) Uani 0.458(15) . 1
F003 F 0.98678(10) -0.09681(9) 0.35618(8) 0.0341(2) Uani 1.000000 . .
O004 O 0.48235(10) 0.24523(9) 0.71789(8) 0.0202(2) Uani 1.000000 . .
O005 O 0.36688(11) 0.14794(9) 0.61248(9) 0.0220(2) Uani 1.000000 . .
F006 F 0.90882(11) 0.01158(10) 0.21780(9) 0.0400(3) Uani 1.000000 . .
F007 F 1.12459(11) -0.11507(11) 0.20372(9) 0.0473(3) Uani 1.000000 . .
F008 F 1.04188(11) 0.05447(10) 0.29791(11) 0.0469(3) Uani 1.000000 . .
N009 N 0.56842(13) 0.33716(12) 0.36173(10) 0.0200(3) Uani 1.000000 . .
N00A N 0.15058(12) 0.56344(11) 0.56883(10) 0.0194(3) Uani 1.000000 . .
N00B N -0.22375(13) 0.74113(12) 0.72701(11) 0.0231(3) Uani 1.000000 . .
N10 N 0.68199(15) 0.43610(14) 0.05950(11) 0.0322(3) Uani 1.000000 . .
C00D C 0.60778(15) 0.26320(13) 0.44471(12) 0.0184(3) Uani 1.000000 . .
C00E C 0.38486(15) 0.36015(13) 0.54016(11) 0.0169(3) Uani 1.000000 . .
C00F C 0.45541(15) 0.44050(14) 0.37489(12) 0.0189(3) Uani 1.000000 . .
C00G C 0.23817(15) 0.55352(13) 0.47828(12) 0.0189(3) Uani 1.000000 . .
C00H C 0.73476(15) 0.17254(14) 0.43602(12) 0.0200(3) Uani 1.000000 . .
H00H H 0.79353(15) 0.15892(14) 0.37207(12) 0.0240(4) Uiso 1.000000 R .
C00I C 0.56548(15) 0.21048(13) 0.62646(12) 0.0178(3) Uani 1.000000 . .
C00J C 0.27339(14) 0.35683(14) 0.60911(12) 0.0182(3) Uani 1.000000 . .
C00K C 0.15964(15) 0.46405(14) 0.62899(12) 0.0201(3) Uani 1.000000 . .
C00L C 0.26792(15) 0.24939(14) 0.65307(12) 0.0201(3) Uani 1.000000 . .
C00M C 0.36055(14) 0.45202(13) 0.46624(11) 0.0173(3) Uani 1.000000 . .
C00N C 0.77268(15) 0.10405(14) 0.52100(13) 0.0216(3) Uani 1.000000 . .
H00N H 0.85750(15) 0.04130(14) 0.51428(13) 0.0259(4) Uiso 1.000000 R .
C00O C 0.51748(14) 0.27744(13) 0.53844(11) 0.0171(3) Uani 1.000000 . .
C00P C 0.42607(16) 0.52793(14) 0.29817(12) 0.0211(3) Uani 1.000000 . .
H00P H 0.48757(16) 0.52103(14) 0.23669(12) 0.0253(4) Uiso 1.000000 R .
C00Q C 0.30622(16) 0.62481(14) 0.31282(12) 0.0219(3) Uani 1.000000 . .
H00Q H 0.28744(16) 0.68377(14) 0.26018(12) 0.0263(4) Uiso 1.000000 R .
C00R C 0.21258(16) 0.63979(14) 0.40048(12) 0.0216(3) Uani 1.000000 . .
H00R H 0.13185(16) 0.70794(14) 0.40766(12) 0.0259(4) Uiso 1.000000 R .
C00S C 0.69025(15) 0.12380(14) 0.61723(12) 0.0207(3) Uani 1.000000 . .
H00S H 0.72041(15) 0.07762(14) 0.67563(12) 0.0249(4) Uiso 1.000000 R .
C00T C 0.05583(16) 0.46786(15) 0.70810(13) 0.0257(4) Uani 1.000000 . .
H00T H -0.01611(16) 0.54110(15) 0.72838(13) 0.0309(4) Uiso 1.000000 R .
C00U C 0.03681(15) 0.67740(14) 0.59468(13) 0.0214(3) Uani 1.000000 . .
H00a H 0.01533(15) 0.68668(14) 0.67078(13) 0.0257(4) Uiso 1.000000 R .
H00b H 0.06048(15) 0.74291(14) 0.56525(13) 0.0257(4) Uiso 1.000000 R .
C00V C -0.08461(15) 0.68906(14) 0.55488(13) 0.0230(3) Uani 1.000000 . .
H00c H -0.07911(15) 0.71374(14) 0.48132(13) 0.0276(4) Uiso 1.000000 R .
H00d H -0.09075(15) 0.61161(14) 0.56034(13) 0.0276(4) Uiso 1.000000 R .
C00W C -0.20436(16) 0.78171(15) 0.61991(13) 0.0254(4) Uani 1.000000 . .
H00e H -0.28227(16) 0.79772(15) 0.58947(13) 0.0305(4) Uiso 1.000000 R .
H00f H -0.19374(16) 0.85681(15) 0.61901(13) 0.0305(4) Uiso 1.000000 R .
C00X C 0.16290(17) 0.25320(16) 0.72586(13) 0.0268(4) Uani 1.000000 . .
H00X H 0.15967(17) 0.18199(16) 0.75579(13) 0.0322(4) Uiso 1.000000 R .
C00Y C 0.06129(17) 0.36316(17) 0.75507(14) 0.0300(4) Uani 1.000000 . .
H00Y H -0.00712(17) 0.36582(17) 0.80979(14) 0.0360(5) Uiso 1.000000 R .
C00Z C 0.64475(16) 0.30356(15) 0.25638(12) 0.0235(3) Uani 1.000000 . .
H00g H 0.68678(16) 0.21580(15) 0.25154(12) 0.0282(4) Uiso 1.000000 R .
H00i H 0.58417(16) 0.33343(15) 0.20620(12) 0.0282(4) Uiso 1.000000 R .
C010 C 0.51864(18) 0.17237(16) 0.80654(13) 0.0303(4) Uani 1.000000 . .
H01a H 0.5390(13) 0.0899(3) 0.7911(4) 0.0454(6) Uiso 1.000000 GR .
H01b H 0.5954(8) 0.1768(9) 0.8240(6) 0.0454(6) Uiso 1.000000 GR .
H01c H 0.4464(5) 0.2006(7) 0.8651(3) 0.0454(6) Uiso 1.000000 GR .
C011 C 0.35808(18) 0.03829(15) 0.64407(15) 0.0318(4) Uani 1.000000 . .
H01d H 0.4313(7) -0.0272(2) 0.6050(8) 0.0478(6) Uiso 1.000000 GR .
H01e H 0.3609(13) 0.0258(6) 0.7181(3) 0.0478(6) Uiso 1.000000 GR .
H01f H 0.2760(6) 0.0411(5) 0.6308(10) 0.0478(6) Uiso 1.000000 GR .
C012 C 0.74968(17) 0.35050(17) 0.22525(13) 0.0289(4) Uani 1.000000 . .
H01g H 0.71632(17) 0.43277(17) 0.25062(13) 0.0347(5) Uiso 1.000000 R .
H01h H 0.82702(17) 0.30046(17) 0.25657(13) 0.0347(5) Uiso 1.000000 R .
C013 C 0.78750(17) 0.34825(17) 0.10754(14) 0.0315(4) Uani 1.000000 . .
H01i H 0.80928(17) 0.26814(17) 0.08199(14) 0.0378(5) Uiso 1.000000 R .
H01j H 0.86590(17) 0.36471(17) 0.08757(14) 0.0378(5) Uiso 1.000000 R .
C014 C -0.29238(17) 0.66462(16) 0.73836(15) 0.0304(4) Uani 1.000000 . .
H01k H -0.3802(5) 0.7100(3) 0.7227(10) 0.0456(6) Uiso 1.000000 GR .
H01l H -0.2448(7) 0.5976(6) 0.6905(7) 0.0456(6) Uiso 1.000000 GR .
H01m H -0.2984(11) 0.6346(9) 0.8095(3) 0.0456(6) Uiso 1.000000 GR .
C015 C -0.29489(19) 0.84093(17) 0.79782(16) 0.0367(4) Uani 1.000000 . .
H01n H -0.2474(7) 0.8912(7) 0.7917(8) 0.0550(7) Uiso 1.000000 GR .
H01o H -0.3816(5) 0.8876(7) 0.7806(7) 0.0550(7) Uiso 1.000000 GR .
H01p H -0.3035(12) 0.81115(17) 0.86889(19) 0.0550(7) Uiso 1.000000 GR .
C016 C 0.6887(2) 0.4026(2) -0.04565(15) 0.0453(5) Uani 1.000000 . .
H01q H 0.7704(7) 0.3981(14) -0.0885(3) 0.0679(8) Uiso 1.000000 GR .
H01r H 0.6853(16) 0.3250(7) -0.0445(2) 0.0679(8) Uiso 1.000000 GR .
H01s H 0.6149(9) 0.4623(8) -0.0745(5) 0.0679(8) Uiso 1.000000 GR .
B017 B 1.01591(19) -0.03685(17) 0.26841(16) 0.0277(4) Uani 1.000000 . .
C018 C 0.6800(2) 0.5533(2) 0.05883(17) 0.0480(5) Uani 1.000000 . .
H01t H 0.6722(17) 0.5767(7) 0.1298(2) 0.0720(8) Uiso 1.000000 GR .
H01u H 0.7608(7) 0.5523(4) 0.0172(11) 0.0720(8) Uiso 1.000000 GR .
H01v H 0.6055(10) 0.6102(3) 0.0290(12) 0.0720(8) Uiso 1.000000 GR .
C19 C 0.8074(17) 0.0176(11) 0.0145(10) 0.042(2) Uani 0.458(15) . 1
H19a H 0.8260(17) 0.0525(11) -0.0537(10) 0.050(3) Uiso 0.458(15) R 1
H19b H 0.8465(17) 0.0432(11) 0.0630(10) 0.050(3) Uiso 0.458(15) R 1
Cl2A Cl 0.6419(4) 0.0565(7) 0.0467(5) 0.0644(13) Uani 0.542(15) . 2
C19A C 0.8195(15) -0.0190(15) 0.0134(11) 0.088(5) Uani 0.542(15) . 2
H19c H 0.8510(15) 0.0059(15) -0.0559(11) 0.106(6) Uiso 0.542(15) R 2
H19d H 0.8612(15) -0.0014(15) 0.0649(11) 0.106(6) Uiso 0.542(15) R 2
Cl1A Cl 0.8530(7) -0.1702(9) 0.0147(3) 0.105(2) Uani 0.542(15) . 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cl2 0.060(2) 0.096(3) 0.0407(12) -0.0360(17) -0.0138(10) 0.0066(13)
Cl1 0.0519(16) 0.0535(15) 0.0420(9) -0.0071(8) -0.0062(9) -0.0074(7)
F003 0.0304(6) 0.0306(6) 0.0385(6) -0.0106(5) -0.0066(5) 0.0047(4)
O004 0.0216(6) 0.0212(5) 0.0180(5) -0.0089(5) -0.0060(4) 0.0040(4)
O005 0.0233(6) 0.0182(5) 0.0278(6) -0.0123(5) -0.0046(5) 0.0029(4)
F006 0.0310(6) 0.0447(7) 0.0409(6) -0.0086(5) -0.0169(5) 0.0036(5)
F007 0.0349(6) 0.0444(7) 0.0394(7) 0.0022(5) 0.0008(5) 0.0009(5)
F008 0.0327(6) 0.0319(6) 0.0830(9) -0.0175(5) -0.0178(6) 0.0038(6)
N009 0.0181(6) 0.0233(7) 0.0193(6) -0.0096(5) -0.0035(5) 0.0020(5)
N00A 0.0166(6) 0.0189(6) 0.0233(7) -0.0069(5) -0.0061(5) 0.0003(5)
N00B 0.0198(7) 0.0209(7) 0.0302(7) -0.0096(6) -0.0039(6) -0.0031(6)
N10 0.0345(8) 0.0390(9) 0.0214(7) -0.0151(7) -0.0022(6) 0.0015(6)
C00D 0.0198(7) 0.0186(7) 0.0216(8) -0.0114(6) -0.0070(6) 0.0011(6)
C00E 0.0199(7) 0.0166(7) 0.0184(7) -0.0104(6) -0.0060(6) -0.0011(6)
C00F 0.0199(7) 0.0207(8) 0.0212(7) -0.0122(6) -0.0069(6) 0.0009(6)
C00G 0.0197(7) 0.0187(7) 0.0232(8) -0.0112(6) -0.0078(6) -0.0000(6)
C00H 0.0180(7) 0.0212(8) 0.0235(8) -0.0105(6) -0.0036(6) -0.0013(6)
C00I 0.0200(7) 0.0172(7) 0.0209(7) -0.0120(6) -0.0049(6) 0.0006(6)
C00J 0.0176(7) 0.0218(8) 0.0192(7) -0.0106(6) -0.0066(6) 0.0011(6)
C00K 0.0193(8) 0.0226(8) 0.0221(8) -0.0110(6) -0.0075(6) 0.0011(6)
C00L 0.0190(7) 0.0223(8) 0.0226(8) -0.0106(6) -0.0080(6) 0.0030(6)
C00M 0.0184(7) 0.0188(7) 0.0195(7) -0.0109(6) -0.0071(6) 0.0007(6)
C00N 0.0170(7) 0.0171(7) 0.0318(9) -0.0069(6) -0.0073(6) 0.0001(6)
C00O 0.0185(7) 0.0166(7) 0.0206(7) -0.0107(6) -0.0054(6) 0.0003(6)
C00P 0.0253(8) 0.0238(8) 0.0196(7) -0.0151(7) -0.0059(6) 0.0019(6)
C00Q 0.0305(9) 0.0193(8) 0.0236(8) -0.0155(7) -0.0127(7) 0.0057(6)
C00R 0.0231(8) 0.0170(7) 0.0274(8) -0.0088(6) -0.0104(6) 0.0018(6)
C00S 0.0221(8) 0.0180(7) 0.0258(8) -0.0105(6) -0.0091(6) 0.0037(6)
C00T 0.0179(8) 0.0294(9) 0.0272(8) -0.0075(7) -0.0040(6) 0.0011(7)
C00U 0.0173(7) 0.0201(8) 0.0276(8) -0.0067(6) -0.0074(6) -0.0025(6)
C00V 0.0202(8) 0.0238(8) 0.0270(8) -0.0089(7) -0.0095(6) 0.0007(6)
C00W 0.0195(8) 0.0228(8) 0.0344(9) -0.0076(7) -0.0097(7) 0.0023(7)
C00X 0.0264(9) 0.0295(9) 0.0292(9) -0.0170(7) -0.0065(7) 0.0086(7)
C00Y 0.0217(8) 0.0393(10) 0.0286(9) -0.0150(8) -0.0000(7) 0.0047(7)
C00Z 0.0223(8) 0.0279(8) 0.0219(8) -0.0115(7) -0.0053(6) -0.0002(6)
C010 0.0336(10) 0.0290(9) 0.0225(8) -0.0086(8) -0.0062(7) 0.0084(7)
C011 0.0339(10) 0.0205(8) 0.0446(11) -0.0162(8) -0.0061(8) 0.0060(7)
C012 0.0256(9) 0.0385(10) 0.0276(9) -0.0178(8) -0.0068(7) 0.0032(7)
C013 0.0239(9) 0.0389(10) 0.0293(9) -0.0135(8) 0.0023(7) -0.0008(8)
C014 0.0263(9) 0.0287(9) 0.0409(10) -0.0157(8) -0.0053(7) -0.0020(7)
C015 0.0358(10) 0.0327(10) 0.0433(11) -0.0173(9) 0.0017(8) -0.0121(8)
C016 0.0508(13) 0.0644(15) 0.0255(10) -0.0301(12) -0.0040(9) 0.0011(9)
B017 0.0197(9) 0.0253(10) 0.0351(11) -0.0060(8) -0.0068(8) 0.0019(8)
C018 0.0621(15) 0.0447(12) 0.0389(12) -0.0254(11) -0.0081(10) 0.0064(9)
C19 0.046(6) 0.050(4) 0.020(3) -0.010(4) -0.013(3) 0.008(2)
Cl2A 0.0317(11) 0.095(3) 0.0411(16) -0.0073(14) -0.0036(9) 0.0211(15)
C19A 0.032(4) 0.145(13) 0.046(4) -0.004(8) -0.003(3) 0.032(7)
Cl1A 0.080(2) 0.150(3) 0.0479(10) -0.007(3) -0.0228(11) 0.0024(16)
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
Cl2 C19 1.650(19) . ?
Cl1 C19 1.780(13) . ?
F003 B017 1.386(2) . ?
O004 C00I 1.3582(18) . ?
O004 C010 1.4315(19) . ?
O005 C00L 1.3544(19) . ?
O005 C011 1.4296(19) . ?
F006 B017 1.397(2) . ?
F007 B017 1.390(2) . ?
F008 B017 1.391(2) . ?
N009 C00D 1.384(2) . ?
N009 C00F 1.381(2) . ?
N009 C00Z 1.479(2) . ?
N00A C00G 1.381(2) . ?
N00A C00K 1.386(2) . ?
N00A C00U 1.475(2) . ?
N00B C00W 1.466(2) . ?
N00B C014 1.455(2) . ?
N00B C015 1.456(2) . ?
N10 C013 1.458(2) . ?
N10 C016 1.460(2) . ?
N10 C018 1.445(3) . ?
C00D C00H 1.407(2) . ?
C00D C00O 1.421(2) . ?
C00E C00J 1.435(2) . ?
C00E C00M 1.406(2) . ?
C00E C00O 1.431(2) . ?
C00F C00M 1.431(2) . ?
C00F C00P 1.397(2) . ?
C00G C00M 1.429(2) . ?
C00G C00R 1.397(2) . ?
C00H H00H 0.9500 . ?
C00H C00N 1.372(2) . ?
C00I C00O 1.428(2) . ?
C00I C00S 1.372(2) . ?
C00J C00K 1.416(2) . ?
C00J C00L 1.431(2) . ?
C00K C00T 1.412(2) . ?
C00L C00X 1.376(2) . ?
C00N H00N 0.9500 . ?
C00N C00S 1.399(2) . ?
C00P H00P 0.9500 . ?
C00P C00Q 1.385(2) . ?
C00Q H00Q 0.9500 . ?
C00Q C00R 1.383(2) . ?
C00R H00R 0.9500 . ?
C00S H00S 0.9500 . ?
C00T H00T 0.9500 . ?
C00T C00Y 1.374(2) . ?
C00U H00a 0.9900 . ?
C00U H00b 0.9900 . ?
C00U C00V 1.533(2) . ?
C00V H00c 0.9900 . ?
C00V H00d 0.9900 . ?
C00V C00W 1.525(2) . ?
C00W H00e 0.9900 . ?
C00W H00f 0.9900 . ?
C00X H00X 0.9500 . ?
C00X C00Y 1.394(3) . ?
C00Y H00Y 0.9500 . ?
C00Z H00g 0.9900 . ?
C00Z H00i 0.9900 . ?
C00Z C012 1.527(2) . ?
C010 H01a 0.9800 . ?
C010 H01b 0.9800 . ?
C010 H01c 0.9800 . ?
C011 H01d 0.9800 . ?
C011 H01e 0.9800 . ?
C011 H01f 0.9800 . ?
C012 H01g 0.9900 . ?
C012 H01h 0.9900 . ?
C012 C013 1.527(2) . ?
C013 H01i 0.9900 . ?
C013 H01j 0.9900 . ?
C014 H01k 0.9800 . ?
C014 H01l 0.9800 . ?
C014 H01m 0.9800 . ?
C015 H01n 0.9800 . ?
C015 H01o 0.9800 . ?
C015 H01p 0.9800 . ?
C016 H01q 0.9800 . ?
C016 H01r 0.9800 . ?
C016 H01s 0.9800 . ?
C018 H01t 0.9800 . ?
C018 H01u 0.9800 . ?
C018 H01v 0.9800 . ?
C19 H19a 0.9900 . ?
C19 H19b 0.9900 . ?
Cl2A C19A 1.830(17) . ?
C19A H19c 0.9900 . ?
C19A H19d 0.9900 . ?
C19A Cl1A 1.750(13) . ?
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
C010 O004 C00I 117.29(12) . . ?
C011 O005 C00L 117.57(13) . . ?
C00F N009 C00D 120.94(13) . . ?
C00Z N009 C00D 120.05(13) . . ?
C00Z N009 C00F 118.97(13) . . ?
C00K N00A C00G 120.55(13) . . ?
C00U N00A C00G 119.58(13) . . ?
C00U N00A C00K 119.38(13) . . ?
C014 N00B C00W 111.48(13) . . ?
C015 N00B C00W 111.35(14) . . ?
C015 N00B C014 109.44(14) . . ?
C016 N10 C013 111.82(16) . . ?
C018 N10 C013 111.99(16) . . ?
C018 N10 C016 109.65(16) . . ?
C00H C00D N009 120.62(14) . . ?
C00O C00D N009 119.34(14) . . ?
C00O C00D C00H 120.02(14) . . ?
C00M C00E C00J 116.60(13) . . ?
C00O C00E C00J 126.07(14) . . ?
C00O C00E C00M 117.32(13) . . ?
C00M C00F N009 118.17(13) . . ?
C00P C00F N009 122.15(14) . . ?
C00P C00F C00M 119.40(14) . . ?
C00M C00G N00A 117.94(13) . . ?
C00R C00G N00A 122.52(14) . . ?
C00R C00G C00M 119.52(14) . . ?
H00H C00H C00D 120.39(9) . . ?
C00N C00H C00D 119.22(14) . . ?
C00N C00H H00H 120.39(9) . . ?
C00O C00I O004 115.00(13) . . ?
C00S C00I O004 124.03(14) . . ?
C00S C00I C00O 120.81(14) . . ?
C00K C00J C00E 118.43(14) . . ?
C00L C00J C00E 123.32(14) . . ?
C00L C00J C00K 118.09(14) . . ?
C00J C00K N00A 119.42(14) . . ?
C00T C00K N00A 120.77(14) . . ?
C00T C00K C00J 119.79(14) . . ?
C00J C00L O005 115.17(13) . . ?
C00X C00L O005 124.26(14) . . ?
C00X C00L C00J 120.40(15) . . ?
C00F C00M C00E 119.88(14) . . ?
C00G C00M C00E 120.44(14) . . ?
C00G C00M C00F 119.55(14) . . ?
H00N C00N C00H 118.99(9) . . ?
C00S C00N C00H 122.02(15) . . ?
C00S C00N H00N 118.99(9) . . ?
C00E C00O C00D 118.38(13) . . ?
C00I C00O C00D 117.84(14) . . ?
C00I C00O C00E 123.76(14) . . ?
H00P C00P C00F 120.40(9) . . ?
C00Q C00P C00F 119.20(15) . . ?
C00Q C00P H00P 120.40(9) . . ?
H00Q C00Q C00P 118.44(9) . . ?
C00R C00Q C00P 123.12(14) . . ?
C00R C00Q H00Q 118.44(9) . . ?
C00Q C00R C00G 119.20(15) . . ?
H00R C00R C00G 120.40(9) . . ?
H00R C00R C00Q 120.40(9) . . ?
C00N C00S C00I 119.38(14) . . ?
H00S C00S C00I 120.31(9) . . ?
H00S C00S C00N 120.31(9) . . ?
H00T C00T C00K 120.77(10) . . ?
C00Y C00T C00K 118.45(16) . . ?
C00Y C00T H00T 120.77(10) . . ?
H00a C00U N00A 108.75(8) . . ?
H00b C00U N00A 108.75(8) . . ?
H00b C00U H00a 107.6 . . ?
C00V C00U N00A 114.01(13) . . ?
C00V C00U H00a 108.75(9) . . ?
C00V C00U H00b 108.75(9) . . ?
H00c C00V C00U 109.98(9) . . ?
H00d C00V C00U 109.98(9) . . ?
H00d C00V H00c 108.4 . . ?
C00W C00V C00U 108.56(13) . . ?
C00W C00V H00c 109.98(9) . . ?
C00W C00V H00d 109.98(9) . . ?
C00V C00W N00B 111.22(13) . . ?
H00e C00W N00B 109.39(8) . . ?
H00e C00W C00V 109.39(9) . . ?
H00f C00W N00B 109.39(8) . . ?
H00f C00W C00V 109.39(9) . . ?
H00f C00W H00e 108.0 . . ?
H00X C00X C00L 120.50(10) . . ?
C00Y C00X C00L 118.99(15) . . ?
C00Y C00X H00X 120.50(10) . . ?
C00X C00Y C00T 122.82(16) . . ?
H00Y C00Y C00T 118.59(10) . . ?
H00Y C00Y C00X 118.59(10) . . ?
H00g C00Z N009 108.61(8) . . ?
H00i C00Z N009 108.61(8) . . ?
H00i C00Z H00g 107.6 . . ?
C012 C00Z N009 114.60(13) . . ?
C012 C00Z H00g 108.61(10) . . ?
C012 C00Z H00i 108.61(9) . . ?
H01a C010 O004 109.5 . . ?
H01b C010 O004 109.5 . . ?
H01b C010 H01a 109.5 . . ?
H01c C010 O004 109.5 . . ?
H01c C010 H01a 109.5 . . ?
H01c C010 H01b 109.5 . . ?
H01d C011 O005 109.5 . . ?
H01e C011 O005 109.5 . . ?
H01e C011 H01d 109.5 . . ?
H01f C011 O005 109.5 . . ?
H01f C011 H01d 109.5 . . ?
H01f C011 H01e 109.5 . . ?
H01g C012 C00Z 109.86(10) . . ?
H01h C012 C00Z 109.86(9) . . ?
H01h C012 H01g 108.3 . . ?
C013 C012 C00Z 109.13(14) . . ?
C013 C012 H01g 109.86(10) . . ?
C013 C012 H01h 109.86(10) . . ?
C012 C013 N10 111.31(14) . . ?
H01i C013 N10 109.37(10) . . ?
H01i C013 C012 109.37(10) . . ?
H01j C013 N10 109.37(9) . . ?
H01j C013 C012 109.37(9) . . ?
H01j C013 H01i 108.0 . . ?
H01k C014 N00B 109.5 . . ?
H01l C014 N00B 109.5 . . ?
H01l C014 H01k 109.5 . . ?
H01m C014 N00B 109.5 . . ?
H01m C014 H01k 109.5 . . ?
H01m C014 H01l 109.5 . . ?
H01n C015 N00B 109.5 . . ?
H01o C015 N00B 109.5 . . ?
H01o C015 H01n 109.5 . . ?
H01p C015 N00B 109.5 . . ?
H01p C015 H01n 109.5 . . ?
H01p C015 H01o 109.5 . . ?
H01q C016 N10 109.5 . . ?
H01r C016 N10 109.5 . . ?
H01r C016 H01q 109.5 . . ?
H01s C016 N10 109.5 . . ?
H01s C016 H01q 109.5 . . ?
H01s C016 H01r 109.5 . . ?
F006 B017 F003 109.18(15) . . ?
F007 B017 F003 109.50(15) . . ?
F007 B017 F006 110.44(16) . . ?
F008 B017 F003 108.82(16) . . ?
F008 B017 F006 109.17(15) . . ?
F008 B017 F007 109.70(15) . . ?
H01t C018 N10 109.5 . . ?
H01u C018 N10 109.5 . . ?
H01u C018 H01t 109.5 . . ?
H01v C018 N10 109.5 . . ?
H01v C018 H01t 109.5 . . ?
H01v C018 H01u 109.5 . . ?
Cl1 C19 Cl2 121.1(10) . . ?
H19a C19 Cl2 107.1(5) . . ?
H19a C19 Cl1 107.1(5) . . ?
H19b C19 Cl2 107.1(5) . . ?
H19b C19 Cl1 107.1(4) . . ?
H19b C19 H19a 106.8 . . ?
H19c C19A Cl2A 110.8(5) . . ?
H19d C19A Cl2A 110.8(5) . . ?
H19d C19A H19c 108.88874069(3) . . ?
Cl1A C19A Cl2A 104.6(8) . . ?
Cl1A C19A H19c 110.8(5) . . ?
Cl1A C19A H19d 110.8(5) . . ?
_iucr_refine_fcf_details
;
data_tlg4xr1
_computing_structure_refinement 'olex2.refine (Bourhis et al., 2015)'
_shelx_refln_list_code 4
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
_cell_length_a 11.5110(3)
_cell_length_b 12.4254(3)
_cell_length_c 13.1831(3)
_cell_angle_alpha 85.1060(18)
_cell_angle_beta 78.778(2)
_cell_angle_gamma 64.945(3)
_cell_volume 1675.45(8)
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_calc
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_F_squared_weight
_refln_observed_status
-13 -10 1 26.058 34.111 3.699 47.005 o
-13 -10 2 9.697 15.475 2.961 101.395 o
-13 -9 1 202.372 210.484 11.903 5.230 o
-13 -9 2 26.082 17.650 3.101 60.495 o
-13 -9 3 44.157 37.924 3.732 34.630 o
-13 -8 1 147.611 159.985 6.356 9.133 o
-13 -8 2 23.808 22.274 3.046 60.969 o
-13 -8 3 182.601 207.638 7.473 6.935 o
-13 -7 1 65.529 64.660 4.428 22.325 o
-13 -7 2 186.359 197.472 7.056 7.093 o
-13 -7 3 36.707 31.577 3.498 41.407 o
-13 -6 1 226.294 217.856 7.202 5.980 o
-13 -6 2 452.807 444.569 12.684 2.386 o
-13 -6 3 13.271 18.455 3.274 79.978 o
-13 -6 4 35.614 38.082 3.828 38.481 o
-13 -5 1 27.994 30.766 4.261 42.971 o
-13 -5 2 21.131 24.692 4.173 51.768 o
-13 -5 3 0.006 0.215 2.695 320.392 o
-13 -4 1 63.557 65.689 4.426 22.621 o
-13 -4 2 15.006 15.820 2.557 91.933 o
-13 -4 3 10.833 19.852 3.040 88.875 o
-13 -3 1 12.021 15.595 2.854 95.693 o
-13 -3 2 51.159 57.392 4.145 27.258 o
-13 -3 3 1.871 2.079 2.360 296.125 o
-13 -2 1 25.082 33.077 5.241 37.637 o
-13 -2 2 4.987 4.862 2.760 171.625 o
-13 -1 1 47.386 52.077 4.412 28.434 o
-12 -12 1 23.333 29.931 3.492 52.998 o
-12 -12 2 22.979 23.817 3.233 59.247 o
-12 -11 1 17.235 23.389 3.150 69.035 o
-12 -11 2 0.297 4.889 2.382 297.341 o
-12 -11 3 0.079 0.733 2.337 404.633 o
-12 -10 1 77.115 82.820 4.742 18.402 o
-12 -10 2 5.361 7.829 2.557 166.058 o
-12 -10 3 1.457 5.280 2.500 244.977 o
-12 -10 4 28.861 25.629 3.501 49.654 o
-12 -9 1 100.528 101.879 5.061 14.411 o
-12 -9 2 217.377 189.226 6.811 6.537 o
-12 -9 3 55.667 53.325 5.297 23.659 o
-12 -9 4 99.163 114.061 5.497 13.632 o
-12 -9 5 44.776 43.368 4.039 32.089 o
-12 -8 1 14.039 13.671 2.625 97.137 o
-12 -8 2 78.056 86.619 4.745 18.014 o
-12 -8 3 0.359 2.484 2.321 351.669 o
-12 -8 4 36.662 42.640 3.777 36.936 o
-12 -8 5 2.469 3.221 3.361 160.873 o
-12 -7 1 243.336 253.089 7.487 5.340 o
-12 -7 2 47.659 54.354 3.921 29.432 o
-12 -7 3 171.897 184.014 6.597 7.813 o
-12 -7 4 5.121 7.568 2.376 181.396 o
-12 -7 5 17.817 28.209 7.042 30.861 o
-12 -7 6 0.594 4.298 2.694 247.748 o
-12 -6 1 93.346 89.887 4.600 16.143 o
-12 -6 2 162.299 160.254 6.087 8.695 o
-12 -6 3 93.600 87.541 4.686 16.155 o
-12 -6 4 196.833 179.703 5.745 7.427 o
-12 -6 5 23.189 27.373 2.784 60.756 o
-12 -6 6 0.718 4.526 2.280 308.208 o
-12 -5 1 76.350 77.630 4.308 19.490 o
-12 -5 2 14.865 20.723 2.804 81.485 o
-12 -5 3 71.641 83.583 3.967 20.241 o
-12 -5 4 40.139 53.541 4.022 31.973 o
-12 -5 5 0.002 0.320 2.262 449.109 o
-12 -5 6 15.325 27.535 3.495 64.449 o
-12 -4 1 178.792 185.871 5.274 7.993 o
-12 -4 2 214.071 211.941 6.106 6.527 o
-12 -4 3 50.076 52.835 3.709 29.470 o
-12 -4 4 10.738 20.608 3.111 86.672 o
-12 -4 5 14.860 23.976 3.261 71.260 o
-12 -4 6 0.446 7.999 2.650 220.671 o
-12 -3 1 47.364 51.027 3.155 32.339 o
-12 -3 2 4.816 9.845 2.062 191.742 o
-12 -3 3 105.678 122.317 5.572 12.773 o
-12 -3 4 59.746 65.116 4.363 23.612 o
-12 -3 5 145.943 162.244 8.078 8.348 o
-12 -2 1 70.668 78.525 4.453 20.110 o
-12 -2 2 31.101 36.941 2.910 46.597 o
-12 -2 3 9.208 6.729 2.350 147.994 o
-12 -2 4 16.040 18.210 2.850 80.955 o
-12 -2 5 0.623 1.179 2.337 364.968 o
-12 -1 1 52.560 50.194 4.025 28.233 o
-12 -1 2 74.423 85.183 4.908 18.380 o
-12 -1 3 4.560 6.700 2.583 178.604 o
-12 -1 4 0.437 4.641 2.259 319.780 o
-12 0 1 11.740 10.678 2.811 106.750 o
-12 0 2 12.673 18.623 4.005 68.607 o
-12 0 3 66.884 72.088 4.683 20.920 o
-12 1 1 77.851 96.129 7.244 14.266 o
-12 1 2 108.048 121.366 6.115 12.225 o
-11 -13 1 111.026 113.978 7.429 11.231 o
-11 -13 2 314.703 274.372 10.999 3.839 o
-11 -12 1 0.788 4.373 2.315 302.121 o
-11 -12 2 26.121 34.576 3.600 47.448 o
-11 -12 3 17.461 16.300 2.571 84.185 o
-11 -12 4 59.348 64.680 3.938 24.625 o
-11 -11 1 96.651 107.331 5.155 14.428 o
-11 -11 2 46.826 48.921 3.295 32.579 o
-11 -11 3 2.229 10.445 2.617 181.411 o
-11 -11 4 1.793 4.796 2.122 296.556 o
-11 -11 5 115.226 137.569 6.905 10.770 o
-11 -10 1 0.343 3.137 2.265 351.832 o
-11 -10 2 4.571 8.940 2.073 200.462 o
-11 -10 3 15.937 21.869 3.005 74.842 o
-11 -10 4 24.185 35.736 3.581 48.739 o
-11 -10 5 57.378 64.565 4.440 24.041 o
-11 -10 6 159.384 162.723 6.736 8.493 o
-11 -9 1 123.856 133.683 5.462 11.332 o
-11 -9 2 102.122 100.621 4.917 14.453 o
-11 -9 3 12.775 17.466 2.803 91.481 o
-11 -9 4 34.046 42.369 3.694 38.795 o
-11 -9 5 16.316 17.903 2.902 79.849 o
-11 -9 6 6.894 13.358 3.370 104.316 o
-11 -8 1 88.352 92.802 4.692 16.439 o
-11 -8 2 14.213 14.091 2.452 99.406 o
-11 -8 3 38.198 34.624 3.232 40.777 o
-11 -8 4 25.267 28.868 3.281 53.258 o
-11 -8 5 29.750 29.437 4.571 40.267 o
-11 -8 6 179.326 173.318 6.545 7.770 o
-11 -8 7 122.021 139.878 7.491 10.004 o
-11 -7 1 0.724 1.483 1.925 479.962 o
-11 -7 2 112.119 121.961 5.104 12.676 o
-11 -7 3 29.228 31.003 3.033 50.077 o
-11 -7 4 81.895 66.274 4.151 19.728 o
-11 -7 5 21.241 20.796 2.812 68.431 o
-11 -7 6 75.724 77.460 3.954 20.089 o
-11 -7 7 105.908 102.666 4.180 14.620 o
-11 -6 1 6.567 8.740 3.490 111.084 o
-11 -6 2 0.287 3.900 2.004 402.835 o
-11 -6 3 129.171 114.241 5.051 11.841 o
-11 -6 4 181.273 176.653 7.570 7.321 o
-11 -6 5 24.339 25.591 2.639 61.645 o
-11 -6 6 29.768 38.386 3.005 46.575 o
-11 -6 7 59.919 65.959 3.378 25.412 o
-11 -5 1 239.182 223.506 5.403 6.031 o
-11 -5 2 2.447 7.110 1.682 303.330 o
-11 -5 3 44.844 34.905 3.979 34.046 o
-11 -5 4 0.158 7.926 2.153 293.827 o
-11 -5 5 28.921 31.576 3.446 47.401 o
-11 -5 6 54.833 51.755 3.313 29.080 o
-11 -5 7 0.896 6.812 1.914 327.266 o
-11 -4 1 370.946 382.162 7.220 3.355 o
-11 -4 2 192.273 192.777 6.648 7.124 o
-11 -4 3 3.802 5.221 1.434 321.190 o
-11 -4 4 2.486 5.616 1.911 294.365 o
-11 -4 5 47.443 54.234 3.979 29.356 o
-11 -4 6 0.055 5.462 3.163 191.721 o
-11 -4 7 1.048 5.624 2.576 240.273 o
-11 -3 1 366.214 370.605 8.616 3.325 o
-11 -3 2 367.309 355.571 6.289 3.546 o
-11 -3 3 6.163 6.402 1.726 220.141 o
-11 -3 4 229.471 222.099 5.856 6.153 o
-11 -3 5 70.172 71.361 4.675 20.432 o
-11 -3 6 7.664 7.540 2.527 148.802 o
-11 -3 7 10.610 15.316 2.375 113.236 o
-11 -2 1 1.902 1.332 1.714 466.873 o
-11 -2 2 1.421 3.985 1.796 390.832 o
-11 -2 3 32.176 37.913 2.767 46.085 o
-11 -2 4 32.353 37.892 2.839 45.594 o
-11 -2 5 79.524 78.199 3.815 19.602 o
-11 -2 6 23.745 26.023 3.157 57.613 o
-11 -2 7 7.886 9.091 2.168 157.296 o
-11 -1 1 66.792 71.276 3.476 23.029 o
-11 -1 2 330.474 327.004 7.167 3.910 o
-11 -1 3 0.679 0.737 1.683 638.582 o
-11 -1 4 7.795 8.672 2.061 165.031 o
-11 -1 5 133.535 143.865 5.019 10.764 o
-11 -1 6 104.943 131.109 4.360 13.374 o
-11 0 1 269.123 258.098 8.303 4.805 o
-11 0 2 3.292 2.980 2.331 251.575 o
-11 0 3 0.552 6.156 1.940 349.274 o
-11 0 4 41.632 45.765 3.184 35.970 o
-11 0 5 243.910 235.791 6.502 5.646 o
-11 0 6 140.845 147.659 5.323 10.160 o
-11 1 1 33.014 43.475 3.853 38.307 o
-11 1 2 7.250 7.555 3.262 119.322 o
-11 1 3 231.437 227.015 9.416 5.322 o
-11 1 4 16.828 18.695 3.134 74.367 o
-11 1 5 3.055 7.326 3.279 144.690 o
-11 2 1 56.792 56.137 6.344 20.650 o
-11 2 2 3.715 10.380 2.926 148.148 o
-11 2 3 19.930 30.674 3.977 51.828 o
-11 2 4 4.970 8.585 3.622 113.492 o
-11 3 1 1.095 -0.003 2.582 311.552 o
-11 3 2 13.750 29.633 4.433 54.112 o
-10 -14 1 207.522 217.366 7.595 6.253 o
-10 -13 1 217.597 208.495 7.941 6.058 o
-10 -13 2 162.955 173.800 6.745 8.190 o
-10 -13 3 9.641 7.284 3.577 99.072 o
-10 -13 4 89.973 82.401 5.011 16.486 o
-10 -12 1 76.608 67.751 3.573 21.299 o
-10 -12 2 184.232 154.230 5.238 8.338 o
-10 -12 3 230.180 235.979 6.557 5.875 o
-10 -12 4 182.310 207.171 6.324 7.288 o
-10 -12 5 73.879 68.987 4.649 20.059 o
-10 -11 1 1.424 2.733 1.673 462.941 o
-10 -11 2 143.131 146.625 4.961 10.240 o
-10 -11 3 25.122 28.051 2.724 58.294 o
-10 -11 4 106.598 109.384 4.622 13.931 o
-10 -11 5 3.879 8.642 2.775 162.962 o
-10 -11 6 5.364 10.262 2.297 168.999 o
-10 -10 1 791.089 744.843 10.897 1.250 o
-10 -10 2 499.313 497.962 8.885 2.292 o
-10 -10 3 57.104 51.845 4.107 26.463 o
-10 -10 4 11.985 11.460 3.110 96.661 o
-10 -10 5 36.157 60.651 4.244 31.358 o
-10 -10 6 47.237 53.352 4.019 29.454 o
-10 -10 7 0.490 3.611 2.031 392.154 o
-10 -9 1 4.695 6.630 1.802 239.213 o
-10 -9 2 192.371 221.317 6.794 6.740 o
-10 -9 3 165.487 157.917 5.887 8.700 o
-10 -9 4 158.416 151.512 5.805 9.115 o
-10 -9 5 24.757 26.389 3.407 54.083 o
-10 -9 6 1.367 4.507 2.311 283.362 o
-10 -9 7 0.333 2.972 2.001 428.821 o
-10 -9 8 15.425 25.785 2.964 72.567 o
-10 -8 1 346.588 318.192 7.837 3.744 o
-10 -8 2 8.223 7.028 2.268 158.730 o
-10 -8 3 247.835 256.265 7.228 5.293 o
-10 -8 4 174.284 174.621 6.181 8.024 o
-10 -8 5 81.394 76.321 4.341 18.791 o
-10 -8 6 92.376 105.570 4.991 15.055 o
-10 -8 7 5.232 8.514 1.951 202.478 o
-10 -8 8 28.008 46.152 3.775 40.852 o
-10 -7 1 41.105 43.735 3.173 36.785 o
-10 -7 2 9.017 9.187 2.085 150.952 o
-10 -7 3 2.744 3.369 1.977 312.194 o
-10 -7 4 78.972 66.738 4.765 19.260 o
-10 -7 5 106.230 93.907 5.062 14.260 o
-10 -7 6 26.992 24.644 2.539 59.516 o
-10 -7 7 79.007 93.176 3.846 18.527 o
-10 -7 8 0.877 3.867 2.455 282.681 o
-10 -7 9 0.721 2.178 2.580 289.424 o
-10 -6 1 1.474 4.392 1.511 444.580 o
-10 -6 2 51.340 57.791 4.290 26.771 o
-10 -6 3 144.025 155.501 5.460 9.774 o
-10 -6 4 64.891 50.035 3.421 26.113 o
-10 -6 5 77.336 100.550 4.712 17.256 o
-10 -6 6 62.074 56.174 3.253 26.373 o
-10 -6 7 92.166 86.891 3.671 17.371 o
-10 -6 8 2.353 3.106 2.288 279.101 o
-10 -6 9 76.044 87.853 5.374 17.348 o
-10 -5 1 291.578 270.034 5.652 4.801 o
-10 -5 2 852.665 815.262 10.495 1.124 o
-10 -5 3 153.922 154.865 4.266 9.822 o
-10 -5 4 35.440 33.386 3.554 41.353 o
-10 -5 5 349.886 315.304 6.986 3.805 o
-10 -5 6 91.513 72.252 3.613 18.491 o
-10 -5 7 1.283 4.480 1.666 415.657 o
-10 -5 8 126.758 101.419 5.431 12.157 o
-10 -5 9 1.692 7.192 2.686 203.799 o
-10 -4 1 6.844 13.079 1.746 166.845 o
-10 -4 2 1.980 6.936 1.723 316.295 o
-10 -4 3 710.971 718.414 8.930 1.433 o
-10 -4 4 71.077 68.458 2.789 23.391 o
-10 -4 5 25.698 26.903 3.106 55.249 o
-10 -4 6 591.284 580.707 9.720 1.836 o
-10 -4 7 3.040 5.554 1.730 302.869 o
-10 -4 8 2.311 5.059 3.468 147.234 o
-10 -4 9 41.215 54.719 4.503 29.715 o
-10 -3 1 929.045 957.654 11.747 0.950 o
-10 -3 2 1055.900 1031.930 12.523 0.805 o
-10 -3 3 1346.080 1321.040 13.131 0.557 o
-10 -3 4 15.519 20.626 1.824 94.647 o
-10 -3 5 11.107 13.157 1.758 132.586 o
-10 -3 6 33.589 36.073 3.198 43.527 o
-10 -3 7 19.829 28.381 3.822 54.568 o
-10 -3 8 9.092 5.809 3.848 95.305 o
-10 -3 9 0.027 -0.196 3.013 258.903 o
-10 -2 1 168.852 162.881 4.003 9.107 o
-10 -2 2 294.194 284.566 5.335 4.708 o
-10 -2 3 47.470 53.378 3.511 30.840 o
-10 -2 4 64.391 61.939 3.154 25.187 o
-10 -2 5 4.894 8.000 1.907 214.760 o
-10 -2 6 23.269 23.496 2.261 68.208 o
-10 -2 7 1.730 3.464 1.891 367.100 o
-10 -2 8 5.321 14.837 2.346 146.893 o
-10 -2 9 3.576 8.179 2.685 174.197 o
-10 -1 1 363.573 366.853 7.122 3.473 o
-10 -1 2 30.498 40.346 2.686 46.862 o
-10 -1 3 32.255 29.242 2.462 51.452 o
-10 -1 4 59.893 55.982 3.483 26.538 o
-10 -1 5 162.351 155.857 4.988 9.189 o
-10 -1 6 5.939 6.657 1.760 219.287 o
-10 -1 7 71.871 83.194 3.456 20.916 o
-10 -1 8 140.620 164.166 5.554 9.692 o
-10 0 1 735.766 670.884 10.761 1.401 o
-10 0 2 231.532 231.542 5.799 6.032 o
-10 0 3 181.924 190.521 6.712 7.403 o
-10 0 4 10.308 14.716 2.126 122.830 o
-10 0 5 80.552 75.634 3.747 19.726 o
-10 0 6 3.095 4.592 1.516 349.940 o
-10 0 7 0.154 7.027 1.801 376.517 o
-10 0 8 40.717 44.545 3.322 36.231 o
-10 1 1 28.195 30.172 3.211 50.241 o
-10 1 2 6.535 8.613 1.894 187.871 o
-10 1 3 2.683 4.072 1.912 312.654 o
-10 1 4 64.287 67.621 3.587 23.793 o
-10 1 5 167.535 166.007 5.361 8.672 o
-10 1 6 54.665 49.123 3.291 29.631 o
-10 1 7 62.415 60.454 3.276 25.666 o
-10 2 1 13.785 18.298 2.880 85.979 o
-10 2 2 51.527 49.194 3.852 29.200 o
-10 2 3 13.084 21.121 3.226 78.244 o
-10 2 4 8.144 14.348 2.875 112.417 o
-10 2 5 44.881 47.648 3.265 33.761 o
-10 2 6 38.025 46.797 3.271 37.224 o
-10 3 1 24.462 23.340 4.118 49.766 o
-10 3 2 0.651 1.786 2.381 339.708 o
-10 3 3 67.744 95.596 6.340 16.491 o
-10 3 4 1.685 3.591 2.363 279.122 o
-10 3 5 0.438 7.762 2.801 206.754 o
-10 4 1 228.791 239.501 7.990 5.579 o
-10 4 2 8.626 13.770 2.850 112.333 o
-10 4 3 112.022 148.651 6.613 10.845 o
-10 5 1 0.784 3.709 2.696 249.789 o
-9 -14 1 28.375 47.530 4.076 38.646 o
-9 -14 2 21.670 18.927 3.317 63.518 o
-9 -14 3 13.551 15.585 2.939 89.258 o
-9 -13 1 67.808 64.058 4.319 22.135 o
-9 -13 2 79.644 73.408 4.669 18.810 o
-9 -13 3 160.172 171.394 6.703 8.335 o
-9 -13 4 13.363 14.757 3.022 89.302 o
-9 -13 5 2.073 9.187 2.429 206.895 o
-9 -12 1 22.939 27.222 3.074 58.611 o
-9 -12 2 8.195 7.353 2.156 162.920 o
-9 -12 3 11.702 19.839 2.989 87.496 o
-9 -12 4 129.262 130.440 5.827 10.907 o
-9 -12 5 399.614 351.874 10.888 2.987 o
-9 -12 6 140.469 128.934 5.166 10.719 o
-9 -11 1 4.827 7.154 1.849 227.754 o
-9 -11 2 3.360 3.495 1.814 314.489 o
-9 -11 3 139.024 138.061 4.825 10.723 o
-9 -11 4 373.645 352.991 7.842 3.396 o
-9 -11 5 3.529 8.878 2.523 182.200 o
-9 -11 6 0.953 10.413 2.475 210.516 o
-9 -11 7 6.083 8.781 3.803 101.962 o
-9 -10 1 496.527 476.373 8.287 2.369 o
-9 -10 2 119.998 130.936 4.455 12.242 o
-9 -10 3 6.627 4.993 2.198 190.698 o
-9 -10 4 0.104 3.852 2.264 346.924 o
-9 -10 5 128.461 123.956 5.433 11.364 o
-9 -10 6 17.335 22.683 2.623 76.323 o
-9 -10 7 71.748 65.513 3.732 22.203 o
-9 -10 8 0.624 0.850 2.379 361.470 o
-9 -9 1 423.077 432.492 7.642 2.847 o
-9 -9 2 8.037 9.130 2.598 137.228 o
-9 -9 3 26.353 39.288 4.986 36.918 o
-9 -9 4 80.316 85.897 4.425 18.166 o
-9 -9 5 29.385 41.989 3.419 43.238 o
-9 -9 6 119.381 113.940 5.141 12.427 o
-9 -9 7 162.907 179.116 5.691 8.490 o
-9 -9 8 11.682 28.000 3.085 76.108 o
-9 -9 9 193.546 223.938 7.080 6.610 o
-9 -8 1 190.715 205.122 6.044 7.173 o
-9 -8 2 41.761 39.830 3.083 37.805 o
-9 -8 3 68.551 64.974 3.747 22.884 o
-9 -8 4 152.067 131.194 5.220 10.067 o
-9 -8 5 68.367 71.457 4.358 21.267 o
-9 -8 6 73.063 68.317 4.068 21.167 o
-9 -8 7 127.232 125.817 4.695 11.808 o
-9 -8 8 27.398 29.573 2.866 53.734 o
-9 -8 9 59.535 58.827 3.929 25.316 o
-9 -7 1 29.501 30.987 1.994 56.016 o
-9 -7 2 17.770 24.533 2.625 73.524 o
-9 -7 3 269.222 271.129 7.039 4.913 o
-9 -7 4 271.872 273.329 7.196 4.841 o
-9 -7 5 19.883 21.401 2.950 68.644 o
-9 -7 6 73.357 77.733 4.242 20.050 o
-9 -7 7 344.163 321.652 6.754 3.847 o
-9 -7 8 191.732 175.482 4.985 7.835 o
-9 -7 9 0.039 1.513 2.311 393.211 o
-9 -7 10 44.804 49.178 4.300 30.113 o
-9 -6 1 6.202 10.013 1.761 190.630 o
-9 -6 2 112.338 103.229 4.553 13.762 o
-9 -6 3 90.449 80.818 3.899 17.755 o
-9 -6 4 21.199 21.596 2.510 71.107 o
-9 -6 5 2.775 1.102 1.834 386.631 o
-9 -6 6 26.157 34.815 3.309 49.308 o
-9 -6 7 114.353 104.333 3.783 14.075 o
-9 -6 8 7.969 12.976 1.983 148.138 o
-9 -6 9 4.076 14.072 3.643 104.972 o
-9 -6 10 23.160 13.396 3.913 58.445 o
-9 -5 1 176.647 162.936 4.101 8.782 o
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10 3 10 0.340 0.850 1.571 761.123 o
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10 6 6 506.311 500.233 7.158 2.323 o
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10 9 9 242.168 212.653 5.914 5.989 o
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10 11 9 73.297 76.687 3.900 20.637 o
10 11 10 0.009 1.028 2.011 526.882 o
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12 6 6 15.425 16.783 2.489 90.447 o
12 6 7 243.913 250.049 6.253 5.569 o
12 6 8 120.524 99.909 5.131 12.842 o
12 6 9 8.389 8.766 2.589 136.483 o
12 6 10 42.233 34.915 5.555 28.770 o
12 6 11 19.712 23.726 3.250 63.624 o
12 7 0 370.911 364.216 8.939 3.288 o
12 7 1 0.758 2.862 2.051 392.610 o
12 7 2 36.683 36.811 4.157 36.678 o
12 7 3 5.213 8.131 2.253 185.065 o
12 7 4 37.813 37.452 3.068 40.863 o
12 7 5 12.023 12.148 2.303 115.913 o
12 7 6 9.095 7.213 2.097 158.109 o
12 7 7 3.298 9.580 2.485 183.507 o
12 7 8 33.263 35.655 3.488 42.380 o
12 7 9 102.423 91.667 5.587 14.204 o
12 7 10 147.750 150.681 6.280 9.346 o
12 7 11 164.922 182.118 6.972 7.915 o
12 8 0 56.937 61.365 4.062 25.361 o
12 8 1 5.659 7.528 2.312 179.603 o
12 8 2 153.799 157.892 5.795 9.175 o
12 8 3 8.000 11.210 2.398 138.531 o
12 8 4 28.339 23.929 2.770 56.539 o
12 8 5 41.683 38.566 3.209 37.708 o
12 8 6 4.036 15.815 5.251 62.942 o
12 8 7 36.026 37.980 2.983 42.228 o
12 8 8 44.644 48.726 3.982 31.306 o
12 8 9 60.226 58.377 4.128 24.775 o
12 8 10 101.623 114.620 5.629 13.306 o
12 8 11 7.127 9.600 2.729 136.144 o
12 9 0 4.796 9.264 2.542 165.458 o
12 9 1 0.523 0.687 2.088 464.661 o
12 9 2 72.092 67.897 4.192 21.186 o
12 9 3 107.262 114.637 5.055 13.336 o
12 9 4 427.652 413.241 9.349 2.777 o
12 9 5 229.742 223.556 9.751 5.296 o
12 9 6 39.220 47.120 4.748 30.861 o
12 9 7 5.472 7.551 2.391 176.549 o
12 9 8 148.299 162.886 5.478 9.427 o
12 9 9 22.962 20.305 2.656 67.615 o
12 9 10 4.014 9.448 2.255 191.717 o
12 10 0 23.606 26.417 4.258 47.978 o
12 10 1 18.305 16.925 3.144 73.064 o
12 10 2 0.361 1.581 1.991 479.964 o
12 10 3 2.526 3.770 2.401 250.921 o
12 10 4 44.432 49.557 4.935 28.070 o
12 10 5 362.117 353.498 11.738 3.127 o
12 10 6 117.035 107.924 5.129 12.807 o
12 10 7 1.451 2.640 2.327 306.389 o
12 10 8 16.695 27.834 2.804 70.315 o
12 10 9 42.522 41.725 3.228 36.377 o
12 11 0 52.551 64.528 4.378 25.340 o
12 11 1 58.869 72.036 4.450 22.886 o
12 11 2 51.936 53.500 3.915 28.211 o
12 11 3 69.055 78.100 6.490 17.110 o
12 11 4 50.098 57.905 10.045 13.909 o
12 11 5 6.102 10.894 3.482 108.754 o
12 11 6 3.218 5.560 2.338 226.530 o
12 11 7 25.143 28.175 3.364 53.082 o
12 11 8 18.164 13.444 2.421 88.498 o
12 12 0 63.742 65.677 4.419 22.598 o
12 12 1 88.973 90.956 4.939 16.203 o
12 12 2 77.995 78.401 8.512 13.333 o
12 12 3 136.457 125.122 7.584 9.642 o
12 12 4 1.253 3.706 3.326 173.083 o
12 12 5 0.401 5.263 3.266 179.129 o
12 12 6 21.180 24.568 3.273 60.716 o
12 12 7 0.072 2.195 2.389 353.444 o
12 13 1 30.364 25.400 4.534 41.367 o
12 13 2 47.299 40.014 6.686 22.974 o
12 13 3 3.934 4.957 4.403 95.553 o
12 13 4 0.391 3.541 6.001 62.378 o
13 0 2 0.672 8.675 2.975 181.660 o
13 0 3 162.502 163.950 7.002 8.261 o
13 0 4 8.232 17.136 4.992 60.645 o
13 1 0 38.590 39.639 5.124 30.938 o
13 1 1 7.329 6.801 2.717 145.066 o
13 1 2 63.014 62.133 6.371 19.158 o
13 1 3 138.040 124.468 7.959 9.368 o
13 1 4 0.357 1.769 3.015 233.139 o
13 1 5 16.926 25.933 3.590 62.141 o
13 1 6 28.542 28.727 4.037 44.833 o
13 2 0 0.866 0.564 2.492 329.506 o
13 2 1 173.979 173.099 6.789 7.846 o
13 2 2 3.579 7.915 3.561 124.731 o
13 2 3 140.210 151.010 6.487 9.548 o
13 2 4 761.122 750.811 14.411 1.231 o
13 2 5 158.240 156.681 6.550 8.715 o
13 2 6 1.133 1.695 6.164 59.489 o
13 2 7 23.458 11.621 3.350 65.961 o
13 2 8 4.129 7.222 3.161 143.934 o
13 3 0 1.974 6.993 2.863 185.621 o
13 3 1 3.270 11.585 2.659 162.028 o
13 3 2 167.010 147.772 7.709 8.079 o
13 3 3 71.510 70.205 4.582 20.458 o
13 3 4 226.723 248.577 7.973 5.542 o
13 3 5 53.173 64.472 5.302 22.994 o
13 3 6 22.951 19.403 3.537 59.047 o
13 3 7 313.913 313.878 8.465 3.990 o
13 3 8 53.846 40.611 3.517 30.827 o
13 4 0 157.931 159.233 5.288 9.187 o
13 4 1 227.837 207.434 7.058 6.081 o
13 4 2 163.429 163.997 6.337 8.493 o
13 4 3 5.438 4.934 2.402 191.823 o
13 4 4 197.008 193.544 7.315 6.809 o
13 4 5 17.377 19.780 2.819 76.662 o
13 4 6 26.895 20.621 2.712 60.927 o
13 4 7 0.012 2.932 2.227 381.692 o
13 4 8 136.500 143.641 5.109 10.573 o
13 4 9 0.027 3.289 2.562 296.959 o
13 5 0 6.045 4.747 3.127 140.939 o
13 5 1 4.839 9.342 2.146 189.218 o
13 5 2 147.198 155.486 5.087 9.794 o
13 5 3 6.263 9.548 2.194 169.153 o
13 5 4 23.990 25.357 2.935 59.695 o
13 5 5 24.175 26.424 3.047 57.804 o
13 5 6 45.662 55.144 3.786 30.378 o
13 5 7 2.203 5.207 2.217 265.703 o
13 5 8 15.926 16.452 2.862 83.166 o
13 5 9 26.639 27.032 3.506 51.040 o
13 6 0 120.332 108.520 5.157 12.536 o
13 6 1 72.864 78.858 4.517 19.637 o
13 6 2 41.776 50.038 3.174 34.915 o
13 6 3 30.435 25.413 3.480 48.503 o
13 6 4 4.474 8.548 3.306 129.870 o
13 6 5 206.155 198.900 6.634 6.723 o
13 6 6 8.345 13.298 2.719 118.904 o
13 6 7 31.938 38.795 3.427 42.537 o
13 6 8 0.663 0.101 2.929 257.101 o
13 6 9 10.149 7.527 2.608 128.619 o
13 7 0 564.357 559.602 11.707 1.875 o
13 7 1 84.919 82.207 4.667 17.508 o
13 7 2 1.220 10.805 2.471 203.822 o
13 7 3 45.995 55.133 3.918 29.873 o
13 7 4 0.289 9.593 2.522 223.478 o
13 7 5 47.329 47.923 3.600 31.659 o
13 7 6 7.646 4.586 2.040 190.535 o
13 7 7 6.631 13.753 3.317 106.244 o
13 7 8 6.278 7.938 2.546 157.703 o
13 7 9 173.535 167.666 6.838 7.923 o
13 8 0 323.376 332.540 8.991 3.764 o
13 8 1 10.546 11.848 3.761 84.750 o
13 8 2 0.062 0.027 2.251 459.519 o
13 8 3 65.346 64.676 4.113 22.945 o
13 8 4 0.010 1.329 2.087 480.136 o
13 8 5 16.890 23.678 2.906 72.541 o
13 8 6 75.514 70.396 10.469 11.347 o
13 8 7 1.229 6.245 3.040 183.851 o
13 8 8 88.035 74.410 4.717 17.545 o
13 8 9 191.029 190.129 7.235 7.015 o
13 9 0 216.234 209.498 7.201 6.255 o
13 9 1 28.545 20.536 3.023 56.303 o
13 9 2 12.850 16.049 2.872 91.988 o
13 9 3 1.457 2.052 2.235 334.964 o
13 9 4 1.499 5.296 2.457 249.523 o
13 9 5 5.646 8.696 3.053 134.114 o
13 9 6 5.639 6.186 3.685 113.393 o
13 9 7 31.644 18.877 4.664 41.760 o
13 9 8 18.063 19.819 3.938 60.572 o
13 10 0 24.826 25.401 4.144 48.317 o
13 10 1 0.369 1.777 2.604 301.650 o
13 10 2 13.111 14.834 2.812 94.322 o
13 10 3 224.227 231.317 7.366 5.860 o
13 10 4 62.299 74.052 5.973 19.160 o
13 10 5 217.971 238.946 10.008 5.295 o
13 10 6 246.637 276.592 10.653 4.550 o
13 10 7 273.061 252.396 11.871 4.180 o
13 10 8 15.462 20.384 4.794 53.074 o
13 11 0 48.296 40.677 3.762 32.180 o
13 11 1 12.659 19.674 3.015 84.678 o
13 11 2 114.633 114.761 5.509 12.463 o
13 11 3 171.277 156.750 8.394 7.542 o
13 11 4 3.845 4.977 3.317 145.330 o
13 11 5 91.112 87.562 10.175 10.473 o
13 11 6 152.368 151.137 8.230 8.248 o
14 4 1 0.154 0.732 2.574 334.168 o
14 4 2 87.932 103.760 5.444 15.110 o
14 4 3 41.300 45.211 5.383 28.119 o
14 4 4 167.949 156.737 6.670 8.333 o
14 4 5 40.594 30.372 3.512 39.328 o
14 5 0 12.137 6.988 5.185 59.145 o
14 5 1 14.002 17.923 4.631 58.070 o
14 5 2 4.832 5.862 5.577 62.849 o
14 5 3 52.477 50.967 4.116 27.892 o
14 5 4 0.015 1.155 2.572 331.866 o
14 5 5 3.988 5.609 2.364 210.703 o
14 5 6 50.869 54.177 4.126 27.867 o
14 6 0 248.308 233.361 9.895 4.940 o
14 6 1 0.029 3.882 4.566 104.919 o
14 6 2 180.691 165.562 10.848 6.279 o
14 6 3 18.398 21.927 3.318 66.212 o
14 6 4 57.726 56.572 4.119 25.643 o
14 6 5 0.962 1.359 2.554 299.372 o
14 6 6 0.607 0.326 3.196 217.290 o
14 7 0 190.897 178.076 6.877 7.279 o
14 7 1 66.526 62.357 4.395 22.418 o
14 7 2 138.759 152.807 6.691 9.468 o
14 7 3 178.611 175.800 6.711 7.699 o
14 7 4 394.545 373.095 11.994 2.864 o
14 7 5 128.188 117.907 5.444 11.550 o
14 7 6 14.403 12.396 3.571 78.837 o
14 8 0 75.106 68.067 4.657 19.923 o
14 8 1 8.051 11.647 2.816 121.364 o
14 8 2 26.410 24.914 3.705 50.694 o
14 8 3 236.546 242.216 7.832 5.465 o
14 8 4 200.335 197.651 7.022 6.768 o
14 8 5 12.536 13.244 3.768 78.233 o
14 8 6 40.695 36.054 4.522 33.359 o
14 9 1 9.550 11.539 3.015 108.178 o
14 9 2 27.130 29.259 4.544 42.140 o
14 9 3 0.036 0.123 2.646 332.806 o
14 9 4 0.101 0.644 2.842 279.727 o
14 9 5 14.271 17.150 3.849 69.611 o
;
_iucr_refine_instructions_details
;
TITL tlg4xr1_a.res in P-1
REM Old TITL tlg4xr1 in P-1 #2
REM SHELXT solution in P-1
REM R1 0.221, Rweak 0.024, Alpha 0.059, Orientation as input
REM Formula found by SHELXT: C32 B2 N3 O2 F6
CELL 0.71073 11.510968 12.425385 13.183068 85.106 78.7779 64.9447
ZERR 2 0.000317 0.000295 0.000277 0.0018 0.002 0.0025
LATT 1
SFAC C H B Cl F N O
UNIT 64 82 2 4 8 8 4
L.S. 20
PLAN 20
TEMP -173.15
BOND $H
LIST 6
fmap 2
ACTA
SHEL 999 0.8
WGHT 0.036747 1.229549
FVAR 0.391556 0.458083
REM
REM
REM
PART 1
Cl2 4 0.64807 0.08010 0.05316 21.00000 0.06027 0.09642 0.04074 =
0.00663 -0.01379 -0.03601
Cl1 4 0.89366 -0.13939 0.00217 21.00000 0.05188 0.05351 0.04201 =
-0.00740 -0.00621 -0.00709
PART 0
F003 5 0.98678 -0.09681 0.35618 11.00000 0.03036 0.03056 0.03853 =
0.00472 -0.00658 -0.01062
O004 7 0.48235 0.24523 0.71789 11.00000 0.02164 0.02116 0.01804 =
0.00404 -0.00604 -0.00894
O005 7 0.36688 0.14794 0.61248 11.00000 0.02331 0.01819 0.02784 =
0.00292 -0.00459 -0.01228
F006 5 0.90882 0.01158 0.21780 11.00000 0.03096 0.04466 0.04087 =
0.00358 -0.01685 -0.00865
F007 5 1.12459 -0.11507 0.20372 11.00000 0.03495 0.04437 0.03940 =
0.00085 0.00084 0.00220
F008 5 1.04188 0.05447 0.29791 11.00000 0.03270 0.03194 0.08303 =
0.00384 -0.01784 -0.01749
N009 6 0.56842 0.33716 0.36173 11.00000 0.01813 0.02331 0.01929 =
0.00198 -0.00347 -0.00962
N00A 6 0.15058 0.56344 0.56883 11.00000 0.01660 0.01888 0.02334 =
0.00028 -0.00612 -0.00689
N00B 6 -0.22375 0.74113 0.72701 11.00000 0.01980 0.02095 0.03021 =
-0.00308 -0.00391 -0.00959
N10 6 0.68199 0.43610 0.05950 11.00000 0.03449 0.03902 0.02135 =
0.00147 -0.00223 -0.01511
C00D 1 0.60778 0.26320 0.44471 11.00000 0.01984 0.01855 0.02157 =
0.00110 -0.00697 -0.01139
C00E 1 0.38486 0.36015 0.54016 11.00000 0.01994 0.01664 0.01844 =
-0.00106 -0.00601 -0.01042
C00F 1 0.45541 0.44050 0.37489 11.00000 0.01990 0.02071 0.02120 =
0.00095 -0.00690 -0.01219
C00G 1 0.23817 0.55352 0.47828 11.00000 0.01975 0.01871 0.02320 =
-0.00005 -0.00779 -0.01115
C00H 1 0.73476 0.17254 0.43602 11.00000 0.01804 0.02124 0.02346 =
-0.00127 -0.00359 -0.01049
AFIX 43
H00H 2 0.79353 0.15892 0.37207 11.00000 -1.20000
AFIX 0
C00I 1 0.56548 0.21048 0.62646 11.00000 0.02003 0.01718 0.02091 =
0.00065 -0.00486 -0.01197
C00J 1 0.27339 0.35683 0.60911 11.00000 0.01756 0.02182 0.01916 =
0.00107 -0.00662 -0.01062
C00K 1 0.15964 0.46405 0.62899 11.00000 0.01934 0.02264 0.02213 =
0.00111 -0.00752 -0.01100
C00L 1 0.26792 0.24939 0.65307 11.00000 0.01896 0.02228 0.02261 =
0.00299 -0.00804 -0.01060
C00M 1 0.36055 0.45202 0.46624 11.00000 0.01836 0.01879 0.01950 =
0.00066 -0.00707 -0.01087
C00N 1 0.77268 0.10405 0.52100 11.00000 0.01704 0.01705 0.03179 =
0.00007 -0.00727 -0.00687
AFIX 43
H00N 2 0.85750 0.04130 0.51428 11.00000 -1.20000
AFIX 0
C00O 1 0.51748 0.27744 0.53844 11.00000 0.01850 0.01662 0.02059 =
0.00031 -0.00541 -0.01068
C00P 1 0.42607 0.52793 0.29817 11.00000 0.02532 0.02379 0.01962 =
0.00190 -0.00587 -0.01509
AFIX 43
H00P 2 0.48757 0.52103 0.23669 11.00000 -1.20000
AFIX 0
C00Q 1 0.30622 0.62481 0.31282 11.00000 0.03050 0.01932 0.02359 =
0.00571 -0.01271 -0.01547
AFIX 43
H00Q 2 0.28744 0.68377 0.26018 11.00000 -1.20000
AFIX 0
C00R 1 0.21258 0.63979 0.40048 11.00000 0.02314 0.01702 0.02739 =
0.00176 -0.01039 -0.00883
AFIX 43
H00R 2 0.13185 0.70794 0.40766 11.00000 -1.20000
AFIX 0
C00S 1 0.69025 0.12380 0.61723 11.00000 0.02213 0.01802 0.02578 =
0.00375 -0.00909 -0.01050
AFIX 43
H00S 2 0.72041 0.07762 0.67563 11.00000 -1.20000
AFIX 0
C00T 1 0.05583 0.46786 0.70810 11.00000 0.01791 0.02940 0.02720 =
0.00114 -0.00396 -0.00749
AFIX 43
H00T 2 -0.01611 0.54110 0.72838 11.00000 -1.20000
AFIX 0
C00U 1 0.03681 0.67740 0.59468 11.00000 0.01727 0.02012 0.02762 =
-0.00253 -0.00738 -0.00667
AFIX 23
H00a 2 0.01533 0.68668 0.67078 11.00000 -1.20000
H00b 2 0.06048 0.74291 0.56525 11.00000 -1.20000
AFIX 0
C00V 1 -0.08461 0.68906 0.55488 11.00000 0.02023 0.02377 0.02696 =
0.00075 -0.00947 -0.00885
AFIX 23
H00c 2 -0.07911 0.71374 0.48132 11.00000 -1.20000
H00d 2 -0.09075 0.61161 0.56034 11.00000 -1.20000
AFIX 0
C00W 1 -0.20436 0.78171 0.61991 11.00000 0.01947 0.02278 0.03442 =
0.00234 -0.00971 -0.00760
AFIX 23
H00e 2 -0.28227 0.79772 0.58947 11.00000 -1.20000
H00f 2 -0.19374 0.85681 0.61901 11.00000 -1.20000
AFIX 0
C00X 1 0.16290 0.25320 0.72586 11.00000 0.02637 0.02955 0.02917 =
0.00862 -0.00653 -0.01701
AFIX 43
H00X 2 0.15967 0.18199 0.75579 11.00000 -1.20000
AFIX 0
C00Y 1 0.06129 0.36316 0.75507 11.00000 0.02169 0.03927 0.02861 =
0.00474 -0.00003 -0.01501
AFIX 43
H00Y 2 -0.00712 0.36582 0.80979 11.00000 -1.20000
AFIX 0
C00Z 1 0.64475 0.30356 0.25638 11.00000 0.02230 0.02791 0.02191 =
-0.00016 -0.00526 -0.01147
AFIX 23
H00g 2 0.68678 0.21580 0.25154 11.00000 -1.20000
H00i 2 0.58417 0.33343 0.20620 11.00000 -1.20000
AFIX 0
C010 1 0.51864 0.17237 0.80654 11.00000 0.03357 0.02899 0.02254 =
0.00840 -0.00621 -0.00863
AFIX 137
H01a 2 0.53895 0.08988 0.79115 11.00000 -1.50000
H01b 2 0.59544 0.17678 0.82405 11.00000 -1.50000
H01c 2 0.44637 0.20056 0.86512 11.00000 -1.50000
AFIX 0
C011 1 0.35808 0.03829 0.64407 11.00000 0.03393 0.02054 0.04461 =
0.00597 -0.00605 -0.01621
AFIX 137
H01d 2 0.43132 -0.02723 0.60497 11.00000 -1.50000
H01e 2 0.36092 0.02580 0.71812 11.00000 -1.50000
H01f 2 0.27596 0.04113 0.63079 11.00000 -1.50000
AFIX 0
C012 1 0.74968 0.35050 0.22525 11.00000 0.02559 0.03847 0.02764 =
0.00320 -0.00678 -0.01776
AFIX 23
H01g 2 0.71632 0.43277 0.25062 11.00000 -1.20000
H01h 2 0.82702 0.30046 0.25657 11.00000 -1.20000
AFIX 0
C013 1 0.78750 0.34825 0.10754 11.00000 0.02392 0.03890 0.02929 =
-0.00084 0.00228 -0.01354
AFIX 23
H01i 2 0.80928 0.26814 0.08199 11.00000 -1.20000
H01j 2 0.86590 0.36471 0.08757 11.00000 -1.20000
AFIX 0
C014 1 -0.29238 0.66462 0.73836 11.00000 0.02627 0.02868 0.04093 =
-0.00202 -0.00529 -0.01574
AFIX 137
H01k 2 -0.38018 0.71005 0.72274 11.00000 -1.50000
H01l 2 -0.24476 0.59763 0.69046 11.00000 -1.50000
H01m 2 -0.29844 0.63464 0.80951 11.00000 -1.50000
AFIX 0
C015 1 -0.29489 0.84093 0.79782 11.00000 0.03581 0.03267 0.04328 =
-0.01208 0.00170 -0.01734
AFIX 137
H01n 2 -0.24736 0.89124 0.79167 11.00000 -1.50000
H01o 2 -0.38163 0.88758 0.78057 11.00000 -1.50000
H01p 2 -0.30355 0.81115 0.86889 11.00000 -1.50000
AFIX 0
C016 1 0.68870 0.40260 -0.04565 11.00000 0.05081 0.06442 0.02549 =
0.00112 -0.00404 -0.03006
AFIX 137
H01q 2 0.77038 0.39806 -0.08853 11.00000 -1.50000
H01r 2 0.68532 0.32500 -0.04450 11.00000 -1.50000
H01s 2 0.61489 0.46226 -0.07452 11.00000 -1.50000
AFIX 0
B017 3 1.01591 -0.03685 0.26841 11.00000 0.01972 0.02530 0.03509 =
0.00194 -0.00682 -0.00602
C018 1 0.67996 0.55325 0.05883 11.00000 0.06211 0.04472 0.03892 =
0.00642 -0.00814 -0.02545
AFIX 137
H01t 2 0.67221 0.57672 0.12980 11.00000 -1.50000
H01u 2 0.76083 0.55227 0.01721 11.00000 -1.50000
H01v 2 0.60547 0.61022 0.02901 11.00000 -1.50000
AFIX 0
PART 1
C19 1 0.80740 0.01762 0.01452 21.00000 0.04588 0.05004 0.01965 =
0.00822 -0.01305 -0.00964
AFIX 23
H19a 2 0.82602 0.05246 -0.05374 21.00000 -1.20000
H19b 2 0.84650 0.04321 0.06302 21.00000 -1.20000
AFIX 0
PART 0
PART 2
Cl2A 4 0.64185 0.05647 0.04673 -21.00000 0.03171 0.09504 0.04113 =
0.02108 -0.00361 -0.00728
C19A 1 0.81947 -0.01901 0.01342 -21.00000 0.03173 0.14467 0.04569 =
0.03179 -0.00290 -0.00376
AFIX 23
H19c 2 0.85104 0.00593 -0.05585 -21.00000 -1.20000
H19d 2 0.86122 -0.00143 0.06490 -21.00000 -1.20000
AFIX 0
Cl1A 4 0.85299 -0.17024 0.01469 -21.00000 0.07976 0.15028 0.04785 =
0.00237 -0.02279 -0.00709
HKLF 4
END
Q1 1 1.083333 0.025 0.244444 11 0.05 0.36
Q2 1 1.083333 -0.15 0.177778 11 0.05 0.35
Q3 1 0.666667 0.375 0.288889 11 0.05 0.35
Q4 1 0.305556 0.5 0.466667 11 0.05 0.34
Q5 1 0.944444 0.05 0.2 11 0.05 0.3
Q6 1 0.694444 0.3 0.177778 11 0.05 0.29
Q7 1 0.777778 -0.1 0 11 0.05 0.28
Q8 1 0.222222 0.6 0.444444 11 0.05 0.27
Q9 1 -0.138889 0.75 0.6 11 0.05 0.27
Q10 1 -0.027778 0.675 0.577778 11 0.05 0.26
Q11 1 0.305556 0.35 0.555556 11 0.05 0.26
Q12 1 0.194444 0.25 0.666667 11 0.05 0.26
Q13 1 0.083333 0.425 0.755556 11 0.05 0.26
Q14 1 0.277778 0.3 0.622222 11 0.05 0.24
Q15 1 0.444444 0.3 0.533333 11 0.05 0.24
Q16 1 0.555556 0.225 0.577778 11 0.05 0.24
Q17 1 0.444444 0.5 0.355556 11 0.05 0.24
Q18 1 0.361111 0.55 0.288889 11 0.05 0.24
Q19 1 0.222222 0.4 0.622222 11 0.05 0.24
Q20 1 0.416667 0.45 0.422222 11 0.05 0.23
REM The information below was added by Olex2.
REM
REM R1 = 0.0459 for 6350 Fo > 4sig(Fo) and 0.0507 for all 6857 data
REM 440 parameters refined using 0 restraints
REM Highest difference peak 0.3598, deepest hole -0.2530
REM Mean Shift 0.0000, Max Shift 0.0009.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0507
REM R1_gt = 0.0459
REM wR_ref = 0.1060
REM GOOF = 1.0699
REM Shift_max = 0.0009
REM Shift_mean = 0.0000
REM Reflections_all = 6857
REM Reflections_gt = 6350
REM Parameters = 440
REM Hole = -0.2530
REM Peak = 0.3598
REM Flack = n/a
;
_olex2_submission_original_sample_id tlg4xr1
_olex2_submission_special_instructions 'No special instructions were received'