# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018
#######################################################################
#
# 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
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data_m18_a03sad
_database_code_depnum_ccdc_archive 'CCDC 1840367'
_audit_update_record
;
2018-04-29 deposited with the CCDC.
2018-05-18 downloaded from the CCDC.
;
_audit_creation_date 2018-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2018/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C26 H33 B Br2 O2'
_chemical_formula_sum 'C26 H33 B Br2 O2'
_chemical_formula_weight 548.15
_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'
B B 0.0013 0.0007 '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'
Br Br -0.2901 2.4595 '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 9.0914(12)
_cell_length_b 10.6006(14)
_cell_length_c 14.3655(18)
_cell_angle_alpha 71.643(2)
_cell_angle_beta 86.345(2)
_cell_angle_gamma 78.848(2)
_cell_volume 1289.2(3)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 4676
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.66
_cell_measurement_theta_min 2.28
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 3.163
_exptl_absorpt_correction_T_max 0.7461
_exptl_absorpt_correction_T_min 0.3691
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1344 before and 0.0644 after correction.
The Ratio of minimum to maximum transmission is 0.4947.
The \l/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.412
_exptl_crystal_density_meas .
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 560
_exptl_crystal_size_max 0.7
_exptl_crystal_size_mid 0.6
_exptl_crystal_size_min 0.08
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0463
_diffrn_reflns_av_unetI/netI 0.0590
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 20064
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 31.160
_diffrn_reflns_theta_min 2.059
_diffrn_ambient_temperature 100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type 'Bruker APEX CCD'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator 'multilayer optics'
_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 6010
_reflns_number_total 7513
_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 0.967
_refine_diff_density_min -0.715
_refine_diff_density_rms 0.091
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.048
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 289
_refine_ls_number_reflns 7513
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0531
_refine_ls_R_factor_gt 0.0393
_refine_ls_restrained_S_all 1.048
_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^)+(0.0420P)^2^+0.1840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0944
_refine_ls_wR_factor_ref 0.1002
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C6(H6), C7(H7), C11(H11), C13(H13)
2.b Idealised Me refined as rotating group:
C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,
H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,
H25B,H25C), C26(H26A,H26B,H26C)
;
_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
Br1 Br 0.40240(3) 0.69783(3) 0.54017(2) 0.03364(8) Uani 1 1 d . . . . .
Br2 Br -0.21092(2) 0.96077(2) -0.01372(2) 0.02333(7) Uani 1 1 d . . . . .
O1 O 0.30618(16) 0.65571(14) 0.37782(10) 0.0181(3) Uani 1 1 d . . . . .
O2 O -0.00064(15) 0.79202(14) 0.11975(10) 0.0147(3) Uani 1 1 d . . . . .
C1 C 0.2108(2) 0.7120(2) 0.29667(15) 0.0157(4) Uani 1 1 d . . . . .
C2 C 0.1399(2) 0.8365(2) 0.29864(16) 0.0189(4) Uani 1 1 d . . . . .
H2 H 0.070642 0.896318 0.252999 0.023 Uiso 1 1 calc R . . . .
C3 C 0.1905(3) 0.8590(2) 0.38316(17) 0.0230(5) Uani 1 1 d . . . . .
H3 H 0.161036 0.935068 0.403696 0.028 Uiso 1 1 calc R . . . .
C4 C 0.2893(2) 0.7474(2) 0.42650(15) 0.0200(4) Uani 1 1 d . . . . .
C5 C 0.1034(2) 0.67120(19) 0.14030(15) 0.0149(4) Uani 1 1 d . . . . .
C6 C 0.0974(2) 0.6177(2) 0.06590(15) 0.0176(4) Uani 1 1 d . . . . .
H6 H 0.154153 0.536691 0.061667 0.021 Uiso 1 1 calc R . . . .
C7 C -0.0098(2) 0.7064(2) -0.00380(15) 0.0186(4) Uani 1 1 d . . . . .
H7 H -0.036639 0.696518 -0.062173 0.022 Uiso 1 1 calc R . . . .
C8 C -0.0641(2) 0.8082(2) 0.03350(15) 0.0161(4) Uani 1 1 d . . . . .
C9 C 0.3172(2) 0.48370(19) 0.24328(14) 0.0139(4) Uani 1 1 d . . . . .
C10 C 0.4627(2) 0.47494(19) 0.19980(14) 0.0138(4) Uani 1 1 d . . . . .
C11 C 0.5477(2) 0.3477(2) 0.20618(15) 0.0157(4) Uani 1 1 d . . . . .
H11 H 0.644074 0.343089 0.179956 0.019 Uiso 1 1 calc R . . . .
C12 C 0.4953(2) 0.22748(19) 0.24985(15) 0.0154(4) Uani 1 1 d . . . . .
C13 C 0.3541(2) 0.2382(2) 0.29208(15) 0.0176(4) Uani 1 1 d . . . . .
H13 H 0.316605 0.159280 0.321662 0.021 Uiso 1 1 calc R . . . .
C14 C 0.2646(2) 0.3611(2) 0.29275(14) 0.0155(4) Uani 1 1 d . . . . .
C15 C 0.5428(2) 0.59637(19) 0.15083(15) 0.0149(4) Uani 1 1 d . . . . .
C16 C 0.4383(2) 0.7287(2) 0.09807(16) 0.0200(4) Uani 1 1 d . . . . .
H16A H 0.386549 0.716160 0.046380 0.030 Uiso 1 1 calc GR . . . .
H16B H 0.496212 0.798645 0.070848 0.030 Uiso 1 1 calc GR . . . .
H16C H 0.366647 0.754272 0.143973 0.030 Uiso 1 1 calc GR . . . .
C17 C 0.6291(3) 0.6202(2) 0.23064(16) 0.0222(5) Uani 1 1 d . . . . .
H17A H 0.559408 0.645727 0.277495 0.033 Uiso 1 1 calc GR . . . .
H17B H 0.684854 0.691091 0.201056 0.033 Uiso 1 1 calc GR . . . .
H17C H 0.696776 0.538585 0.263181 0.033 Uiso 1 1 calc GR . . . .
C18 C 0.6553(2) 0.5678(2) 0.07214(17) 0.0230(5) Uani 1 1 d . . . . .
H18A H 0.738247 0.499249 0.103064 0.035 Uiso 1 1 calc GR . . . .
H18B H 0.691101 0.649105 0.036219 0.035 Uiso 1 1 calc GR . . . .
H18C H 0.606813 0.537279 0.027988 0.035 Uiso 1 1 calc GR . . . .
C19 C 0.5855(2) 0.0891(2) 0.25185(16) 0.0191(4) Uani 1 1 d . . . . .
C20 C 0.7424(3) 0.0973(2) 0.2068(2) 0.0293(5) Uani 1 1 d . . . . .
H20A H 0.733635 0.155665 0.140287 0.044 Uiso 1 1 calc GR . . . .
H20B H 0.793432 0.008574 0.208028 0.044 Uiso 1 1 calc GR . . . .
H20C H 0.798426 0.132715 0.244085 0.044 Uiso 1 1 calc GR . . . .
C21 C 0.6012(3) -0.0061(2) 0.35784(18) 0.0346(6) Uani 1 1 d . . . . .
H21A H 0.655591 0.029716 0.395692 0.052 Uiso 1 1 calc GR . . . .
H21B H 0.654348 -0.093760 0.358069 0.052 Uiso 1 1 calc GR . . . .
H21C H 0.503400 -0.013738 0.385992 0.052 Uiso 1 1 calc GR . . . .
C22 C 0.5000(3) 0.0289(2) 0.19205(18) 0.0238(5) Uani 1 1 d . . . . .
H22A H 0.404002 0.016973 0.221837 0.036 Uiso 1 1 calc GR . . . .
H22B H 0.556545 -0.056989 0.190798 0.036 Uiso 1 1 calc GR . . . .
H22C H 0.486134 0.089180 0.126242 0.036 Uiso 1 1 calc GR . . . .
C23 C 0.1136(2) 0.3479(2) 0.34854(15) 0.0177(4) Uani 1 1 d . . . . .
C24 C 0.1446(3) 0.2446(2) 0.45129(17) 0.0281(5) Uani 1 1 d . . . . .
H24A H 0.188749 0.157703 0.445028 0.042 Uiso 1 1 calc GR . . . .
H24B H 0.052091 0.238220 0.487155 0.042 Uiso 1 1 calc GR . . . .
H24C H 0.212157 0.273342 0.485713 0.042 Uiso 1 1 calc GR . . . .
C25 C 0.0123(3) 0.2979(2) 0.29139(18) 0.0269(5) Uani 1 1 d . . . . .
H25A H -0.010565 0.364022 0.228403 0.040 Uiso 1 1 calc GR . . . .
H25B H -0.079047 0.284232 0.327367 0.040 Uiso 1 1 calc GR . . . .
H25C H 0.063097 0.214072 0.282716 0.040 Uiso 1 1 calc GR . . . .
C26 C 0.0257(2) 0.4765(2) 0.36627(16) 0.0209(4) Uani 1 1 d . . . . .
H26A H 0.085559 0.507917 0.403972 0.031 Uiso 1 1 calc GR . . . .
H26B H -0.064894 0.457555 0.401529 0.031 Uiso 1 1 calc GR . . . .
H26C H 0.001084 0.544966 0.304453 0.031 Uiso 1 1 calc GR . . . .
B1 B 0.2088(2) 0.6248(2) 0.22916(16) 0.0145(4) 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
Br1 0.04745(17) 0.04189(15) 0.01688(12) -0.00773(10) -0.00856(11) -0.02024(12)
Br2 0.02115(12) 0.01918(11) 0.02503(13) 0.00045(9) -0.00879(9) -0.00220(8)
O1 0.0217(7) 0.0201(7) 0.0133(7) -0.0044(6) -0.0044(6) -0.0052(6)
O2 0.0155(7) 0.0141(6) 0.0140(7) -0.0037(5) -0.0036(5) -0.0012(5)
C1 0.0162(9) 0.0177(9) 0.0128(9) -0.0028(7) -0.0019(7) -0.0048(7)
C2 0.0188(10) 0.0181(9) 0.0198(10) -0.0058(8) 0.0024(8) -0.0039(8)
C3 0.0303(12) 0.0218(10) 0.0224(11) -0.0123(9) 0.0069(9) -0.0110(9)
C4 0.0258(11) 0.0257(10) 0.0132(10) -0.0078(8) 0.0020(8) -0.0138(9)
C5 0.0138(9) 0.0139(8) 0.0170(10) -0.0046(7) 0.0016(7) -0.0032(7)
C6 0.0172(10) 0.0199(9) 0.0172(10) -0.0077(8) 0.0006(8) -0.0040(8)
C7 0.0189(10) 0.0270(10) 0.0124(9) -0.0067(8) -0.0008(8) -0.0089(8)
C8 0.0141(9) 0.0170(9) 0.0143(9) 0.0008(7) -0.0028(7) -0.0050(7)
C9 0.0164(9) 0.0139(8) 0.0113(9) -0.0024(7) -0.0029(7) -0.0044(7)
C10 0.0156(9) 0.0135(8) 0.0125(9) -0.0029(7) -0.0029(7) -0.0041(7)
C11 0.0149(9) 0.0158(9) 0.0171(10) -0.0053(8) -0.0028(7) -0.0033(7)
C12 0.0193(10) 0.0128(8) 0.0150(9) -0.0050(7) -0.0059(8) -0.0019(7)
C13 0.0231(10) 0.0133(8) 0.0170(10) -0.0025(8) -0.0034(8) -0.0074(8)
C14 0.0184(9) 0.0175(9) 0.0113(9) -0.0027(7) -0.0016(7) -0.0074(8)
C15 0.0143(9) 0.0144(8) 0.0166(10) -0.0038(7) -0.0003(7) -0.0055(7)
C16 0.0200(10) 0.0163(9) 0.0197(11) 0.0009(8) 0.0025(8) -0.0056(8)
C17 0.0247(11) 0.0189(10) 0.0230(11) -0.0025(9) -0.0055(9) -0.0090(8)
C18 0.0213(11) 0.0221(10) 0.0267(12) -0.0072(9) 0.0083(9) -0.0097(9)
C19 0.0227(10) 0.0137(9) 0.0219(11) -0.0074(8) -0.0058(9) -0.0010(8)
C20 0.0195(11) 0.0220(11) 0.0504(16) -0.0187(11) -0.0064(10) 0.0011(9)
C21 0.0544(17) 0.0181(10) 0.0258(13) -0.0050(10) -0.0146(12) 0.0077(11)
C22 0.0269(11) 0.0206(10) 0.0282(12) -0.0122(9) 0.0004(9) -0.0068(9)
C23 0.0191(10) 0.0200(9) 0.0143(10) -0.0034(8) 0.0003(8) -0.0075(8)
C24 0.0297(12) 0.0284(12) 0.0201(11) 0.0014(9) 0.0054(9) -0.0075(10)
C25 0.0211(11) 0.0343(12) 0.0327(13) -0.0169(11) 0.0031(10) -0.0125(10)
C26 0.0192(10) 0.0265(11) 0.0178(10) -0.0069(9) 0.0068(8) -0.0082(9)
B1 0.0155(10) 0.0150(10) 0.0133(10) -0.0033(8) 0.0027(8) -0.0060(8)
_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
Br1 C4 1.861(2) . ?
Br2 C8 1.856(2) . ?
O1 C1 1.399(2) . ?
O1 C4 1.347(3) . ?
O2 C5 1.397(2) . ?
O2 C8 1.348(2) . ?
C1 C2 1.360(3) . ?
C1 B1 1.539(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.428(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.338(3) . ?
C5 C6 1.367(3) . ?
C5 B1 1.539(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.419(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.349(3) . ?
C9 C10 1.426(3) . ?
C9 C14 1.427(3) . ?
C9 B1 1.585(3) . ?
C10 C11 1.397(3) . ?
C10 C15 1.552(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.392(3) . ?
C12 C13 1.384(3) . ?
C12 C19 1.529(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.398(3) . ?
C14 C23 1.553(3) . ?
C15 C16 1.534(3) . ?
C15 C17 1.538(3) . ?
C15 C18 1.537(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.535(3) . ?
C19 C21 1.537(3) . ?
C19 C22 1.540(3) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.541(3) . ?
C23 C25 1.538(3) . ?
C23 C26 1.528(3) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
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
C4 O1 C1 106.52(16) . . ?
C8 O2 C5 106.26(15) . . ?
O1 C1 B1 116.48(17) . . ?
C2 C1 O1 107.89(18) . . ?
C2 C1 B1 135.63(19) . . ?
C1 C2 H2 126.0 . . ?
C1 C2 C3 107.95(19) . . ?
C3 C2 H2 126.0 . . ?
C2 C3 H3 127.3 . . ?
C4 C3 C2 105.31(19) . . ?
C4 C3 H3 127.3 . . ?
O1 C4 Br1 115.92(16) . . ?
C3 C4 Br1 131.74(17) . . ?
C3 C4 O1 112.33(19) . . ?
O2 C5 B1 121.43(17) . . ?
C6 C5 O2 107.75(17) . . ?
C6 C5 B1 130.62(19) . . ?
C5 C6 H6 125.7 . . ?
C5 C6 C7 108.63(19) . . ?
C7 C6 H6 125.7 . . ?
C6 C7 H7 127.7 . . ?
C8 C7 C6 104.61(18) . . ?
C8 C7 H7 127.7 . . ?
O2 C8 Br2 116.75(15) . . ?
O2 C8 C7 112.75(18) . . ?
C7 C8 Br2 130.50(16) . . ?
C10 C9 C14 118.31(18) . . ?
C10 C9 B1 121.50(16) . . ?
C14 C9 B1 119.93(17) . . ?
C9 C10 C15 125.30(17) . . ?
C11 C10 C9 119.16(17) . . ?
C11 C10 C15 115.40(17) . . ?
C10 C11 H11 118.4 . . ?
C12 C11 C10 123.26(19) . . ?
C12 C11 H11 118.4 . . ?
C11 C12 C19 123.05(19) . . ?
C13 C12 C11 116.59(18) . . ?
C13 C12 C19 120.37(17) . . ?
C12 C13 H13 118.2 . . ?
C12 C13 C14 123.69(18) . . ?
C14 C13 H13 118.2 . . ?
C9 C14 C23 126.53(18) . . ?
C13 C14 C9 118.85(19) . . ?
C13 C14 C23 114.61(17) . . ?
C16 C15 C10 114.77(16) . . ?
C16 C15 C17 108.65(17) . . ?
C16 C15 C18 105.12(17) . . ?
C17 C15 C10 108.23(16) . . ?
C18 C15 C10 111.45(16) . . ?
C18 C15 C17 108.43(17) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C19 C20 112.58(17) . . ?
C12 C19 C21 110.11(18) . . ?
C12 C19 C22 108.27(17) . . ?
C20 C19 C21 108.9(2) . . ?
C20 C19 C22 108.19(18) . . ?
C21 C19 C22 108.68(19) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C14 108.94(17) . . ?
C25 C23 C14 108.93(17) . . ?
C25 C23 C24 109.44(18) . . ?
C26 C23 C14 116.01(16) . . ?
C26 C23 C24 105.37(18) . . ?
C26 C23 C25 107.98(18) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C1 B1 C9 123.14(18) . . ?
C5 B1 C1 121.91(18) . . ?
C5 B1 C9 114.93(17) . . ?
_shelx_res_file
;
TITL m18_a03sad_a.res in P-1
m18_a03sad.res
created by SHELXL-2018/1 at 09:03:22 on 24-Apr-2018
REM Old TITL m18_a03sad_a.res in P-1
REM SHELXT solution in P-1
REM R1 0.136, Rweak 0.009, Alpha 0.052, Orientation as input
REM Formula found by SHELXT: C27 O2 Br2
CELL 0.71073 9.0914 10.6006 14.3655 71.643 86.345 78.848
ZERR 2 0.0012 0.0014 0.0018 0.002 0.002 0.002
LATT 1
SFAC C H B O Br
UNIT 52 66 2 4 4
L.S. 50
PLAN 20
TEMP 0
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.042000 0.184000
FVAR 0.43951
BR1 5 0.402404 0.697828 0.540173 11.00000 0.04745 0.04189 =
0.01688 -0.00773 -0.00856 -0.02024
BR2 5 -0.210920 0.960773 -0.013723 11.00000 0.02115 0.01918 =
0.02503 0.00045 -0.00879 -0.00220
O1 4 0.306183 0.655710 0.377824 11.00000 0.02172 0.02008 =
0.01328 -0.00443 -0.00441 -0.00524
O2 4 -0.000643 0.792016 0.119753 11.00000 0.01548 0.01410 =
0.01403 -0.00367 -0.00361 -0.00121
C1 1 0.210807 0.711966 0.296671 11.00000 0.01621 0.01766 =
0.01277 -0.00280 -0.00186 -0.00483
C2 1 0.139880 0.836451 0.298642 11.00000 0.01876 0.01814 =
0.01977 -0.00584 0.00237 -0.00393
AFIX 43
H2 2 0.070642 0.896318 0.252999 11.00000 -1.20000
AFIX 0
C3 1 0.190476 0.859016 0.383159 11.00000 0.03031 0.02185 =
0.02235 -0.01227 0.00695 -0.01095
AFIX 43
H3 2 0.161036 0.935068 0.403696 11.00000 -1.20000
AFIX 0
C4 1 0.289273 0.747402 0.426500 11.00000 0.02584 0.02571 =
0.01324 -0.00777 0.00204 -0.01380
C5 1 0.103403 0.671200 0.140304 11.00000 0.01383 0.01388 =
0.01701 -0.00464 0.00156 -0.00315
C6 1 0.097415 0.617706 0.065905 11.00000 0.01722 0.01990 =
0.01723 -0.00767 0.00055 -0.00403
AFIX 43
H6 2 0.154153 0.536691 0.061667 11.00000 -1.20000
AFIX 0
C7 1 -0.009806 0.706385 -0.003797 11.00000 0.01893 0.02701 =
0.01241 -0.00670 -0.00079 -0.00892
AFIX 43
H7 2 -0.036639 0.696518 -0.062173 11.00000 -1.20000
AFIX 0
C8 1 -0.064147 0.808207 0.033498 11.00000 0.01414 0.01702 =
0.01432 0.00084 -0.00280 -0.00495
C9 1 0.317154 0.483704 0.243283 11.00000 0.01636 0.01390 =
0.01133 -0.00243 -0.00292 -0.00439
C10 1 0.462725 0.474942 0.199795 11.00000 0.01558 0.01350 =
0.01254 -0.00291 -0.00294 -0.00412
C11 1 0.547702 0.347696 0.206180 11.00000 0.01488 0.01582 =
0.01706 -0.00525 -0.00278 -0.00331
AFIX 43
H11 2 0.644074 0.343089 0.179956 11.00000 -1.20000
AFIX 0
C12 1 0.495261 0.227483 0.249846 11.00000 0.01933 0.01276 =
0.01498 -0.00503 -0.00590 -0.00192
C13 1 0.354078 0.238229 0.292075 11.00000 0.02305 0.01330 =
0.01701 -0.00251 -0.00339 -0.00743
AFIX 43
H13 2 0.316605 0.159280 0.321662 11.00000 -1.20000
AFIX 0
C14 1 0.264633 0.361107 0.292752 11.00000 0.01836 0.01752 =
0.01130 -0.00273 -0.00164 -0.00737
C15 1 0.542830 0.596368 0.150827 11.00000 0.01430 0.01440 =
0.01657 -0.00378 -0.00030 -0.00546
C16 1 0.438280 0.728744 0.098072 11.00000 0.01998 0.01628 =
0.01968 0.00088 0.00253 -0.00564
AFIX 137
H16A 2 0.386549 0.716160 0.046380 11.00000 -1.50000
H16B 2 0.496212 0.798645 0.070848 11.00000 -1.50000
H16C 2 0.366647 0.754272 0.143973 11.00000 -1.50000
AFIX 0
C17 1 0.629073 0.620181 0.230642 11.00000 0.02473 0.01885 =
0.02300 -0.00248 -0.00550 -0.00900
AFIX 137
H17A 2 0.559408 0.645727 0.277495 11.00000 -1.50000
H17B 2 0.684854 0.691091 0.201056 11.00000 -1.50000
H17C 2 0.696776 0.538585 0.263181 11.00000 -1.50000
AFIX 0
C18 1 0.655308 0.567820 0.072136 11.00000 0.02134 0.02206 =
0.02671 -0.00720 0.00829 -0.00972
AFIX 137
H18A 2 0.738247 0.499249 0.103064 11.00000 -1.50000
H18B 2 0.691101 0.649105 0.036219 11.00000 -1.50000
H18C 2 0.606813 0.537279 0.027988 11.00000 -1.50000
AFIX 0
C19 1 0.585467 0.089059 0.251853 11.00000 0.02271 0.01374 =
0.02191 -0.00736 -0.00582 -0.00105
C20 1 0.742447 0.097273 0.206847 11.00000 0.01952 0.02202 =
0.05037 -0.01868 -0.00638 0.00115
AFIX 137
H20A 2 0.733635 0.155665 0.140287 11.00000 -1.50000
H20B 2 0.793432 0.008574 0.208028 11.00000 -1.50000
H20C 2 0.798426 0.132715 0.244085 11.00000 -1.50000
AFIX 0
C21 1 0.601175 -0.006108 0.357844 11.00000 0.05439 0.01813 =
0.02584 -0.00498 -0.01460 0.00774
AFIX 137
H21A 2 0.655591 0.029716 0.395692 11.00000 -1.50000
H21B 2 0.654348 -0.093760 0.358069 11.00000 -1.50000
H21C 2 0.503400 -0.013738 0.385992 11.00000 -1.50000
AFIX 0
C22 1 0.499992 0.028893 0.192054 11.00000 0.02685 0.02055 =
0.02817 -0.01219 0.00039 -0.00684
AFIX 137
H22A 2 0.404002 0.016973 0.221837 11.00000 -1.50000
H22B 2 0.556545 -0.056989 0.190798 11.00000 -1.50000
H22C 2 0.486134 0.089180 0.126242 11.00000 -1.50000
AFIX 0
C23 1 0.113594 0.347903 0.348541 11.00000 0.01909 0.01998 =
0.01433 -0.00340 0.00035 -0.00754
C24 1 0.144566 0.244555 0.451289 11.00000 0.02971 0.02838 =
0.02011 0.00142 0.00536 -0.00745
AFIX 137
H24A 2 0.188749 0.157703 0.445028 11.00000 -1.50000
H24B 2 0.052091 0.238220 0.487155 11.00000 -1.50000
H24C 2 0.212157 0.273342 0.485713 11.00000 -1.50000
AFIX 0
C25 1 0.012253 0.297857 0.291390 11.00000 0.02112 0.03429 =
0.03268 -0.01687 0.00312 -0.01247
AFIX 137
H25A 2 -0.010565 0.364022 0.228403 11.00000 -1.50000
H25B 2 -0.079047 0.284232 0.327367 11.00000 -1.50000
H25C 2 0.063097 0.214072 0.282716 11.00000 -1.50000
AFIX 0
C26 1 0.025665 0.476538 0.366272 11.00000 0.01920 0.02648 =
0.01784 -0.00687 0.00677 -0.00820
AFIX 137
H26A 2 0.085559 0.507917 0.403972 11.00000 -1.50000
H26B 2 -0.064894 0.457555 0.401529 11.00000 -1.50000
H26C 2 0.001084 0.544966 0.304453 11.00000 -1.50000
AFIX 0
B1 3 0.208828 0.624769 0.229155 11.00000 0.01545 0.01503 =
0.01327 -0.00327 0.00265 -0.00597
HKLF 4
REM m18_a03sad_a.res in P-1
REM R1 = 0.0393 for 6010 Fo > 4sig(Fo) and 0.0531 for all 7513 data
REM 289 parameters refined using 0 restraints
END
WGHT 0.0420 0.1830
REM Highest difference peak 0.967, deepest hole -0.715, 1-sigma level 0.091
Q1 1 -0.1449 0.8910 0.0082 11.00000 0.05 0.97
Q2 1 -0.2767 1.0207 -0.0316 11.00000 0.05 0.89
Q3 1 0.3424 0.7738 0.5137 11.00000 0.05 0.66
Q4 1 -0.1358 0.9610 -0.0524 11.00000 0.05 0.62
Q5 1 -0.1794 1.0047 0.0099 11.00000 0.05 0.57
Q6 1 0.3718 0.6438 0.5206 11.00000 0.05 0.57
Q7 1 0.4643 0.6123 0.5656 11.00000 0.05 0.56
Q8 1 0.2644 0.5542 0.2450 11.00000 0.05 0.56
Q9 1 0.4798 0.7042 0.5064 11.00000 0.05 0.55
Q10 1 0.2056 0.6786 0.2597 11.00000 0.05 0.52
Q11 1 0.6562 0.1034 0.2191 11.00000 0.05 0.47
Q12 1 -0.2333 0.9167 -0.0509 11.00000 0.05 0.47
Q13 1 0.4915 0.6580 0.1318 11.00000 0.05 0.46
Q14 1 0.1486 0.6591 0.1870 11.00000 0.05 0.45
Q15 1 0.5057 0.4141 0.2116 11.00000 0.05 0.45
Q16 1 0.5469 0.1699 0.2473 11.00000 0.05 0.44
Q17 1 0.4229 0.7361 0.5734 11.00000 0.05 0.44
Q18 1 0.1907 0.3584 0.3288 11.00000 0.05 0.43
Q19 1 0.5561 0.0707 0.2188 11.00000 0.05 0.43
Q20 1 -0.0607 0.7293 -0.1242 11.00000 0.05 0.43
;
_shelx_res_checksum 84420
_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_m18_a13sad
_database_code_depnum_ccdc_archive 'CCDC 1840368'
_audit_update_record
;
2018-04-29 deposited with the CCDC.
2018-05-18 downloaded from the CCDC.
;
_audit_creation_date 2018-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2018/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '0.75(C26 H33 B I2 O2)'
_chemical_formula_sum 'C19.50 H24.75 B0.75 I1.50 O1.50'
_chemical_formula_weight 481.60
_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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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 10.7568(12)
_cell_length_b 17.0259(18)
_cell_length_c 22.758(2)
_cell_angle_alpha 94.956(2)
_cell_angle_beta 94.394(2)
_cell_angle_gamma 103.556(2)
_cell_volume 4016.5(7)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 8399
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 25.32
_cell_measurement_theta_min 2.30
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.368
_exptl_absorpt_correction_T_max 0.7452
_exptl_absorpt_correction_T_min 0.5790
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1441 before and 0.0464 after correction.
The Ratio of minimum to maximum transmission is 0.7770.
The \l/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.593
_exptl_crystal_density_meas .
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1896
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0386
_diffrn_reflns_av_unetI/netI 0.0416
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 45558
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.584
_diffrn_reflns_theta_min 0.903
_diffrn_ambient_temperature 100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Bruker APEX CCD'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator 'multilayer optics'
_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 12055
_reflns_number_total 15014
_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 1.579
_refine_diff_density_min -0.719
_refine_diff_density_rms 0.118
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.021
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 865
_refine_ls_number_reflns 15014
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0482
_refine_ls_R_factor_gt 0.0351
_refine_ls_restrained_S_all 1.021
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0835
_refine_ls_wR_factor_ref 0.0901
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C6(H6), C7(H7), C11(H11), C13(H13), C28(H28), C29(H29),
C32(H32), C33(H33), C37(H37), C39(H39), C55(H55), C56(H56), C59(H59), C60(H60),
C64(H64), C66(H66)
2.b Idealised Me refined as rotating group:
C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,
H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,
H25B,H25C), C26(H26A,H26B,H26C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C),
C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,
H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C69(H69A,
H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C73(H73A,H73B,H73C),
C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C), C78(H78A,H78B,
H78C), C79(H79A,H79B,H79C)
;
_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
I1 I -0.03434(3) 0.67706(2) 0.20025(2) 0.03531(8) Uani 1 1 d . . . . .
I2 I 0.32394(2) 1.25540(2) 0.22722(2) 0.02452(7) Uani 1 1 d . . . . .
O1 O 0.1760(2) 0.81657(14) 0.18563(11) 0.0191(6) Uani 1 1 d . . . . .
O2 O 0.3351(2) 1.08464(13) 0.20380(11) 0.0162(5) Uani 1 1 d . . . . .
C1 C 0.2233(4) 0.9013(2) 0.19718(16) 0.0175(8) Uani 1 1 d . . . . .
C2 C 0.1371(4) 0.9304(2) 0.22781(17) 0.0210(8) Uani 1 1 d . . . . .
H2 H 0.144398 0.984675 0.241122 0.025 Uiso 1 1 calc R . . . .
C3 C 0.0343(4) 0.8645(2) 0.23612(17) 0.0235(9) Uani 1 1 d . . . . .
H3 H -0.037749 0.866736 0.255717 0.028 Uiso 1 1 calc R . . . .
C4 C 0.0626(4) 0.7983(2) 0.20984(17) 0.0218(9) Uani 1 1 d . . . . .
C5 C 0.4026(3) 1.0318(2) 0.17792(16) 0.0154(8) Uani 1 1 d . . . . .
C6 C 0.5060(4) 1.0781(2) 0.15586(17) 0.0202(8) Uani 1 1 d . . . . .
H6 H 0.567225 1.058584 0.136220 0.024 Uiso 1 1 calc R . . . .
C7 C 0.5049(3) 1.1610(2) 0.16785(16) 0.0198(8) Uani 1 1 d . . . . .
H7 H 0.564326 1.205906 0.158099 0.024 Uiso 1 1 calc R . . . .
C8 C 0.3999(3) 1.1612(2) 0.19623(16) 0.0177(8) Uani 1 1 d . . . . .
C9 C 0.4321(3) 0.8895(2) 0.13501(16) 0.0153(8) Uani 1 1 d . . . . .
C10 C 0.5425(4) 0.8702(2) 0.16267(16) 0.0176(8) Uani 1 1 d . . . . .
C11 C 0.6274(3) 0.8418(2) 0.12761(16) 0.0179(8) Uani 1 1 d . . . . .
H11 H 0.700960 0.831490 0.146346 0.021 Uiso 1 1 calc R . . . .
C12 C 0.6073(3) 0.8282(2) 0.06624(16) 0.0161(8) Uani 1 1 d . . . . .
C13 C 0.4946(3) 0.8422(2) 0.04017(16) 0.0154(8) Uani 1 1 d . . . . .
H13 H 0.476040 0.830120 -0.000663 0.019 Uiso 1 1 calc R . . . .
C14 C 0.4074(3) 0.8734(2) 0.07214(16) 0.0151(8) Uani 1 1 d . . . . .
C15 C 0.5838(4) 0.8809(2) 0.23017(16) 0.0185(8) Uani 1 1 d . . . . .
C16 C 0.4804(4) 0.8940(2) 0.26985(17) 0.0250(9) Uani 1 1 d . . . . .
H16A H 0.459442 0.944669 0.263529 0.037 Uiso 1 1 calc GR . . . .
H16B H 0.511926 0.895361 0.310631 0.037 Uiso 1 1 calc GR . . . .
H16C H 0.404844 0.850398 0.260305 0.037 Uiso 1 1 calc GR . . . .
C17 C 0.6238(4) 0.8043(2) 0.24861(18) 0.0287(10) Uani 1 1 d . . . . .
H17A H 0.554354 0.757301 0.236962 0.043 Uiso 1 1 calc GR . . . .
H17B H 0.643911 0.809901 0.290823 0.043 Uiso 1 1 calc GR . . . .
H17C H 0.698003 0.798184 0.229488 0.043 Uiso 1 1 calc GR . . . .
C18 C 0.7003(4) 0.9546(2) 0.24452(17) 0.0264(9) Uani 1 1 d . . . . .
H18A H 0.768595 0.946464 0.221757 0.040 Uiso 1 1 calc GR . . . .
H18B H 0.728982 0.960248 0.286004 0.040 Uiso 1 1 calc GR . . . .
H18C H 0.675651 1.002924 0.234738 0.040 Uiso 1 1 calc GR . . . .
C19 C 0.7053(3) 0.7983(2) 0.03026(17) 0.0185(8) Uani 1 1 d . . . . .
C20 C 0.8395(4) 0.8559(3) 0.04678(18) 0.0302(10) Uani 1 1 d . . . . .
H20A H 0.838224 0.909102 0.036272 0.045 Uiso 1 1 calc GR . . . .
H20B H 0.901524 0.835652 0.025710 0.045 Uiso 1 1 calc GR . . . .
H20C H 0.862360 0.858749 0.088664 0.045 Uiso 1 1 calc GR . . . .
C21 C 0.7111(4) 0.7123(2) 0.04442(19) 0.0312(10) Uani 1 1 d . . . . .
H21A H 0.728389 0.712364 0.086440 0.047 Uiso 1 1 calc GR . . . .
H21B H 0.778273 0.696008 0.024702 0.047 Uiso 1 1 calc GR . . . .
H21C H 0.630311 0.674840 0.030928 0.047 Uiso 1 1 calc GR . . . .
C22 C 0.6733(4) 0.7962(2) -0.03642(16) 0.0224(9) Uani 1 1 d . . . . .
H22A H 0.593527 0.757095 -0.048738 0.034 Uiso 1 1 calc GR . . . .
H22B H 0.740557 0.781216 -0.056860 0.034 Uiso 1 1 calc GR . . . .
H22C H 0.665786 0.848951 -0.045627 0.034 Uiso 1 1 calc GR . . . .
C23 C 0.2882(3) 0.8842(2) 0.03330(16) 0.0181(8) Uani 1 1 d . . . . .
C24 C 0.1958(5) 0.8012(3) 0.0176(3) 0.079(2) Uani 1 1 d . . . . .
H24A H 0.237033 0.766105 -0.004947 0.119 Uiso 1 1 calc GR . . . .
H24B H 0.120521 0.806814 -0.005518 0.119 Uiso 1 1 calc GR . . . .
H24C H 0.171594 0.778129 0.053289 0.119 Uiso 1 1 calc GR . . . .
C25 C 0.2125(5) 0.9396(3) 0.0610(2) 0.0526(15) Uani 1 1 d . . . . .
H25A H 0.173726 0.916281 0.094105 0.079 Uiso 1 1 calc GR . . . .
H25B H 0.146561 0.945941 0.032149 0.079 Uiso 1 1 calc GR . . . .
H25C H 0.268987 0.991731 0.074284 0.079 Uiso 1 1 calc GR . . . .
C26 C 0.3268(5) 0.9187(4) -0.0230(2) 0.089(3) Uani 1 1 d . . . . .
H26A H 0.392468 0.968231 -0.013633 0.134 Uiso 1 1 calc GR . . . .
H26B H 0.253391 0.929808 -0.044389 0.134 Uiso 1 1 calc GR . . . .
H26C H 0.359045 0.880269 -0.046982 0.134 Uiso 1 1 calc GR . . . .
B1 B 0.3501(4) 0.9389(2) 0.17233(18) 0.0158(9) Uani 1 1 d . . . . .
I3 I 1.36761(3) 0.65612(2) 0.11387(2) 0.03422(8) Uani 1 1 d . . . . .
I4 I 1.02931(2) 0.07421(2) 0.11759(2) 0.02472(7) Uani 1 1 d . . . . .
O3 O 1.1702(2) 0.51524(14) 0.13692(11) 0.0189(6) Uani 1 1 d . . . . .
O4 O 1.0204(2) 0.24591(13) 0.13328(11) 0.0166(5) Uani 1 1 d . . . . .
C27 C 1.1337(3) 0.4305(2) 0.13456(15) 0.0146(8) Uani 1 1 d . . . . .
C28 C 1.2269(4) 0.4006(2) 0.10997(17) 0.0211(8) Uani 1 1 d . . . . .
H28 H 1.226768 0.346016 0.102688 0.025 Uiso 1 1 calc R . . . .
C29 C 1.3244(4) 0.4672(2) 0.09740(16) 0.0218(9) Uani 1 1 d . . . . .
H29 H 1.399893 0.465008 0.080720 0.026 Uiso 1 1 calc R . . . .
C30 C 1.2852(4) 0.5341(2) 0.11452(17) 0.0209(9) Uani 1 1 d . . . . .
C31 C 0.9544(3) 0.3009(2) 0.15697(15) 0.0146(8) Uani 1 1 d . . . . .
C32 C 0.8516(3) 0.2576(2) 0.18185(16) 0.0191(8) Uani 1 1 d . . . . .
H32 H 0.791228 0.279064 0.200593 0.023 Uiso 1 1 calc R . . . .
C33 C 0.8531(4) 0.1741(2) 0.17410(17) 0.0211(8) Uani 1 1 d . . . . .
H33 H 0.794719 0.130654 0.186407 0.025 Uiso 1 1 calc R . . . .
C34 C 0.9563(3) 0.1711(2) 0.14534(16) 0.0182(8) Uani 1 1 d . . . . .
C35 C 0.9212(3) 0.44387(19) 0.19258(16) 0.0144(8) Uani 1 1 d . . . . .
C36 C 0.9424(3) 0.4638(2) 0.25541(16) 0.0150(8) Uani 1 1 d . . . . .
C37 C 0.8515(3) 0.4947(2) 0.28456(16) 0.0173(8) Uani 1 1 d . . . . .
H37 H 0.866739 0.507910 0.325400 0.021 Uiso 1 1 calc R . . . .
C38 C 0.7397(3) 0.5066(2) 0.25595(16) 0.0159(8) Uani 1 1 d . . . . .
C39 C 0.7224(3) 0.4894(2) 0.19557(16) 0.0167(8) Uani 1 1 d . . . . .
H39 H 0.649243 0.498296 0.175439 0.020 Uiso 1 1 calc R . . . .
C40 C 0.8094(3) 0.45908(19) 0.16220(15) 0.0147(8) Uani 1 1 d . . . . .
C42 C 1.0668(4) 0.4592(2) 0.29342(16) 0.0192(8) Uani 1 1 d . . . . .
C43 C 1.1148(4) 0.3837(3) 0.2787(2) 0.0363(11) Uani 1 1 d . . . . .
H43A H 1.046615 0.336313 0.280058 0.054 Uiso 1 1 calc GR . . . .
H43B H 1.185407 0.383118 0.307006 0.054 Uiso 1 1 calc GR . . . .
H43C H 1.142941 0.383944 0.239657 0.054 Uiso 1 1 calc GR . . . .
C44 C 1.1745(4) 0.5355(2) 0.2860(2) 0.0343(11) Uani 1 1 d . . . . .
H44A H 1.192685 0.534717 0.245388 0.051 Uiso 1 1 calc GR . . . .
H44B H 1.250754 0.535140 0.310765 0.051 Uiso 1 1 calc GR . . . .
H44C H 1.146459 0.583630 0.297432 0.051 Uiso 1 1 calc GR . . . .
C45 C 1.0479(4) 0.4624(3) 0.35940(18) 0.0354(11) Uani 1 1 d . . . . .
H45A H 1.035429 0.514691 0.373028 0.053 Uiso 1 1 calc GR . . . .
H45B H 1.122493 0.453590 0.381227 0.053 Uiso 1 1 calc GR . . . .
H45C H 0.973806 0.420903 0.365372 0.053 Uiso 1 1 calc GR . . . .
C46 C 0.6439(4) 0.5390(2) 0.29194(17) 0.0216(9) Uani 1 1 d . . . . .
C47 C 0.7136(4) 0.6188(2) 0.3295(2) 0.0342(11) Uani 1 1 d . . . . .
H47A H 0.778902 0.608682 0.356954 0.051 Uiso 1 1 calc GR . . . .
H47B H 0.652923 0.639846 0.351003 0.051 Uiso 1 1 calc GR . . . .
H47C H 0.752388 0.657623 0.304048 0.051 Uiso 1 1 calc GR . . . .
C48 C 0.5865(4) 0.4775(2) 0.33295(19) 0.0322(10) Uani 1 1 d . . . . .
H48A H 0.539902 0.428105 0.309822 0.048 Uiso 1 1 calc GR . . . .
H48B H 0.529209 0.499000 0.356423 0.048 Uiso 1 1 calc GR . . . .
H48C H 0.654172 0.466539 0.358550 0.048 Uiso 1 1 calc GR . . . .
C49 C 0.5351(4) 0.5567(3) 0.25258(19) 0.0371(11) Uani 1 1 d . . . . .
H49A H 0.570324 0.592725 0.224583 0.056 Uiso 1 1 calc GR . . . .
H49B H 0.482415 0.581670 0.276599 0.056 Uiso 1 1 calc GR . . . .
H49C H 0.483921 0.506780 0.231693 0.056 Uiso 1 1 calc GR . . . .
C50 C 0.7702(3) 0.4418(2) 0.09460(16) 0.0187(8) Uani 1 1 d . . . . .
C51 C 0.7296(4) 0.5153(2) 0.07105(17) 0.0273(9) Uani 1 1 d . . . . .
H51A H 0.656444 0.524252 0.089876 0.041 Uiso 1 1 calc GR . . . .
H51B H 0.707512 0.504646 0.028963 0.041 Uiso 1 1 calc GR . . . .
H51C H 0.799407 0.562794 0.079661 0.041 Uiso 1 1 calc GR . . . .
C52 C 0.6550(4) 0.3672(2) 0.08290(17) 0.0245(9) Uani 1 1 d . . . . .
H52A H 0.680898 0.320219 0.094769 0.037 Uiso 1 1 calc GR . . . .
H52B H 0.625666 0.358415 0.041410 0.037 Uiso 1 1 calc GR . . . .
H52C H 0.586744 0.376609 0.105238 0.037 Uiso 1 1 calc GR . . . .
C53 C 0.8754(4) 0.4262(2) 0.05691(16) 0.0242(9) Uani 1 1 d . . . . .
H53A H 0.949511 0.471177 0.064766 0.036 Uiso 1 1 calc GR . . . .
H53B H 0.844341 0.420275 0.015696 0.036 Uiso 1 1 calc GR . . . .
H53C H 0.898499 0.377378 0.066608 0.036 Uiso 1 1 calc GR . . . .
B2 B 1.0054(4) 0.3930(2) 0.15879(17) 0.0156(9) Uani 1 1 d . . . . .
I5 I 0.31468(3) 0.02199(2) 0.54793(2) 0.03211(8) Uani 1 1 d . . . . .
I6 I 0.65803(3) 0.59586(2) 0.53339(2) 0.03102(8) Uani 1 1 d . . . . .
O5 O 0.5242(2) 0.15834(14) 0.52693(11) 0.0179(6) Uani 1 1 d . . . . .
O6 O 0.6736(2) 0.42465(14) 0.52433(11) 0.0173(5) Uani 1 1 d . . . . .
C54 C 0.5744(3) 0.2425(2) 0.53680(16) 0.0163(8) Uani 1 1 d . . . . .
C55 C 0.4954(3) 0.2746(2) 0.57009(16) 0.0190(8) Uani 1 1 d . . . . .
H55 H 0.506575 0.329228 0.583336 0.023 Uiso 1 1 calc R . . . .
C56 C 0.3925(4) 0.2101(2) 0.58118(16) 0.0216(9) Uani 1 1 d . . . . .
H56 H 0.323738 0.214037 0.602675 0.026 Uiso 1 1 calc R . . . .
C57 C 0.4149(3) 0.1424(2) 0.55436(17) 0.0200(8) Uani 1 1 d . . . . .
C58 C 0.7416(3) 0.3693(2) 0.50234(16) 0.0158(8) Uani 1 1 d . . . . .
C59 C 0.8407(4) 0.4115(2) 0.47485(17) 0.0203(8) Uani 1 1 d . . . . .
H59 H 0.901494 0.389726 0.456620 0.024 Uiso 1 1 calc R . . . .
C60 C 0.8350(4) 0.4946(2) 0.47892(17) 0.0232(9) Uani 1 1 d . . . . .
H60 H 0.890239 0.537068 0.463909 0.028 Uiso 1 1 calc R . . . .
C61 C 0.7333(4) 0.4990(2) 0.50896(17) 0.0205(8) Uani 1 1 d . . . . .
C62 C 0.7753(3) 0.2235(2) 0.47288(16) 0.0154(8) Uani 1 1 d . . . . .
C63 C 0.8806(3) 0.2005(2) 0.50389(16) 0.0149(8) Uani 1 1 d . . . . .
C64 C 0.9627(3) 0.1664(2) 0.47158(16) 0.0187(8) Uani 1 1 d . . . . .
H64 H 1.030591 0.151906 0.492164 0.022 Uiso 1 1 calc R . . . .
C65 C 0.9488(3) 0.1527(2) 0.41002(17) 0.0174(8) Uani 1 1 d . . . . .
C66 C 0.8429(3) 0.1704(2) 0.38125(16) 0.0168(8) Uani 1 1 d . . . . .
H66 H 0.829172 0.159395 0.340211 0.020 Uiso 1 1 calc R . . . .
C67 C 0.7543(3) 0.2045(2) 0.41099(16) 0.0151(8) Uani 1 1 d . . . . .
C68 C 0.9061(4) 0.2107(2) 0.57282(16) 0.0193(8) Uani 1 1 d . . . . .
C69 C 1.0385(4) 0.1981(2) 0.59378(17) 0.0248(9) Uani 1 1 d . . . . .
H69A H 1.042845 0.143933 0.580280 0.037 Uiso 1 1 calc GR . . . .
H69B H 1.051254 0.206091 0.636294 0.037 Uiso 1 1 calc GR . . . .
H69C H 1.104205 0.236547 0.577876 0.037 Uiso 1 1 calc GR . . . .
C70 C 0.9033(4) 0.2953(2) 0.60082(17) 0.0243(9) Uani 1 1 d . . . . .
H70A H 0.962677 0.335823 0.583355 0.037 Uiso 1 1 calc GR . . . .
H70B H 0.927346 0.299804 0.642708 0.037 Uiso 1 1 calc GR . . . .
H70C H 0.818190 0.303275 0.593952 0.037 Uiso 1 1 calc GR . . . .
C71 C 0.8045(4) 0.1465(2) 0.59862(17) 0.0250(9) Uani 1 1 d . . . . .
H71A H 0.721255 0.156913 0.590674 0.037 Uiso 1 1 calc GR . . . .
H71B H 0.825121 0.149331 0.640667 0.037 Uiso 1 1 calc GR . . . .
H71C H 0.803978 0.093306 0.580567 0.037 Uiso 1 1 calc GR . . . .
C72 C 1.0478(4) 0.1196(2) 0.37678(17) 0.0206(8) Uani 1 1 d . . . . .
C73 C 1.0367(4) 0.0309(2) 0.3880(2) 0.0330(11) Uani 1 1 d . . . . .
H73A H 1.050251 0.027654 0.429773 0.050 Uiso 1 1 calc GR . . . .
H73B H 1.100256 0.010579 0.368174 0.050 Uiso 1 1 calc GR . . . .
H73C H 0.952563 -0.001062 0.372944 0.050 Uiso 1 1 calc GR . . . .
C74 C 1.1834(4) 0.1697(3) 0.3967(2) 0.0366(11) Uani 1 1 d . . . . .
H74A H 1.189962 0.225063 0.389279 0.055 Uiso 1 1 calc GR . . . .
H74B H 1.243490 0.148168 0.375180 0.055 Uiso 1 1 calc GR . . . .
H74C H 1.202316 0.167436 0.438394 0.055 Uiso 1 1 calc GR . . . .
C75 C 1.0253(4) 0.1211(2) 0.30920(18) 0.0278(10) Uani 1 1 d . . . . .
H75A H 0.944242 0.084830 0.294393 0.042 Uiso 1 1 calc GR . . . .
H75B H 1.093000 0.104153 0.290405 0.042 Uiso 1 1 calc GR . . . .
H75C H 1.024602 0.175270 0.300729 0.042 Uiso 1 1 calc GR . . . .
C76 C 0.6413(4) 0.2167(2) 0.36900(16) 0.0187(8) Uani 1 1 d . . . . .
C77 C 0.5706(4) 0.1338(2) 0.33616(19) 0.0363(11) Uani 1 1 d . . . . .
H77A H 0.629257 0.111641 0.314064 0.054 Uiso 1 1 calc GR . . . .
H77B H 0.500986 0.140391 0.309522 0.054 Uiso 1 1 calc GR . . . .
H77C H 0.537219 0.097543 0.364358 0.054 Uiso 1 1 calc GR . . . .
C78 C 0.6951(4) 0.2754(3) 0.32430(18) 0.0311(10) Uani 1 1 d . . . . .
H78A H 0.738399 0.327228 0.345129 0.047 Uiso 1 1 calc GR . . . .
H78B H 0.625779 0.281868 0.297426 0.047 Uiso 1 1 calc GR . . . .
H78C H 0.754586 0.253766 0.302415 0.047 Uiso 1 1 calc GR . . . .
C79 C 0.5380(4) 0.2506(2) 0.39816(17) 0.0255(9) Uani 1 1 d . . . . .
H79A H 0.498184 0.213846 0.424783 0.038 Uiso 1 1 calc GR . . . .
H79B H 0.474191 0.256551 0.368113 0.038 Uiso 1 1 calc GR . . . .
H79C H 0.576979 0.302590 0.419840 0.038 Uiso 1 1 calc GR . . . .
B3 B 0.6957(4) 0.2775(2) 0.50637(17) 0.0150(9) 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
I1 0.03537(18) 0.02093(14) 0.04247(19) 0.00838(12) 0.00264(13) -0.00881(12)
I2 0.02607(15) 0.01522(13) 0.03194(16) -0.00145(10) -0.00324(11) 0.00775(10)
O1 0.0207(14) 0.0126(12) 0.0230(15) 0.0026(11) 0.0052(11) 0.0009(11)
O2 0.0130(13) 0.0125(12) 0.0218(14) -0.0012(10) 0.0013(11) 0.0017(10)
C1 0.023(2) 0.0092(17) 0.019(2) -0.0004(14) 0.0011(16) 0.0024(15)
C2 0.023(2) 0.0189(19) 0.022(2) 0.0021(16) 0.0051(17) 0.0065(16)
C3 0.019(2) 0.028(2) 0.026(2) 0.0070(17) 0.0105(17) 0.0066(17)
C4 0.018(2) 0.020(2) 0.026(2) 0.0100(17) 0.0052(17) -0.0010(16)
C5 0.018(2) 0.0137(18) 0.0153(19) 0.0005(14) 0.0008(15) 0.0058(15)
C6 0.019(2) 0.0176(19) 0.023(2) -0.0006(16) 0.0007(16) 0.0037(16)
C7 0.017(2) 0.0180(19) 0.023(2) 0.0054(16) 0.0006(16) 0.0002(15)
C8 0.019(2) 0.0126(18) 0.019(2) 0.0005(15) -0.0053(16) 0.0008(15)
C9 0.0140(19) 0.0122(17) 0.019(2) 0.0027(14) 0.0021(15) 0.0005(14)
C10 0.021(2) 0.0135(18) 0.017(2) 0.0020(15) 0.0010(16) 0.0020(15)
C11 0.0150(19) 0.0143(18) 0.024(2) 0.0015(15) 0.0007(16) 0.0041(15)
C12 0.016(2) 0.0090(17) 0.022(2) 0.0023(14) 0.0019(16) 0.0009(14)
C13 0.017(2) 0.0124(17) 0.0161(19) 0.0009(14) 0.0017(15) 0.0021(14)
C14 0.0163(19) 0.0096(17) 0.018(2) 0.0014(14) 0.0011(15) 0.0000(14)
C15 0.019(2) 0.0186(19) 0.018(2) 0.0023(15) 0.0016(16) 0.0045(16)
C16 0.026(2) 0.033(2) 0.018(2) 0.0043(17) 0.0030(17) 0.0093(18)
C17 0.038(3) 0.028(2) 0.024(2) 0.0056(18) 0.0006(19) 0.0153(19)
C18 0.028(2) 0.022(2) 0.025(2) -0.0065(17) -0.0036(18) 0.0015(17)
C19 0.018(2) 0.0160(19) 0.023(2) 0.0032(15) 0.0040(16) 0.0059(15)
C20 0.017(2) 0.042(3) 0.029(2) -0.001(2) 0.0038(18) 0.0056(19)
C21 0.040(3) 0.026(2) 0.036(3) 0.0103(19) 0.017(2) 0.020(2)
C22 0.022(2) 0.021(2) 0.024(2) -0.0016(16) 0.0062(17) 0.0042(16)
C23 0.017(2) 0.023(2) 0.015(2) -0.0011(15) 0.0002(15) 0.0087(16)
C24 0.049(4) 0.029(3) 0.145(6) -0.020(3) -0.064(4) 0.014(3)
C25 0.061(4) 0.075(4) 0.032(3) -0.021(3) -0.021(2) 0.055(3)
C26 0.037(3) 0.203(8) 0.060(4) 0.088(5) 0.024(3) 0.060(4)
B1 0.016(2) 0.017(2) 0.012(2) 0.0027(16) -0.0011(17) 0.0012(17)
I3 0.03725(18) 0.02144(14) 0.03585(18) 0.00977(12) -0.00062(13) -0.01015(12)
I4 0.02400(15) 0.01344(13) 0.03608(17) -0.00155(11) -0.00219(11) 0.00646(10)
O3 0.0211(14) 0.0132(13) 0.0223(15) 0.0022(10) 0.0055(11) 0.0025(11)
O4 0.0164(13) 0.0111(12) 0.0213(14) 0.0003(10) 0.0032(11) 0.0012(10)
C27 0.019(2) 0.0098(17) 0.0143(19) -0.0005(14) 0.0009(15) 0.0031(14)
C28 0.022(2) 0.0186(19) 0.024(2) 0.0008(16) 0.0048(17) 0.0064(16)
C29 0.016(2) 0.029(2) 0.021(2) 0.0065(17) 0.0072(16) 0.0044(17)
C30 0.019(2) 0.0166(19) 0.022(2) 0.0076(16) -0.0001(16) -0.0057(16)
C31 0.0154(19) 0.0146(18) 0.0157(19) 0.0005(14) 0.0014(15) 0.0075(15)
C32 0.019(2) 0.0190(19) 0.018(2) 0.0022(15) 0.0040(16) 0.0015(16)
C33 0.022(2) 0.0146(19) 0.026(2) 0.0061(16) 0.0033(17) 0.0015(16)
C34 0.019(2) 0.0121(18) 0.021(2) 0.0007(15) -0.0074(16) 0.0020(15)
C35 0.0145(19) 0.0091(17) 0.019(2) 0.0016(14) 0.0041(15) 0.0004(14)
C36 0.0151(19) 0.0123(17) 0.017(2) 0.0026(14) 0.0020(15) 0.0011(14)
C37 0.021(2) 0.0171(18) 0.0137(19) -0.0007(15) 0.0034(15) 0.0045(15)
C38 0.0135(19) 0.0117(17) 0.022(2) 0.0030(15) 0.0039(15) 0.0007(14)
C39 0.0140(19) 0.0130(18) 0.023(2) 0.0025(15) 0.0002(15) 0.0043(14)
C40 0.0163(19) 0.0098(17) 0.016(2) 0.0023(14) -0.0007(15) 0.0004(14)
C42 0.019(2) 0.0180(19) 0.019(2) -0.0009(15) 0.0002(16) 0.0043(16)
C43 0.042(3) 0.038(3) 0.034(3) -0.003(2) -0.009(2) 0.024(2)
C44 0.026(2) 0.034(2) 0.040(3) 0.001(2) -0.001(2) 0.0032(19)
C45 0.031(3) 0.054(3) 0.023(2) 0.002(2) -0.0026(19) 0.017(2)
C46 0.018(2) 0.021(2) 0.027(2) -0.0004(16) 0.0057(17) 0.0074(16)
C47 0.028(2) 0.028(2) 0.045(3) -0.007(2) 0.012(2) 0.0067(19)
C48 0.033(3) 0.033(2) 0.034(3) 0.0062(19) 0.014(2) 0.011(2)
C49 0.030(3) 0.050(3) 0.037(3) 0.001(2) 0.007(2) 0.020(2)
C50 0.019(2) 0.0182(19) 0.018(2) 0.0005(15) -0.0020(16) 0.0053(16)
C51 0.036(3) 0.025(2) 0.024(2) 0.0057(17) -0.0027(18) 0.0123(18)
C52 0.025(2) 0.022(2) 0.021(2) 0.0002(16) -0.0030(17) -0.0014(17)
C53 0.028(2) 0.025(2) 0.017(2) -0.0003(16) 0.0004(17) 0.0025(17)
B2 0.020(2) 0.017(2) 0.009(2) 0.0014(16) -0.0021(17) 0.0049(17)
I5 0.03065(17) 0.02151(14) 0.03825(18) 0.00640(12) 0.00392(13) -0.00677(11)
I6 0.02937(16) 0.01518(13) 0.04774(19) -0.00025(12) -0.00588(13) 0.00826(11)
O5 0.0182(14) 0.0123(12) 0.0225(15) 0.0028(10) 0.0056(11) 0.0008(10)
O6 0.0141(13) 0.0127(12) 0.0259(15) 0.0026(10) 0.0027(11) 0.0046(10)
C54 0.020(2) 0.0124(17) 0.0161(19) 0.0021(14) 0.0020(15) 0.0033(15)
C55 0.021(2) 0.0170(19) 0.021(2) 0.0062(15) 0.0059(16) 0.0059(16)
C56 0.018(2) 0.032(2) 0.018(2) 0.0064(17) 0.0075(16) 0.0080(17)
C57 0.017(2) 0.021(2) 0.021(2) 0.0085(16) 0.0022(16) 0.0007(16)
C58 0.017(2) 0.0137(18) 0.017(2) -0.0010(14) -0.0017(15) 0.0060(15)
C59 0.018(2) 0.020(2) 0.023(2) 0.0052(16) 0.0022(16) 0.0030(16)
C60 0.023(2) 0.0182(19) 0.025(2) 0.0054(16) -0.0024(17) -0.0024(16)
C61 0.024(2) 0.0119(18) 0.024(2) 0.0052(15) -0.0058(17) 0.0022(15)
C62 0.0146(19) 0.0100(17) 0.020(2) 0.0020(14) 0.0022(15) -0.0007(14)
C63 0.0150(19) 0.0104(17) 0.017(2) 0.0001(14) -0.0007(15) 0.0002(14)
C64 0.018(2) 0.0132(18) 0.025(2) 0.0031(15) 0.0009(16) 0.0026(15)
C65 0.018(2) 0.0097(17) 0.025(2) 0.0007(15) 0.0052(16) 0.0021(14)
C66 0.020(2) 0.0132(18) 0.016(2) -0.0012(14) 0.0039(15) 0.0006(15)
C67 0.0155(19) 0.0131(18) 0.017(2) 0.0007(14) 0.0004(15) 0.0038(15)
C68 0.021(2) 0.0192(19) 0.018(2) 0.0049(15) -0.0014(16) 0.0068(16)
C69 0.023(2) 0.027(2) 0.023(2) -0.0001(17) -0.0013(17) 0.0061(17)
C70 0.030(2) 0.024(2) 0.020(2) -0.0016(16) -0.0005(17) 0.0102(18)
C71 0.028(2) 0.024(2) 0.023(2) 0.0075(17) 0.0018(18) 0.0063(17)
C72 0.019(2) 0.0150(19) 0.028(2) -0.0012(16) 0.0051(17) 0.0063(16)
C73 0.039(3) 0.026(2) 0.044(3) 0.008(2) 0.018(2) 0.021(2)
C74 0.020(2) 0.040(3) 0.045(3) -0.009(2) 0.009(2) 0.0006(19)
C75 0.029(2) 0.025(2) 0.033(3) 0.0031(18) 0.0108(19) 0.0116(18)
C76 0.022(2) 0.0196(19) 0.015(2) 0.0024(15) 0.0016(16) 0.0060(16)
C77 0.041(3) 0.031(2) 0.034(3) -0.006(2) -0.016(2) 0.011(2)
C78 0.029(2) 0.041(3) 0.032(3) 0.016(2) 0.0104(19) 0.017(2)
C79 0.018(2) 0.041(2) 0.019(2) 0.0004(18) -0.0024(16) 0.0119(18)
B3 0.020(2) 0.017(2) 0.008(2) 0.0018(16) -0.0037(16) 0.0049(17)
_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
I1 C4 2.068(4) . ?
I2 C8 2.061(4) . ?
O1 C1 1.407(4) . ?
O1 C4 1.357(4) . ?
O2 C5 1.402(4) . ?
O2 C8 1.358(4) . ?
C1 C2 1.358(5) . ?
C1 B1 1.536(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.416(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.339(5) . ?
C5 C6 1.361(5) . ?
C5 B1 1.541(5) . ?
C6 H6 0.9300 . ?
C6 C7 1.418(5) . ?
C7 H7 0.9300 . ?
C7 C8 1.343(5) . ?
C9 C10 1.421(5) . ?
C9 C14 1.426(5) . ?
C9 B1 1.595(5) . ?
C10 C11 1.399(5) . ?
C10 C15 1.549(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.388(5) . ?
C12 C13 1.387(5) . ?
C12 C19 1.535(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.402(5) . ?
C14 C23 1.557(5) . ?
C15 C16 1.530(5) . ?
C15 C17 1.546(5) . ?
C15 C18 1.543(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.541(5) . ?
C19 C21 1.540(5) . ?
C19 C22 1.526(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.522(5) . ?
C23 C25 1.512(5) . ?
C23 C26 1.502(6) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
I3 C30 2.061(3) . ?
I4 C34 2.059(4) . ?
O3 C27 1.398(4) . ?
O3 C30 1.354(4) . ?
O4 C31 1.398(4) . ?
O4 C34 1.360(4) . ?
C27 C28 1.362(5) . ?
C27 B2 1.542(5) . ?
C28 H28 0.9300 . ?
C28 C29 1.418(5) . ?
C29 H29 0.9300 . ?
C29 C30 1.341(5) . ?
C31 C32 1.368(5) . ?
C31 B2 1.531(5) . ?
C32 H32 0.9300 . ?
C32 C33 1.421(5) . ?
C33 H33 0.9300 . ?
C33 C34 1.340(5) . ?
C35 C36 1.429(5) . ?
C35 C40 1.428(5) . ?
C35 B2 1.588(5) . ?
C36 C37 1.397(5) . ?
C36 C42 1.559(5) . ?
C37 H37 0.9300 . ?
C37 C38 1.390(5) . ?
C38 C39 1.369(5) . ?
C38 C46 1.535(5) . ?
C39 H39 0.9300 . ?
C39 C40 1.410(5) . ?
C40 C50 1.548(5) . ?
C42 C43 1.514(5) . ?
C42 C44 1.555(5) . ?
C42 C45 1.529(5) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 C47 1.536(5) . ?
C46 C48 1.517(5) . ?
C46 C49 1.521(5) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 C51 1.543(5) . ?
C50 C52 1.540(5) . ?
C50 C53 1.529(5) . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
I5 C57 2.067(4) . ?
I6 C61 2.054(4) . ?
O5 C54 1.400(4) . ?
O5 C57 1.355(4) . ?
O6 C58 1.403(4) . ?
O6 C61 1.367(4) . ?
C54 C55 1.356(5) . ?
C54 B3 1.543(5) . ?
C55 H55 0.9300 . ?
C55 C56 1.419(5) . ?
C56 H56 0.9300 . ?
C56 C57 1.338(5) . ?
C58 C59 1.365(5) . ?
C58 B3 1.538(5) . ?
C59 H59 0.9300 . ?
C59 C60 1.426(5) . ?
C60 H60 0.9300 . ?
C60 C61 1.347(5) . ?
C62 C63 1.437(5) . ?
C62 C67 1.406(5) . ?
C62 B3 1.584(5) . ?
C63 C64 1.388(5) . ?
C63 C68 1.559(5) . ?
C64 H64 0.9300 . ?
C64 C65 1.391(5) . ?
C65 C66 1.378(5) . ?
C65 C72 1.535(5) . ?
C66 H66 0.9300 . ?
C66 C67 1.412(5) . ?
C67 C76 1.552(5) . ?
C68 C69 1.535(5) . ?
C68 C70 1.532(5) . ?
C68 C71 1.544(5) . ?
C69 H69A 0.9600 . ?
C69 H69B 0.9600 . ?
C69 H69C 0.9600 . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C71 H71A 0.9600 . ?
C71 H71B 0.9600 . ?
C71 H71C 0.9600 . ?
C72 C73 1.531(5) . ?
C72 C74 1.519(5) . ?
C72 C75 1.542(5) . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?
C75 H75A 0.9600 . ?
C75 H75B 0.9600 . ?
C75 H75C 0.9600 . ?
C76 C77 1.536(5) . ?
C76 C78 1.537(5) . ?
C76 C79 1.534(5) . ?
C77 H77A 0.9600 . ?
C77 H77B 0.9600 . ?
C77 H77C 0.9600 . ?
C78 H78A 0.9600 . ?
C78 H78B 0.9600 . ?
C78 H78C 0.9600 . ?
C79 H79A 0.9600 . ?
C79 H79B 0.9600 . ?
C79 H79C 0.9600 . ?
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
C4 O1 C1 106.2(3) . . ?
C8 O2 C5 106.6(3) . . ?
O1 C1 B1 117.0(3) . . ?
C2 C1 O1 107.5(3) . . ?
C2 C1 B1 135.5(3) . . ?
C1 C2 H2 125.6 . . ?
C1 C2 C3 108.7(3) . . ?
C3 C2 H2 125.6 . . ?
C2 C3 H3 127.2 . . ?
C4 C3 C2 105.6(3) . . ?
C4 C3 H3 127.2 . . ?
O1 C4 I1 116.3(3) . . ?
C3 C4 I1 131.7(3) . . ?
C3 C4 O1 112.1(3) . . ?
O2 C5 B1 121.5(3) . . ?
C6 C5 O2 107.5(3) . . ?
C6 C5 B1 130.6(3) . . ?
C5 C6 H6 125.7 . . ?
C5 C6 C7 108.6(3) . . ?
C7 C6 H6 125.7 . . ?
C6 C7 H7 127.2 . . ?
C8 C7 C6 105.7(3) . . ?
C8 C7 H7 127.2 . . ?
O2 C8 I2 117.3(2) . . ?
C7 C8 I2 131.1(3) . . ?
C7 C8 O2 111.6(3) . . ?
C10 C9 C14 118.0(3) . . ?
C10 C9 B1 120.4(3) . . ?
C14 C9 B1 121.0(3) . . ?
C9 C10 C15 125.9(3) . . ?
C11 C10 C9 119.5(3) . . ?
C11 C10 C15 114.6(3) . . ?
C10 C11 H11 118.4 . . ?
C12 C11 C10 123.2(3) . . ?
C12 C11 H11 118.4 . . ?
C11 C12 C19 120.6(3) . . ?
C13 C12 C11 116.6(3) . . ?
C13 C12 C19 122.8(3) . . ?
C12 C13 H13 118.3 . . ?
C12 C13 C14 123.4(3) . . ?
C14 C13 H13 118.3 . . ?
C9 C14 C23 126.7(3) . . ?
C13 C14 C9 119.0(3) . . ?
C13 C14 C23 114.2(3) . . ?
C16 C15 C10 115.4(3) . . ?
C16 C15 C17 106.1(3) . . ?
C16 C15 C18 107.7(3) . . ?
C17 C15 C10 110.0(3) . . ?
C18 C15 C10 108.8(3) . . ?
C18 C15 C17 108.7(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C19 C20 109.5(3) . . ?
C12 C19 C21 110.0(3) . . ?
C21 C19 C20 108.7(3) . . ?
C22 C19 C12 112.5(3) . . ?
C22 C19 C20 107.4(3) . . ?
C22 C19 C21 108.7(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C14 108.3(3) . . ?
C25 C23 C14 116.4(3) . . ?
C25 C23 C24 106.9(4) . . ?
C26 C23 C14 110.9(3) . . ?
C26 C23 C24 108.8(4) . . ?
C26 C23 C25 105.3(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C1 B1 C5 120.5(3) . . ?
C1 B1 C9 125.3(3) . . ?
C5 B1 C9 114.0(3) . . ?
C30 O3 C27 106.8(3) . . ?
C34 O4 C31 106.4(3) . . ?
O3 C27 B2 117.2(3) . . ?
C28 C27 O3 107.6(3) . . ?
C28 C27 B2 135.2(3) . . ?
C27 C28 H28 125.9 . . ?
C27 C28 C29 108.2(3) . . ?
C29 C28 H28 125.9 . . ?
C28 C29 H29 127.1 . . ?
C30 C29 C28 105.9(3) . . ?
C30 C29 H29 127.1 . . ?
O3 C30 I3 116.2(3) . . ?
C29 C30 I3 132.3(3) . . ?
C29 C30 O3 111.6(3) . . ?
O4 C31 B2 122.3(3) . . ?
C32 C31 O4 107.8(3) . . ?
C32 C31 B2 129.5(3) . . ?
C31 C32 H32 125.9 . . ?
C31 C32 C33 108.2(3) . . ?
C33 C32 H32 125.9 . . ?
C32 C33 H33 127.2 . . ?
C34 C33 C32 105.5(3) . . ?
C34 C33 H33 127.2 . . ?
O4 C34 I4 117.1(2) . . ?
C33 C34 I4 130.9(3) . . ?
C33 C34 O4 112.1(3) . . ?
C36 C35 C40 118.1(3) . . ?
C36 C35 B2 121.0(3) . . ?
C40 C35 B2 120.1(3) . . ?
C35 C36 C42 123.7(3) . . ?
C37 C36 C35 118.9(3) . . ?
C37 C36 C42 117.2(3) . . ?
C36 C37 H37 118.2 . . ?
C38 C37 C36 123.7(3) . . ?
C38 C37 H37 118.2 . . ?
C37 C38 C46 120.0(3) . . ?
C39 C38 C37 116.7(3) . . ?
C39 C38 C46 123.3(3) . . ?
C38 C39 H39 118.2 . . ?
C38 C39 C40 123.7(3) . . ?
C40 C39 H39 118.2 . . ?
C35 C40 C50 125.7(3) . . ?
C39 C40 C35 118.8(3) . . ?
C39 C40 C50 115.4(3) . . ?
C43 C42 C36 115.3(3) . . ?
C43 C42 C44 109.0(3) . . ?
C43 C42 C45 106.1(3) . . ?
C44 C42 C36 108.2(3) . . ?
C45 C42 C36 111.3(3) . . ?
C45 C42 C44 106.5(3) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C38 C46 C47 109.6(3) . . ?
C48 C46 C38 109.9(3) . . ?
C48 C46 C47 108.8(3) . . ?
C48 C46 C49 108.6(3) . . ?
C49 C46 C38 112.3(3) . . ?
C49 C46 C47 107.5(3) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C49 H49A 109.5 . . ?
C46 C49 H49B 109.5 . . ?
C46 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 C40 110.0(3) . . ?
C52 C50 C40 108.7(3) . . ?
C52 C50 C51 108.7(3) . . ?
C53 C50 C40 115.6(3) . . ?
C53 C50 C51 105.5(3) . . ?
C53 C50 C52 108.2(3) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C27 B2 C35 124.5(3) . . ?
C31 B2 C27 121.6(3) . . ?
C31 B2 C35 113.7(3) . . ?
C57 O5 C54 106.3(3) . . ?
C61 O6 C58 106.8(3) . . ?
O5 C54 B3 116.7(3) . . ?
C55 C54 O5 108.0(3) . . ?
C55 C54 B3 135.2(3) . . ?
C54 C55 H55 126.0 . . ?
C54 C55 C56 108.0(3) . . ?
C56 C55 H55 126.0 . . ?
C55 C56 H56 127.1 . . ?
C57 C56 C55 105.9(3) . . ?
C57 C56 H56 127.1 . . ?
O5 C57 I5 116.4(2) . . ?
C56 C57 I5 131.9(3) . . ?
C56 C57 O5 111.7(3) . . ?
O6 C58 B3 121.9(3) . . ?
C59 C58 O6 107.8(3) . . ?
C59 C58 B3 130.1(3) . . ?
C58 C59 H59 125.9 . . ?
C58 C59 C60 108.2(3) . . ?
C60 C59 H59 125.9 . . ?
C59 C60 H60 127.0 . . ?
C61 C60 C59 106.0(3) . . ?
C61 C60 H60 127.0 . . ?
O6 C61 I6 117.7(3) . . ?
C60 C61 I6 131.0(3) . . ?
C60 C61 O6 111.3(3) . . ?
C63 C62 B3 120.8(3) . . ?
C67 C62 C63 118.1(3) . . ?
C67 C62 B3 120.8(3) . . ?
C62 C63 C68 123.0(3) . . ?
C64 C63 C62 119.1(3) . . ?
C64 C63 C68 117.8(3) . . ?
C63 C64 H64 118.3 . . ?
C63 C64 C65 123.4(4) . . ?
C65 C64 H64 118.3 . . ?
C64 C65 C72 120.8(3) . . ?
C66 C65 C64 116.6(3) . . ?
C66 C65 C72 122.6(3) . . ?
C65 C66 H66 118.4 . . ?
C65 C66 C67 123.3(3) . . ?
C67 C66 H66 118.4 . . ?
C62 C67 C66 119.2(3) . . ?
C62 C67 C76 127.3(3) . . ?
C66 C67 C76 113.5(3) . . ?
C69 C68 C63 112.1(3) . . ?
C69 C68 C71 107.2(3) . . ?
C70 C68 C63 113.0(3) . . ?
C70 C68 C69 105.9(3) . . ?
C70 C68 C71 108.8(3) . . ?
C71 C68 C63 109.6(3) . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
C68 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C68 C70 H70A 109.5 . . ?
C68 C70 H70B 109.5 . . ?
C68 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C68 C71 H71A 109.5 . . ?
C68 C71 H71B 109.5 . . ?
C68 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C65 C72 C75 112.1(3) . . ?
C73 C72 C65 109.3(3) . . ?
C73 C72 C75 107.2(3) . . ?
C74 C72 C65 110.9(3) . . ?
C74 C72 C73 109.9(3) . . ?
C74 C72 C75 107.3(3) . . ?
C72 C73 H73A 109.5 . . ?
C72 C73 H73B 109.5 . . ?
C72 C73 H73C 109.5 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C72 C74 H74A 109.5 . . ?
C72 C74 H74B 109.5 . . ?
C72 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C72 C75 H75A 109.5 . . ?
C72 C75 H75B 109.5 . . ?
C72 C75 H75C 109.5 . . ?
H75A C75 H75B 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C77 C76 C67 108.4(3) . . ?
C77 C76 C78 110.0(3) . . ?
C78 C76 C67 109.1(3) . . ?
C79 C76 C67 116.7(3) . . ?
C79 C76 C77 105.7(3) . . ?
C79 C76 C78 106.8(3) . . ?
C76 C77 H77A 109.5 . . ?
C76 C77 H77B 109.5 . . ?
C76 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C76 C78 H78A 109.5 . . ?
C76 C78 H78B 109.5 . . ?
C76 C78 H78C 109.5 . . ?
H78A C78 H78B 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C76 C79 H79A 109.5 . . ?
C76 C79 H79B 109.5 . . ?
C76 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C54 B3 C62 123.9(3) . . ?
C58 B3 C54 121.1(3) . . ?
C58 B3 C62 114.8(3) . . ?
_shelx_res_file
;
TITL m18_a13sad_a.res in P-1
m18_a13sad.res
created by SHELXL-2018/1 at 09:08:07 on 24-Apr-2018
REM Old TITL m18_a13sad_a.res in P-1
REM SHELXT solution in P-1
REM R1 0.140, Rweak 0.005, Alpha 0.049, Orientation as input
REM Formula found by SHELXT: C81 I6 O6
CELL 0.71073 10.7568 17.0259 22.7583 94.956 94.394 103.556
ZERR 8 0.0012 0.0018 0.0024 0.002 0.002 0.002
LATT 1
SFAC C H B I O
UNIT 156 198 6 12 12
L.S. 50
PLAN 20
TEMP 0
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.045000 0.200000
FVAR 0.14309
I1 4 -0.034335 0.677060 0.200252 11.00000 0.03537 0.02093 =
0.04247 0.00838 0.00264 -0.00881
I2 4 0.323938 1.255401 0.227224 11.00000 0.02607 0.01522 =
0.03194 -0.00145 -0.00324 0.00775
O1 5 0.175976 0.816571 0.185634 11.00000 0.02075 0.01259 =
0.02296 0.00262 0.00521 0.00089
O2 5 0.335100 1.084641 0.203804 11.00000 0.01296 0.01250 =
0.02180 -0.00116 0.00132 0.00174
C1 1 0.223263 0.901348 0.197176 11.00000 0.02305 0.00924 =
0.01888 -0.00043 0.00111 0.00237
C2 1 0.137090 0.930432 0.227807 11.00000 0.02292 0.01889 =
0.02247 0.00209 0.00511 0.00653
AFIX 43
H2 2 0.144398 0.984675 0.241122 11.00000 -1.20000
AFIX 0
C3 1 0.034303 0.864521 0.236116 11.00000 0.01914 0.02758 =
0.02625 0.00702 0.01048 0.00659
AFIX 43
H3 2 -0.037749 0.866736 0.255717 11.00000 -1.20000
AFIX 0
C4 1 0.062598 0.798347 0.209837 11.00000 0.01785 0.02043 =
0.02623 0.00997 0.00524 -0.00096
C5 1 0.402649 1.031781 0.177919 11.00000 0.01785 0.01369 =
0.01529 0.00050 0.00077 0.00577
C6 1 0.506049 1.078080 0.155862 11.00000 0.01913 0.01757 =
0.02286 -0.00056 0.00069 0.00367
AFIX 43
H6 2 0.567225 1.058584 0.136220 11.00000 -1.20000
AFIX 0
C7 1 0.504852 1.160999 0.167852 11.00000 0.01656 0.01798 =
0.02314 0.00544 0.00056 0.00020
AFIX 43
H7 2 0.564326 1.205906 0.158099 11.00000 -1.20000
AFIX 0
C8 1 0.399921 1.161182 0.196232 11.00000 0.01874 0.01257 =
0.01906 0.00052 -0.00529 0.00081
C9 1 0.432085 0.889532 0.135008 11.00000 0.01395 0.01221 =
0.01874 0.00270 0.00208 0.00055
C10 1 0.542522 0.870190 0.162669 11.00000 0.02094 0.01346 =
0.01717 0.00198 0.00098 0.00198
C11 1 0.627407 0.841796 0.127610 11.00000 0.01499 0.01435 =
0.02420 0.00154 0.00065 0.00410
AFIX 43
H11 2 0.700960 0.831490 0.146346 11.00000 -1.20000
AFIX 0
C12 1 0.607254 0.828247 0.066239 11.00000 0.01601 0.00898 =
0.02243 0.00233 0.00191 0.00090
C13 1 0.494629 0.842151 0.040169 11.00000 0.01696 0.01245 =
0.01613 0.00095 0.00174 0.00215
AFIX 43
H13 2 0.476040 0.830120 -0.000663 11.00000 -1.20000
AFIX 0
C14 1 0.407350 0.873390 0.072144 11.00000 0.01633 0.00959 =
0.01784 0.00142 0.00110 -0.00001
C15 1 0.583782 0.880858 0.230167 11.00000 0.01920 0.01862 =
0.01774 0.00233 0.00160 0.00454
C16 1 0.480372 0.894050 0.269852 11.00000 0.02564 0.03330 =
0.01750 0.00433 0.00304 0.00930
AFIX 137
H16A 2 0.459442 0.944669 0.263529 11.00000 -1.50000
H16B 2 0.511926 0.895361 0.310631 11.00000 -1.50000
H16C 2 0.404844 0.850398 0.260305 11.00000 -1.50000
AFIX 0
C17 1 0.623805 0.804307 0.248607 11.00000 0.03788 0.02796 =
0.02407 0.00562 0.00058 0.01533
AFIX 137
H17A 2 0.554354 0.757301 0.236962 11.00000 -1.50000
H17B 2 0.643911 0.809901 0.290823 11.00000 -1.50000
H17C 2 0.698003 0.798184 0.229488 11.00000 -1.50000
AFIX 0
C18 1 0.700257 0.954590 0.244523 11.00000 0.02785 0.02192 =
0.02468 -0.00647 -0.00357 0.00154
AFIX 137
H18A 2 0.768595 0.946464 0.221757 11.00000 -1.50000
H18B 2 0.728982 0.960248 0.286004 11.00000 -1.50000
H18C 2 0.675651 1.002924 0.234738 11.00000 -1.50000
AFIX 0
C19 1 0.705344 0.798256 0.030257 11.00000 0.01763 0.01597 =
0.02342 0.00318 0.00402 0.00586
C20 1 0.839516 0.855873 0.046784 11.00000 0.01740 0.04219 =
0.02947 -0.00149 0.00381 0.00556
AFIX 137
H20A 2 0.838224 0.909102 0.036272 11.00000 -1.50000
H20B 2 0.901524 0.835652 0.025710 11.00000 -1.50000
H20C 2 0.862360 0.858749 0.088664 11.00000 -1.50000
AFIX 0
C21 1 0.711124 0.712269 0.044415 11.00000 0.04036 0.02624 =
0.03649 0.01031 0.01743 0.02048
AFIX 137
H21A 2 0.728389 0.712364 0.086440 11.00000 -1.50000
H21B 2 0.778273 0.696008 0.024702 11.00000 -1.50000
H21C 2 0.630311 0.674840 0.030928 11.00000 -1.50000
AFIX 0
C22 1 0.673337 0.796188 -0.036423 11.00000 0.02223 0.02076 =
0.02357 -0.00160 0.00617 0.00421
AFIX 137
H22A 2 0.593527 0.757095 -0.048738 11.00000 -1.50000
H22B 2 0.740557 0.781216 -0.056860 11.00000 -1.50000
H22C 2 0.665786 0.848951 -0.045627 11.00000 -1.50000
AFIX 0
C23 1 0.288184 0.884233 0.033298 11.00000 0.01750 0.02268 =
0.01530 -0.00105 0.00020 0.00871
C24 1 0.195809 0.801154 0.017580 11.00000 0.04912 0.02918 =
0.14465 -0.02008 -0.06363 0.01433
AFIX 137
H24A 2 0.237033 0.766105 -0.004947 11.00000 -1.50000
H24B 2 0.120521 0.806814 -0.005518 11.00000 -1.50000
H24C 2 0.171594 0.778129 0.053289 11.00000 -1.50000
AFIX 0
C25 1 0.212455 0.939598 0.060985 11.00000 0.06123 0.07476 =
0.03211 -0.02085 -0.02087 0.05476
AFIX 137
H25A 2 0.173726 0.916281 0.094105 11.00000 -1.50000
H25B 2 0.146561 0.945941 0.032149 11.00000 -1.50000
H25C 2 0.268987 0.991731 0.074284 11.00000 -1.50000
AFIX 0
C26 1 0.326752 0.918750 -0.023008 11.00000 0.03698 0.20299 =
0.06026 0.08824 0.02422 0.06020
AFIX 137
H26A 2 0.392468 0.968231 -0.013633 11.00000 -1.50000
H26B 2 0.253391 0.929808 -0.044389 11.00000 -1.50000
H26C 2 0.359045 0.880269 -0.046982 11.00000 -1.50000
AFIX 0
B1 3 0.350070 0.938856 0.172330 11.00000 0.01619 0.01718 =
0.01245 0.00267 -0.00107 0.00119
I3 4 1.367607 0.656123 0.113872 11.00000 0.03725 0.02144 =
0.03585 0.00977 -0.00062 -0.01015
I4 4 1.029312 0.074209 0.117594 11.00000 0.02400 0.01344 =
0.03608 -0.00155 -0.00219 0.00646
O3 5 1.170185 0.515236 0.136916 11.00000 0.02107 0.01316 =
0.02227 0.00223 0.00547 0.00250
O4 5 1.020358 0.245907 0.133284 11.00000 0.01640 0.01111 =
0.02127 0.00033 0.00322 0.00117
C27 1 1.133680 0.430517 0.134562 11.00000 0.01896 0.00984 =
0.01426 -0.00050 0.00088 0.00311
C28 1 1.226942 0.400639 0.109974 11.00000 0.02171 0.01864 =
0.02392 0.00084 0.00478 0.00639
AFIX 43
H28 2 1.226768 0.346016 0.102688 11.00000 -1.20000
AFIX 0
C29 1 1.324365 0.467237 0.097404 11.00000 0.01628 0.02902 =
0.02098 0.00649 0.00722 0.00437
AFIX 43
H29 2 1.399893 0.465008 0.080720 11.00000 -1.20000
AFIX 0
C30 1 1.285202 0.534085 0.114520 11.00000 0.01950 0.01660 =
0.02228 0.00756 -0.00007 -0.00573
C31 1 0.954386 0.300900 0.156972 11.00000 0.01537 0.01461 =
0.01569 0.00053 0.00140 0.00752
C32 1 0.851630 0.257578 0.181847 11.00000 0.01871 0.01902 =
0.01833 0.00221 0.00398 0.00151
AFIX 43
H32 2 0.791228 0.279064 0.200593 11.00000 -1.20000
AFIX 0
C33 1 0.853113 0.174089 0.174099 11.00000 0.02228 0.01461 =
0.02579 0.00609 0.00333 0.00147
AFIX 43
H33 2 0.794719 0.130654 0.186407 11.00000 -1.20000
AFIX 0
C34 1 0.956319 0.171091 0.145335 11.00000 0.01912 0.01205 =
0.02070 0.00071 -0.00741 0.00196
C35 1 0.921192 0.443873 0.192577 11.00000 0.01451 0.00911 =
0.01866 0.00163 0.00413 0.00036
C36 1 0.942411 0.463833 0.255409 11.00000 0.01513 0.01231 =
0.01676 0.00256 0.00204 0.00110
C37 1 0.851534 0.494651 0.284556 11.00000 0.02073 0.01712 =
0.01369 -0.00069 0.00339 0.00447
AFIX 43
H37 2 0.866739 0.507910 0.325400 11.00000 -1.20000
AFIX 0
C38 1 0.739672 0.506614 0.255950 11.00000 0.01352 0.01167 =
0.02178 0.00303 0.00389 0.00070
C39 1 0.722440 0.489436 0.195568 11.00000 0.01405 0.01295 =
0.02348 0.00254 0.00023 0.00433
AFIX 43
H39 2 0.649243 0.498296 0.175439 11.00000 -1.20000
AFIX 0
C40 1 0.809404 0.459075 0.162195 11.00000 0.01631 0.00980 =
0.01645 0.00230 -0.00072 0.00041
C42 1 1.066829 0.459184 0.293422 11.00000 0.01946 0.01795 =
0.01926 -0.00089 0.00024 0.00429
C43 1 1.114840 0.383737 0.278688 11.00000 0.04168 0.03751 =
0.03389 -0.00318 -0.00920 0.02446
AFIX 137
H43A 2 1.046615 0.336313 0.280058 11.00000 -1.50000
H43B 2 1.185407 0.383118 0.307006 11.00000 -1.50000
H43C 2 1.142941 0.383944 0.239657 11.00000 -1.50000
AFIX 0
C44 1 1.174481 0.535465 0.286046 11.00000 0.02587 0.03408 =
0.03966 0.00108 -0.00101 0.00318
AFIX 137
H44A 2 1.192685 0.534717 0.245388 11.00000 -1.50000
H44B 2 1.250754 0.535140 0.310765 11.00000 -1.50000
H44C 2 1.146459 0.583630 0.297432 11.00000 -1.50000
AFIX 0
C45 1 1.047876 0.462390 0.359399 11.00000 0.03147 0.05390 =
0.02301 0.00249 -0.00265 0.01730
AFIX 137
H45A 2 1.035429 0.514691 0.373028 11.00000 -1.50000
H45B 2 1.122493 0.453590 0.381227 11.00000 -1.50000
H45C 2 0.973806 0.420903 0.365372 11.00000 -1.50000
AFIX 0
C46 1 0.643860 0.539023 0.291942 11.00000 0.01843 0.02084 =
0.02686 -0.00038 0.00570 0.00737
C47 1 0.713556 0.618774 0.329511 11.00000 0.02828 0.02842 =
0.04523 -0.00666 0.01183 0.00668
AFIX 137
H47A 2 0.778902 0.608682 0.356954 11.00000 -1.50000
H47B 2 0.652923 0.639846 0.351003 11.00000 -1.50000
H47C 2 0.752388 0.657623 0.304048 11.00000 -1.50000
AFIX 0
C48 1 0.586520 0.477519 0.332950 11.00000 0.03314 0.03329 =
0.03407 0.00616 0.01380 0.01144
AFIX 137
H48A 2 0.539902 0.428105 0.309822 11.00000 -1.50000
H48B 2 0.529209 0.499000 0.356423 11.00000 -1.50000
H48C 2 0.654172 0.466539 0.358550 11.00000 -1.50000
AFIX 0
C49 1 0.535106 0.556677 0.252576 11.00000 0.03010 0.05005 =
0.03655 0.00142 0.00690 0.02050
AFIX 137
H49A 2 0.570324 0.592725 0.224583 11.00000 -1.50000
H49B 2 0.482415 0.581670 0.276599 11.00000 -1.50000
H49C 2 0.483921 0.506780 0.231693 11.00000 -1.50000
AFIX 0
C50 1 0.770230 0.441825 0.094598 11.00000 0.01929 0.01820 =
0.01808 0.00050 -0.00200 0.00526
C51 1 0.729556 0.515322 0.071050 11.00000 0.03557 0.02475 =
0.02366 0.00574 -0.00270 0.01230
AFIX 137
H51A 2 0.656444 0.524252 0.089876 11.00000 -1.50000
H51B 2 0.707512 0.504646 0.028963 11.00000 -1.50000
H51C 2 0.799407 0.562794 0.079661 11.00000 -1.50000
AFIX 0
C52 1 0.655036 0.367243 0.082902 11.00000 0.02504 0.02231 =
0.02141 0.00018 -0.00299 -0.00137
AFIX 137
H52A 2 0.680898 0.320219 0.094769 11.00000 -1.50000
H52B 2 0.625666 0.358415 0.041410 11.00000 -1.50000
H52C 2 0.586744 0.376609 0.105238 11.00000 -1.50000
AFIX 0
C53 1 0.875430 0.426212 0.056912 11.00000 0.02827 0.02492 =
0.01679 -0.00029 0.00037 0.00248
AFIX 137
H53A 2 0.949511 0.471177 0.064766 11.00000 -1.50000
H53B 2 0.844341 0.420275 0.015696 11.00000 -1.50000
H53C 2 0.898499 0.377378 0.066608 11.00000 -1.50000
AFIX 0
B2 3 1.005442 0.393012 0.158792 11.00000 0.02012 0.01719 =
0.00916 0.00137 -0.00209 0.00493
I5 4 0.314680 0.021989 0.547932 11.00000 0.03065 0.02151 =
0.03825 0.00640 0.00392 -0.00677
I6 4 0.658029 0.595856 0.533393 11.00000 0.02937 0.01518 =
0.04774 -0.00025 -0.00588 0.00826
O5 5 0.524155 0.158337 0.526935 11.00000 0.01820 0.01225 =
0.02251 0.00281 0.00557 0.00079
O6 5 0.673604 0.424648 0.524327 11.00000 0.01412 0.01269 =
0.02587 0.00260 0.00275 0.00457
C54 1 0.574383 0.242548 0.536800 11.00000 0.02000 0.01244 =
0.01611 0.00206 0.00200 0.00328
C55 1 0.495364 0.274567 0.570089 11.00000 0.02095 0.01701 =
0.02094 0.00617 0.00587 0.00586
AFIX 43
H55 2 0.506575 0.329228 0.583336 11.00000 -1.20000
AFIX 0
C56 1 0.392543 0.210067 0.581179 11.00000 0.01774 0.03162 =
0.01808 0.00639 0.00751 0.00802
AFIX 43
H56 2 0.323738 0.214037 0.602675 11.00000 -1.20000
AFIX 0
C57 1 0.414938 0.142378 0.554355 11.00000 0.01714 0.02077 =
0.02119 0.00855 0.00219 0.00072
C58 1 0.741624 0.369350 0.502343 11.00000 0.01703 0.01371 =
0.01681 -0.00105 -0.00168 0.00601
C59 1 0.840735 0.411474 0.474853 11.00000 0.01762 0.02025 =
0.02287 0.00522 0.00220 0.00296
AFIX 43
H59 2 0.901494 0.389726 0.456620 11.00000 -1.20000
AFIX 0
C60 1 0.835012 0.494600 0.478923 11.00000 0.02291 0.01820 =
0.02458 0.00542 -0.00236 -0.00239
AFIX 43
H60 2 0.890239 0.537068 0.463909 11.00000 -1.20000
AFIX 0
C61 1 0.733272 0.499037 0.508956 11.00000 0.02367 0.01186 =
0.02427 0.00524 -0.00577 0.00224
C62 1 0.775276 0.223475 0.472877 11.00000 0.01460 0.00997 =
0.01982 0.00204 0.00216 -0.00074
C63 1 0.880578 0.200546 0.503887 11.00000 0.01501 0.01035 =
0.01734 0.00014 -0.00067 0.00021
C64 1 0.962735 0.166389 0.471584 11.00000 0.01787 0.01318 =
0.02458 0.00306 0.00086 0.00262
AFIX 43
H64 2 1.030591 0.151906 0.492164 11.00000 -1.20000
AFIX 0
C65 1 0.948833 0.152695 0.410018 11.00000 0.01752 0.00971 =
0.02467 0.00066 0.00516 0.00213
C66 1 0.842947 0.170416 0.381249 11.00000 0.01963 0.01316 =
0.01565 -0.00117 0.00394 0.00056
AFIX 43
H66 2 0.829172 0.159395 0.340211 11.00000 -1.20000
AFIX 0
C67 1 0.754268 0.204493 0.410988 11.00000 0.01546 0.01310 =
0.01654 0.00068 0.00036 0.00384
C68 1 0.906125 0.210662 0.572819 11.00000 0.02136 0.01922 =
0.01826 0.00486 -0.00140 0.00681
C69 1 1.038507 0.198135 0.593781 11.00000 0.02342 0.02694 =
0.02303 -0.00010 -0.00133 0.00609
AFIX 137
H69A 2 1.042845 0.143933 0.580280 11.00000 -1.50000
H69B 2 1.051254 0.206091 0.636294 11.00000 -1.50000
H69C 2 1.104205 0.236547 0.577876 11.00000 -1.50000
AFIX 0
C70 1 0.903323 0.295293 0.600823 11.00000 0.03048 0.02361 =
0.01957 -0.00164 -0.00053 0.01017
AFIX 137
H70A 2 0.962677 0.335823 0.583355 11.00000 -1.50000
H70B 2 0.927346 0.299804 0.642708 11.00000 -1.50000
H70C 2 0.818190 0.303275 0.593952 11.00000 -1.50000
AFIX 0
C71 1 0.804516 0.146488 0.598620 11.00000 0.02831 0.02400 =
0.02343 0.00745 0.00176 0.00635
AFIX 137
H71A 2 0.721255 0.156913 0.590674 11.00000 -1.50000
H71B 2 0.825121 0.149331 0.640667 11.00000 -1.50000
H71C 2 0.803978 0.093306 0.580567 11.00000 -1.50000
AFIX 0
C72 1 1.047824 0.119562 0.376781 11.00000 0.01938 0.01499 =
0.02816 -0.00121 0.00507 0.00629
C73 1 1.036685 0.030921 0.387960 11.00000 0.03937 0.02566 =
0.04355 0.00818 0.01785 0.02089
AFIX 137
H73A 2 1.050251 0.027654 0.429773 11.00000 -1.50000
H73B 2 1.100256 0.010579 0.368174 11.00000 -1.50000
H73C 2 0.952563 -0.001062 0.372944 11.00000 -1.50000
AFIX 0
C74 1 1.183375 0.169669 0.396746 11.00000 0.01965 0.04039 =
0.04480 -0.00922 0.00863 0.00056
AFIX 137
H74A 2 1.189962 0.225063 0.389279 11.00000 -1.50000
H74B 2 1.243490 0.148168 0.375180 11.00000 -1.50000
H74C 2 1.202316 0.167436 0.438394 11.00000 -1.50000
AFIX 0
C75 1 1.025291 0.121099 0.309200 11.00000 0.02940 0.02495 =
0.03273 0.00307 0.01076 0.01161
AFIX 137
H75A 2 0.944242 0.084830 0.294393 11.00000 -1.50000
H75B 2 1.093000 0.104153 0.290405 11.00000 -1.50000
H75C 2 1.024602 0.175270 0.300729 11.00000 -1.50000
AFIX 0
C76 1 0.641258 0.216744 0.369003 11.00000 0.02219 0.01956 =
0.01481 0.00237 0.00157 0.00602
C77 1 0.570554 0.133808 0.336159 11.00000 0.04076 0.03057 =
0.03377 -0.00630 -0.01641 0.01097
AFIX 137
H77A 2 0.629257 0.111641 0.314064 11.00000 -1.50000
H77B 2 0.500986 0.140391 0.309522 11.00000 -1.50000
H77C 2 0.537219 0.097543 0.364358 11.00000 -1.50000
AFIX 0
C78 1 0.695055 0.275408 0.324297 11.00000 0.02854 0.04088 =
0.03169 0.01583 0.01041 0.01735
AFIX 137
H78A 2 0.738399 0.327228 0.345129 11.00000 -1.50000
H78B 2 0.625779 0.281868 0.297426 11.00000 -1.50000
H78C 2 0.754586 0.253766 0.302415 11.00000 -1.50000
AFIX 0
C79 1 0.537991 0.250601 0.398163 11.00000 0.01809 0.04057 =
0.01895 0.00036 -0.00240 0.01188
AFIX 137
H79A 2 0.498184 0.213846 0.424783 11.00000 -1.50000
H79B 2 0.474191 0.256551 0.368113 11.00000 -1.50000
H79C 2 0.576979 0.302590 0.419840 11.00000 -1.50000
AFIX 0
B3 3 0.695679 0.277534 0.506368 11.00000 0.01969 0.01668 =
0.00805 0.00181 -0.00367 0.00487
HKLF 4
REM m18_a13sad_a.res in P-1
REM R1 = 0.0351 for 12055 Fo > 4sig(Fo) and 0.0482 for all 15014 data
REM 865 parameters refined using 0 restraints
END
WGHT 0.0450 0.2762
REM Highest difference peak 1.579, deepest hole -0.719, 1-sigma level 0.118
Q1 1 0.6246 0.5855 0.5717 11.00000 0.05 1.58
Q2 1 1.3535 0.6522 0.1470 11.00000 0.05 1.28
Q3 1 0.3631 1.2705 0.1956 11.00000 0.05 1.23
Q4 1 0.0440 0.6646 0.2086 11.00000 0.05 1.11
Q5 1 -0.0632 0.6696 0.2314 11.00000 0.05 0.93
Q6 1 0.3716 0.0134 0.5213 11.00000 0.05 0.91
Q7 1 0.2779 0.0038 0.5408 11.00000 0.05 0.89
Q8 1 0.2732 0.0147 0.5800 11.00000 0.05 0.83
Q9 1 0.9529 0.0816 0.1305 11.00000 0.05 0.81
Q10 1 1.1749 0.4296 0.2631 11.00000 0.05 0.80
Q11 1 1.1299 0.5214 0.3383 11.00000 0.05 0.79
Q12 1 0.0120 0.6769 0.1720 11.00000 0.05 0.73
Q13 1 1.0247 0.0690 0.1587 11.00000 0.05 0.73
Q14 1 0.9984 0.0599 0.1512 11.00000 0.05 0.71
Q15 1 0.5958 0.5753 0.4954 11.00000 0.05 0.70
Q16 1 1.0133 0.3776 0.3308 11.00000 0.05 0.68
Q17 1 0.2742 0.0027 0.5020 11.00000 0.05 0.67
Q18 1 0.3764 0.0285 0.5703 11.00000 0.05 0.65
Q19 1 1.2876 0.6483 0.1006 11.00000 0.05 0.63
Q20 1 0.2229 0.0148 0.5130 11.00000 0.05 0.63
;
_shelx_res_checksum 12635
_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_m18_a15sad
_database_code_depnum_ccdc_archive 'CCDC 1843527'
_audit_update_record
;
2018-05-16 deposited with the CCDC.
2018-05-18 downloaded from the CCDC.
;
_audit_creation_date 2018-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2018/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C34.01 H39.01 B O2 S1.99'
_chemical_formula_sum 'C34 H39 B O2 S2'
_chemical_formula_weight 554.58
_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'
B B 0.0013 0.0007 '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'
S S 0.1246 0.1234 '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 9.299(3)
_cell_length_b 13.239(5)
_cell_length_c 13.676(5)
_cell_angle_alpha 97.674(8)
_cell_angle_beta 101.180(7)
_cell_angle_gamma 107.537(7)
_cell_volume 1541.5(10)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 1672
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 21.82
_cell_measurement_theta_min 2.37
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.201
_exptl_absorpt_correction_T_max 0.7453
_exptl_absorpt_correction_T_min 0.5432
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1697 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.7288.
The \l/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.195
_exptl_crystal_density_meas .
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 592
_exptl_crystal_size_max 0.27
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0794
_diffrn_reflns_av_unetI/netI 0.0959
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 18294
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.117
_diffrn_reflns_theta_min 2.018
_diffrn_ambient_temperature 100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Bruker APEX CCD'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator 'multilayer optics'
_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 3415
_reflns_number_total 6097
_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 0.306
_refine_diff_density_min -0.401
_refine_diff_density_rms 0.060
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.009
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 431
_refine_ls_number_reflns 6097
_refine_ls_number_restraints 8
_refine_ls_R_factor_all 0.1247
_refine_ls_R_factor_gt 0.0661
_refine_ls_restrained_S_all 1.011
_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^)+(0.0880P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1544
_refine_ls_wR_factor_ref 0.1833
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
C31-C32B = C34-C32B
1.4 with sigma of 0.02
S2A-C34 = S2A-C31
1.6 with sigma of 0.02
C32A-C33 = C32A-C31
1.4 with sigma of 0.02
S2B-C31 = S2B-C33
1.6 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
Sof(H3B)=Sof(O1A)=Sof(C4A)=Sof(C30A)=Sof(H30A)=Sof(C27A)=Sof(C28A)=Sof(H28A)=
Sof(C29A)=Sof(H29A)=1-FVAR(1)
Sof(H3A)=Sof(O1B)=Sof(C4B)=Sof(C27B)=Sof(C28B)=Sof(H28B)=Sof(C29B)=Sof(H29B)=
Sof(C30B)=Sof(H30B)=FVAR(1)
Sof(H34A)=Sof(C32B)=Sof(H32B)=1-FVAR(2)
Sof(H34)=Sof(S2A)=FVAR(2)
Sof(H33A)=Sof(S2B)=1-FVAR(3)
Sof(H33)=Sof(C32A)=Sof(H32A)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
C11(H11), C2(H2), C3(H3A), C3(H3B), C6(H6), C7(H7), C13(H13), C34(H34),
C34(H34A), C33(H33), C33(H33A), C28B(H28B), C29B(H29B), C30B(H30B), C32B(H32B),
C30A(H30A), C28A(H28A), C29A(H29A), C32A(H32A)
5.b Idealised Me refined as rotating group:
C21(H21A,H21B,H21C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,
H22C), C24(H24A,H24B,H24C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C), C17(H17A,
H17B,H17C), C26(H26A,H26B,H26C)
;
_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
S1 S 0.94304(11) 0.92659(8) 0.71045(7) 0.0515(3) Uani 1 1 d . . . . .
O2 O 0.2157(2) 0.48732(16) 0.33360(15) 0.0308(5) Uani 1 1 d . . . . .
C8 C 0.0814(3) 0.4092(2) 0.2768(2) 0.0320(7) Uani 1 1 d . . . . .
C1 C 0.5252(4) 0.6714(2) 0.4195(2) 0.0302(7) Uani 1 1 d . . . . .
C10 C 0.4759(3) 0.7762(2) 0.1892(2) 0.0287(7) Uani 1 1 d . . . . .
C11 C 0.5358(3) 0.8204(2) 0.1125(2) 0.0297(7) Uani 1 1 d . . . . .
H11 H 0.503519 0.875231 0.090215 0.036 Uiso 1 1 calc R . . . .
C5 C 0.2927(4) 0.5377(2) 0.2656(2) 0.0304(7) Uani 1 1 d . . . . .
C19 C 0.7009(4) 0.8427(2) -0.0164(2) 0.0304(7) Uani 1 1 d . . . . .
C14 C 0.6288(3) 0.6547(2) 0.1771(2) 0.0265(7) Uani 1 1 d . . . . .
C2 C 0.5033(4) 0.6396(3) 0.5084(2) 0.0344(8) Uani 1 1 d . . . . .
H2 H 0.426265 0.577857 0.513111 0.041 Uiso 1 1 calc R . . . .
C15 C 0.3622(4) 0.8273(3) 0.2278(2) 0.0367(8) Uani 1 1 d . . . . .
C3 C 0.6145(4) 0.7145(3) 0.5908(2) 0.0375(8) Uani 1 1 d . . . . .
H3A H 0.630448 0.709442 0.658977 0.045 Uiso 0.826(5) 1 calc R . P A 1
H3B H 0.609783 0.721134 0.658555 0.045 Uiso 0.174(5) 1 calc R . P A 2
C6 C 0.2034(4) 0.4894(3) 0.1703(2) 0.0363(8) Uani 1 1 d . . . . .
H6 H 0.226744 0.507494 0.110425 0.044 Uiso 1 1 calc R . . . .
C31 C -0.0215(4) 0.3502(3) 0.3337(3) 0.0377(8) Uani 1 1 d D . . . .
C7 C 0.0686(4) 0.4068(3) 0.1764(3) 0.0384(8) Uani 1 1 d . . . . .
H7 H -0.011793 0.360743 0.122542 0.046 Uiso 1 1 calc R . . . .
C21 C 0.5622(4) 0.8241(3) -0.1063(2) 0.0464(9) Uani 1 1 d . . . . .
H21A H 0.493386 0.858985 -0.084899 0.070 Uiso 1 1 calc GR . . . .
H21B H 0.507234 0.747879 -0.129521 0.070 Uiso 1 1 calc GR . . . .
H21C H 0.598934 0.853882 -0.160676 0.070 Uiso 1 1 calc GR . . . .
C18 C 0.3092(4) 0.7940(3) 0.3212(3) 0.0412(9) Uani 1 1 d . . . . .
H18A H 0.256684 0.717198 0.307025 0.062 Uiso 1 1 calc GR . . . .
H18B H 0.239339 0.830584 0.337438 0.062 Uiso 1 1 calc GR . . . .
H18C H 0.398105 0.813375 0.377926 0.062 Uiso 1 1 calc GR . . . .
C20 C 0.7812(5) 0.9634(3) 0.0232(3) 0.0518(10) Uani 1 1 d . . . . .
H20A H 0.813207 0.996685 -0.030772 0.078 Uiso 1 1 calc GR . . . .
H20B H 0.870741 0.975896 0.077826 0.078 Uiso 1 1 calc GR . . . .
H20C H 0.710322 0.994089 0.047733 0.078 Uiso 1 1 calc GR . . . .
C22 C 0.8132(4) 0.7946(3) -0.0562(3) 0.0505(10) Uani 1 1 d . . . . .
H22A H 0.761829 0.718521 -0.083062 0.076 Uiso 1 1 calc GR . . . .
H22B H 0.902093 0.805534 -0.001606 0.076 Uiso 1 1 calc GR . . . .
H22C H 0.846462 0.829553 -0.109063 0.076 Uiso 1 1 calc GR . . . .
C24 C 0.8622(5) 0.6252(3) 0.2743(3) 0.0686(13) Uani 1 1 d . . . . .
H24A H 0.923038 0.671237 0.237906 0.103 Uiso 1 1 calc GR . . . .
H24B H 0.909652 0.572822 0.292069 0.103 Uiso 1 1 calc GR . . . .
H24C H 0.857223 0.668072 0.335088 0.103 Uiso 1 1 calc GR . . . .
C16 C 0.2141(5) 0.7987(4) 0.1415(3) 0.0645(12) Uani 1 1 d . . . . .
H16A H 0.241565 0.823667 0.082720 0.097 Uiso 1 1 calc GR . . . .
H16B H 0.145038 0.832880 0.163558 0.097 Uiso 1 1 calc GR . . . .
H16C H 0.163170 0.721624 0.124516 0.097 Uiso 1 1 calc GR . . . .
C25 C 0.7064(5) 0.4941(3) 0.1136(3) 0.0580(11) Uani 1 1 d . . . . .
H25A H 0.605487 0.464132 0.066915 0.087 Uiso 1 1 calc GR . . . .
H25B H 0.739881 0.436552 0.134042 0.087 Uiso 1 1 calc GR . . . .
H25C H 0.779331 0.535831 0.080927 0.087 Uiso 1 1 calc GR . . . .
C23 C 0.6979(3) 0.5668(2) 0.2070(2) 0.0275(7) Uani 1 1 d . . . . .
C12 C 0.6402(3) 0.7882(2) 0.0672(2) 0.0258(7) Uani 1 1 d . . . . .
C9 C 0.5210(3) 0.6895(2) 0.2229(2) 0.0269(7) Uani 1 1 d . . . . .
C13 C 0.6847(3) 0.7057(2) 0.1025(2) 0.0280(7) Uani 1 1 d . . . . .
H13 H 0.756324 0.683115 0.074693 0.034 Uiso 1 1 calc R . . . .
C17 C 0.4411(5) 0.9515(3) 0.2585(3) 0.0637(12) Uani 1 1 d . . . . .
H17A H 0.535552 0.968928 0.310537 0.096 Uiso 1 1 calc GR . . . .
H17B H 0.372048 0.983261 0.284042 0.096 Uiso 1 1 calc GR . . . .
H17C H 0.464862 0.979529 0.200168 0.096 Uiso 1 1 calc GR . . . .
C34 C -0.2403(5) 0.2337(3) 0.3815(4) 0.0629(12) Uani 1 1 d D . . . .
H34 H -0.334689 0.184405 0.383428 0.075 Uiso 0.712(8) 1 calc R . P B 1
H34A H -0.338965 0.184923 0.375570 0.075 Uiso 0.288(8) 1 calc R . P B 2
C26 C 0.6107(5) 0.4898(3) 0.2658(3) 0.0677(14) Uani 1 1 d . . . . .
H26A H 0.611593 0.530041 0.329933 0.102 Uiso 1 1 calc GR . . . .
H26B H 0.660451 0.437169 0.277634 0.102 Uiso 1 1 calc GR . . . .
H26C H 0.505104 0.453751 0.227060 0.102 Uiso 1 1 calc GR . . . .
C33 C -0.1345(5) 0.2929(4) 0.4650(4) 0.0812(16) Uani 1 1 d D . . . .
H33 H -0.140928 0.285470 0.530834 0.097 Uiso 0.719(8) 1 calc R . P B 1
H33A H -0.154217 0.289191 0.528776 0.097 Uiso 0.281(8) 1 calc R . P B 2
B1 B 0.4476(4) 0.6321(3) 0.3053(3) 0.0303(8) Uani 1 1 d . . . . .
S2A S -0.1939(4) 0.2530(2) 0.2747(3) 0.0404(8) Uani 0.712(8) 1 d D . P B 1
O1B O 0.6464(8) 0.7707(8) 0.4479(8) 0.0292(13) Uani 0.826(5) 1 d . . P A 1
C4B C 0.6953(6) 0.7967(4) 0.5507(4) 0.0296(12) Uani 0.826(5) 1 d . . P A 1
C27B C 0.8161(5) 0.9006(4) 0.5938(3) 0.0320(11) Uani 0.826(5) 1 d . . P A 1
C28B C 0.8482(4) 0.9893(3) 0.5504(3) 0.0337(11) Uani 0.826(5) 1 d . . P A 1
H28B H 0.792283 0.992463 0.487345 0.040 Uiso 0.826(5) 1 calc R . P A 1
C29B C 0.9781(5) 1.0765(3) 0.6139(3) 0.0388(11) Uani 0.826(5) 1 d . . P A 1
H29B H 1.016311 1.143176 0.596186 0.047 Uiso 0.826(5) 1 calc R . P A 1
C30B C 1.0397(6) 1.0536(4) 0.7012(4) 0.0402(12) Uani 0.826(5) 1 d . . P A 1
H30B H 1.125109 1.101560 0.750595 0.048 Uiso 0.826(5) 1 calc R . P A 1
O1A O 0.689(4) 0.757(4) 0.446(4) 0.042(9) Uani 0.174(5) 1 d . . P A 2
C32B C -0.166(2) 0.263(2) 0.3025(15) 0.058(15) Uani 0.288(8) 1 d D . P B 2
H32B H -0.208683 0.227379 0.234860 0.070 Uiso 0.288(8) 1 calc R . P B 2
C4A C 0.734(4) 0.778(3) 0.554(2) 0.037(10) Uiso 0.174(5) 1 d . U P A 2
C30A C 1.112(3) 1.0204(19) 0.6919(18) 0.049(7) Uani 0.174(5) 1 d . . P A 2
H30A H 1.171930 1.085906 0.735943 0.059 Uiso 0.174(5) 1 calc R . P A 2
C27A C 0.881(3) 0.8625(19) 0.5957(18) 0.050(7) Uani 0.174(5) 1 d . . P A 2
C28A C 1.004(2) 0.8877(17) 0.5483(15) 0.045(6) Uani 0.174(5) 1 d . . P A 2
H28A H 1.002198 0.848232 0.486127 0.053 Uiso 0.174(5) 1 calc R . P A 2
C29A C 1.137(3) 0.9826(17) 0.6064(18) 0.058(7) Uani 0.174(5) 1 d . . P A 2
H29A H 1.226909 1.011819 0.585121 0.069 Uiso 0.174(5) 1 calc R . P A 2
C32A C -0.0082(19) 0.3702(15) 0.4402(10) 0.083(9) Uani 0.719(8) 1 d D . P B 1
H32A H 0.071336 0.425744 0.487476 0.099 Uiso 0.719(8) 1 calc R . P B 1
S2B S 0.0267(17) 0.3703(8) 0.4545(8) 0.056(2) Uani 0.281(8) 1 d D . P B 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_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0449(6) 0.0532(7) 0.0433(6) 0.0069(5) 0.0064(4) 0.0019(5)
O2 0.0233(11) 0.0277(12) 0.0406(12) 0.0121(10) 0.0131(9) 0.0019(9)
C8 0.0243(17) 0.0255(18) 0.047(2) 0.0103(15) 0.0115(14) 0.0066(14)
C1 0.0322(18) 0.0218(17) 0.0412(18) 0.0124(14) 0.0177(14) 0.0078(14)
C10 0.0246(16) 0.0248(17) 0.0357(17) 0.0069(14) 0.0100(13) 0.0051(13)
C11 0.0261(17) 0.0247(17) 0.0395(18) 0.0123(14) 0.0096(14) 0.0070(14)
C5 0.0329(18) 0.0283(18) 0.0365(18) 0.0119(14) 0.0194(14) 0.0104(15)
C19 0.0303(17) 0.0258(18) 0.0328(17) 0.0104(14) 0.0119(14) 0.0016(14)
C14 0.0236(16) 0.0236(17) 0.0294(16) 0.0061(13) 0.0084(12) 0.0024(13)
C2 0.0350(19) 0.0317(19) 0.0382(18) 0.0144(15) 0.0168(15) 0.0060(15)
C15 0.0370(19) 0.039(2) 0.0443(19) 0.0183(16) 0.0202(16) 0.0175(16)
C3 0.040(2) 0.039(2) 0.0339(18) 0.0161(16) 0.0143(15) 0.0070(16)
C6 0.0343(19) 0.036(2) 0.0392(19) 0.0062(15) 0.0189(15) 0.0077(16)
C31 0.0264(19) 0.0293(19) 0.056(2) 0.0145(17) 0.0114(16) 0.0036(16)
C7 0.0290(18) 0.036(2) 0.044(2) 0.0014(16) 0.0111(15) 0.0046(15)
C21 0.055(2) 0.043(2) 0.039(2) 0.0190(17) 0.0146(17) 0.0085(18)
C18 0.047(2) 0.041(2) 0.051(2) 0.0176(17) 0.0277(17) 0.0232(18)
C20 0.063(3) 0.038(2) 0.047(2) 0.0158(17) 0.0246(19) -0.0040(19)
C22 0.055(2) 0.057(3) 0.055(2) 0.030(2) 0.0338(19) 0.020(2)
C24 0.052(3) 0.040(2) 0.099(3) 0.018(2) -0.016(2) 0.015(2)
C16 0.047(2) 0.107(4) 0.059(3) 0.023(2) 0.020(2) 0.048(3)
C25 0.096(3) 0.039(2) 0.047(2) 0.0094(18) 0.019(2) 0.034(2)
C23 0.0291(17) 0.0236(17) 0.0315(16) 0.0085(13) 0.0127(13) 0.0069(14)
C12 0.0233(16) 0.0219(16) 0.0289(16) 0.0075(13) 0.0070(12) 0.0016(13)
C9 0.0220(16) 0.0231(17) 0.0322(16) 0.0059(13) 0.0088(13) 0.0013(13)
C13 0.0228(16) 0.0284(18) 0.0301(16) 0.0049(14) 0.0088(13) 0.0039(13)
C17 0.083(3) 0.043(2) 0.095(3) 0.029(2) 0.065(3) 0.032(2)
C34 0.033(2) 0.051(3) 0.101(4) 0.028(3) 0.026(2) -0.0013(19)
C26 0.093(3) 0.063(3) 0.099(3) 0.058(3) 0.070(3) 0.054(3)
C33 0.055(3) 0.105(4) 0.068(3) 0.041(3) 0.026(2) -0.012(3)
B1 0.033(2) 0.0237(19) 0.040(2) 0.0119(16) 0.0172(16) 0.0105(16)
S2A 0.0239(10) 0.0346(10) 0.0556(19) 0.0075(10) 0.0092(14) 0.0008(7)
O1B 0.023(3) 0.029(2) 0.031(2) 0.0074(18) 0.014(2) -0.003(2)
C4B 0.024(3) 0.031(3) 0.033(3) 0.006(2) 0.010(2) 0.006(2)
C27B 0.030(2) 0.029(3) 0.039(2) 0.006(2) 0.0151(19) 0.008(2)
C28B 0.031(2) 0.029(2) 0.041(2) 0.0039(18) 0.0177(18) 0.0070(18)
C29B 0.032(2) 0.026(2) 0.054(3) 0.004(2) 0.016(2) 0.0017(18)
C30B 0.034(3) 0.029(3) 0.044(3) -0.004(2) 0.011(2) -0.004(2)
O1A 0.034(19) 0.057(18) 0.034(11) 0.007(10) 0.027(14) 0.005(13)
C32B 0.05(2) 0.08(2) 0.040(15) -0.005(10) -0.019(9) 0.043(18)
C30A 0.054(18) 0.020(13) 0.044(14) -0.009(10) 0.006(12) -0.017(11)
C27A 0.08(2) 0.025(13) 0.051(14) 0.026(11) 0.030(14) 0.001(13)
C28A 0.042(12) 0.041(12) 0.042(11) 0.013(10) 0.001(9) 0.005(10)
C29A 0.062(16) 0.030(12) 0.055(15) 0.005(11) -0.007(11) -0.007(11)
C32A 0.027(8) 0.116(12) 0.077(11) 0.033(7) 0.010(5) -0.021(5)
S2B 0.038(5) 0.065(4) 0.047(3) 0.023(3) 0.014(3) -0.014(3)
_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
S1 C27B 1.713(5) . ?
S1 C30B 1.685(5) . ?
S1 C30A 1.77(2) . ?
S1 C27A 1.59(2) . ?
O2 C8 1.365(4) . ?
O2 C5 1.400(3) . ?
C8 C31 1.460(4) . ?
C8 C7 1.350(4) . ?
C1 C2 1.369(4) . ?
C1 B1 1.534(5) . ?
C1 O1B 1.397(10) . ?
C1 O1A 1.54(5) . ?
C10 C11 1.396(4) . ?
C10 C15 1.551(4) . ?
C10 C9 1.435(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.385(4) . ?
C5 C6 1.354(4) . ?
C5 B1 1.537(5) . ?
C19 C21 1.533(4) . ?
C19 C20 1.516(4) . ?
C19 C22 1.523(4) . ?
C19 C12 1.541(4) . ?
C14 C23 1.553(4) . ?
C14 C9 1.433(4) . ?
C14 C13 1.394(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.398(4) . ?
C15 C18 1.528(4) . ?
C15 C16 1.539(5) . ?
C15 C17 1.546(5) . ?
C3 H3A 0.9300 . ?
C3 H3B 0.9300 . ?
C3 C4B 1.370(6) . ?
C3 C4A 1.40(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.419(4) . ?
C31 S2A 1.690(4) . ?
C31 C32B 1.424(17) . ?
C31 C32A 1.420(13) . ?
C31 S2B 1.588(11) . ?
C7 H7 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C24 C23 1.527(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C25 C23 1.524(4) . ?
C23 C26 1.522(4) . ?
C12 C13 1.390(4) . ?
C9 B1 1.589(4) . ?
C13 H13 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C34 H34 0.9300 . ?
C34 H34A 0.9300 . ?
C34 C33 1.322(6) . ?
C34 S2A 1.632(5) . ?
C34 C32B 1.428(17) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C33 H33 0.9300 . ?
C33 H33A 0.9300 . ?
C33 C32A 1.437(13) . ?
C33 S2B 1.586(11) . ?
O1B C4B 1.353(11) . ?
C4B C27B 1.449(7) . ?
C27B C28B 1.366(6) . ?
C28B H28B 0.9300 . ?
C28B C29B 1.425(5) . ?
C29B H29B 0.9300 . ?
C29B C30B 1.335(6) . ?
C30B H30B 0.9300 . ?
O1A C4A 1.42(6) . ?
C32B H32B 0.9300 . ?
C4A C27A 1.43(4) . ?
C30A H30A 0.9300 . ?
C30A C29A 1.30(3) . ?
C27A C28A 1.40(3) . ?
C28A H28A 0.9300 . ?
C28A C29A 1.47(3) . ?
C29A H29A 0.9300 . ?
C32A H32A 0.9300 . ?
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
C30B S1 C27B 92.9(2) . . ?
C27A S1 C30A 95.3(11) . . ?
C8 O2 C5 107.2(2) . . ?
O2 C8 C31 116.1(3) . . ?
C7 C8 O2 110.8(3) . . ?
C7 C8 C31 132.9(3) . . ?
C2 C1 B1 137.6(3) . . ?
C2 C1 O1B 106.1(5) . . ?
C2 C1 O1A 106.4(19) . . ?
B1 C1 O1A 114.9(19) . . ?
O1B C1 B1 116.1(5) . . ?
C11 C10 C15 114.3(3) . . ?
C11 C10 C9 118.8(3) . . ?
C9 C10 C15 126.9(3) . . ?
C10 C11 H11 117.8 . . ?
C12 C11 C10 124.4(3) . . ?
C12 C11 H11 117.8 . . ?
O2 C5 B1 120.5(3) . . ?
C6 C5 O2 107.3(3) . . ?
C6 C5 B1 132.2(3) . . ?
C21 C19 C12 108.5(2) . . ?
C20 C19 C21 108.9(3) . . ?
C20 C19 C22 109.3(3) . . ?
C20 C19 C12 110.5(3) . . ?
C22 C19 C21 107.5(3) . . ?
C22 C19 C12 112.0(3) . . ?
C9 C14 C23 125.4(2) . . ?
C13 C14 C23 115.3(3) . . ?
C13 C14 C9 119.2(3) . . ?
C1 C2 H2 125.3 . . ?
C1 C2 C3 109.4(3) . . ?
C3 C2 H2 125.3 . . ?
C18 C15 C10 117.3(3) . . ?
C18 C15 C16 106.7(3) . . ?
C18 C15 C17 104.8(3) . . ?
C16 C15 C10 108.8(3) . . ?
C16 C15 C17 109.7(3) . . ?
C17 C15 C10 109.3(3) . . ?
C2 C3 H3A 127.0 . . ?
C2 C3 H3B 125.8 . . ?
C2 C3 C4A 108.4(14) . . ?
C4B C3 C2 106.0(3) . . ?
C4B C3 H3A 127.0 . . ?
C4A C3 H3B 125.8 . . ?
C5 C6 H6 125.4 . . ?
C5 C6 C7 109.2(3) . . ?
C7 C6 H6 125.4 . . ?
C8 C31 S2A 121.9(3) . . ?
C8 C31 S2B 121.6(4) . . ?
C32B C31 C8 132.5(8) . . ?
C32B C31 S2B 105.7(9) . . ?
C32A C31 C8 128.5(6) . . ?
C32A C31 S2A 109.2(6) . . ?
C8 C7 C6 105.5(3) . . ?
C8 C7 H7 127.2 . . ?
C6 C7 H7 127.2 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
C24 C23 C14 107.5(3) . . ?
C25 C23 C14 111.5(3) . . ?
C25 C23 C24 109.0(3) . . ?
C26 C23 C14 116.4(3) . . ?
C26 C23 C24 107.0(3) . . ?
C26 C23 C25 105.1(3) . . ?
C11 C12 C19 120.6(3) . . ?
C11 C12 C13 115.8(3) . . ?
C13 C12 C19 123.6(3) . . ?
C10 C9 B1 120.4(3) . . ?
C14 C9 C10 117.8(3) . . ?
C14 C9 B1 121.8(3) . . ?
C14 C13 H13 118.0 . . ?
C12 C13 C14 124.0(3) . . ?
C12 C13 H13 118.0 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C33 C34 H34 122.3 . . ?
C33 C34 H34A 128.6 . . ?
C33 C34 S2A 115.4(3) . . ?
C33 C34 C32B 102.8(8) . . ?
S2A C34 H34 122.3 . . ?
C32B C34 H34A 128.6 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C34 C33 H33 124.6 . . ?
C34 C33 H33A 120.6 . . ?
C34 C33 C32A 110.8(7) . . ?
C34 C33 S2B 118.8(5) . . ?
C32A C33 H33 124.6 . . ?
S2B C33 H33A 120.6 . . ?
C1 B1 C5 121.4(3) . . ?
C1 B1 C9 121.5(3) . . ?
C5 B1 C9 117.0(3) . . ?
C34 S2A C31 93.3(3) . . ?
C4B O1B C1 108.7(7) . . ?
C3 C4B C27B 134.3(4) . . ?
O1B C4B C3 109.5(5) . . ?
O1B C4B C27B 116.2(5) . . ?
C4B C27B S1 122.5(4) . . ?
C28B C27B S1 110.5(3) . . ?
C28B C27B C4B 127.0(4) . . ?
C27B C28B H28B 124.2 . . ?
C27B C28B C29B 111.5(4) . . ?
C29B C28B H28B 124.2 . . ?
C28B C29B H29B 123.2 . . ?
C30B C29B C28B 113.7(4) . . ?
C30B C29B H29B 123.2 . . ?
S1 C30B H30B 124.3 . . ?
C29B C30B S1 111.5(4) . . ?
C29B C30B H30B 124.3 . . ?
C4A O1A C1 104(3) . . ?
C31 C32B C34 115.9(14) . . ?
C31 C32B H32B 122.0 . . ?
C34 C32B H32B 122.0 . . ?
C3 C4A O1A 110(3) . . ?
C3 C4A C27A 137(3) . . ?
O1A C4A C27A 113(3) . . ?
S1 C30A H30A 125.7 . . ?
C29A C30A S1 108.6(16) . . ?
C29A C30A H30A 125.7 . . ?
C4A C27A S1 125(2) . . ?
C28A C27A S1 108.5(19) . . ?
C28A C27A C4A 125(2) . . ?
C27A C28A H28A 123.4 . . ?
C27A C28A C29A 113(2) . . ?
C29A C28A H28A 123.4 . . ?
C30A C29A C28A 111(2) . . ?
C30A C29A H29A 124.6 . . ?
C28A C29A H29A 124.6 . . ?
C31 C32A C33 110.7(10) . . ?
C31 C32A H32A 124.7 . . ?
C33 C32A H32A 124.7 . . ?
C33 S2B C31 95.5(7) . . ?
_shelx_res_file
;
TITL m18_a15sad_a.res in P-1
m18_a15sad.res
created by SHELXL-2018/1 at 08:48:37 on 24-Apr-2018
REM Old TITL m18_a15sad_a.res in P-1
REM SHELXT solution in P-1
REM R1 0.224, Rweak 0.026, Alpha 0.043, Orientation as input
REM Formula found by SHELXT: C34 O3 S2
CELL 0.71073 9.299 13.2392 13.6762 97.674 101.18 107.537
ZERR 2 0.0034 0.0048 0.005 0.008 0.007 0.007
LATT 1
SFAC C H B O S
UNIT 68 78 2 4 4
DFIX 1.4 C31 C32B C34 C32B
DFIX 1.6 S2A C34 S2A C31
DFIX 1.4 C32A C33 C32A C31
DFIX 1.6 S2B C31 S2B C33
ISOR C4A
L.S. 10
PLAN 20
TEMP 0
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.088000
FVAR 0.53353 0.82612 0.71199 0.71907
S1 5 0.943042 0.926593 0.710446 11.00000 0.04485 0.05325 =
0.04333 0.00691 0.00640 0.00193
O2 4 0.215715 0.487324 0.333597 11.00000 0.02327 0.02774 =
0.04057 0.01210 0.01312 0.00191
C8 1 0.081399 0.409250 0.276812 11.00000 0.02430 0.02548 =
0.04683 0.01027 0.01149 0.00656
C1 1 0.525250 0.671358 0.419527 11.00000 0.03220 0.02177 =
0.04117 0.01239 0.01773 0.00779
C10 1 0.475877 0.776166 0.189198 11.00000 0.02458 0.02484 =
0.03571 0.00688 0.01003 0.00505
C11 1 0.535836 0.820399 0.112467 11.00000 0.02610 0.02472 =
0.03948 0.01235 0.00957 0.00704
AFIX 43
H11 2 0.503519 0.875231 0.090215 11.00000 -1.20000
AFIX 0
C5 1 0.292747 0.537744 0.265578 11.00000 0.03287 0.02833 =
0.03653 0.01194 0.01944 0.01038
C19 1 0.700947 0.842716 -0.016370 11.00000 0.03027 0.02583 =
0.03279 0.01037 0.01190 0.00158
C14 1 0.628753 0.654731 0.177059 11.00000 0.02358 0.02362 =
0.02937 0.00611 0.00842 0.00244
C2 1 0.503260 0.639619 0.508355 11.00000 0.03504 0.03171 =
0.03824 0.01436 0.01681 0.00598
AFIX 43
H2 2 0.426265 0.577857 0.513111 11.00000 -1.20000
AFIX 0
C15 1 0.362234 0.827283 0.227770 11.00000 0.03702 0.03935 =
0.04427 0.01827 0.02015 0.01745
C3 1 0.614512 0.714464 0.590791 11.00000 0.03975 0.03937 =
0.03385 0.01612 0.01431 0.00701
PART 1
AFIX 43
H3A 2 0.630448 0.709442 0.658977 21.00000 -1.20000
AFIX 43
PART 0
PART 2
H3B 2 0.609783 0.721134 0.658555 -21.00000 -1.20000
AFIX 0
PART 0
C6 1 0.203412 0.489423 0.170305 11.00000 0.03433 0.03631 =
0.03918 0.00623 0.01889 0.00773
AFIX 43
H6 2 0.226744 0.507494 0.110425 11.00000 -1.20000
AFIX 0
C31 1 -0.021507 0.350233 0.333693 11.00000 0.02635 0.02926 =
0.05576 0.01445 0.01144 0.00357
C7 1 0.068557 0.406842 0.176393 11.00000 0.02902 0.03615 =
0.04448 0.00139 0.01107 0.00459
AFIX 43
H7 2 -0.011793 0.360743 0.122542 11.00000 -1.20000
AFIX 0
C21 1 0.562155 0.824128 -0.106267 11.00000 0.05514 0.04326 =
0.03945 0.01904 0.01463 0.00850
AFIX 137
H21A 2 0.493386 0.858985 -0.084899 11.00000 -1.50000
H21B 2 0.507234 0.747879 -0.129521 11.00000 -1.50000
H21C 2 0.598934 0.853882 -0.160676 11.00000 -1.50000
AFIX 0
C18 1 0.309157 0.794018 0.321226 11.00000 0.04696 0.04060 =
0.05121 0.01764 0.02775 0.02325
AFIX 137
H18A 2 0.256684 0.717198 0.307025 11.00000 -1.50000
H18B 2 0.239339 0.830584 0.337438 11.00000 -1.50000
H18C 2 0.398105 0.813375 0.377926 11.00000 -1.50000
AFIX 0
C20 1 0.781154 0.963406 0.023233 11.00000 0.06259 0.03834 =
0.04658 0.01582 0.02458 -0.00404
AFIX 137
H20A 2 0.813207 0.996685 -0.030772 11.00000 -1.50000
H20B 2 0.870741 0.975896 0.077826 11.00000 -1.50000
H20C 2 0.710322 0.994089 0.047733 11.00000 -1.50000
AFIX 0
C22 1 0.813210 0.794637 -0.056208 11.00000 0.05544 0.05684 =
0.05468 0.03032 0.03378 0.02026
AFIX 137
H22A 2 0.761829 0.718521 -0.083062 11.00000 -1.50000
H22B 2 0.902093 0.805534 -0.001606 11.00000 -1.50000
H22C 2 0.846462 0.829553 -0.109063 11.00000 -1.50000
AFIX 0
C24 1 0.862200 0.625151 0.274260 11.00000 0.05208 0.03996 =
0.09923 0.01809 -0.01569 0.01459
AFIX 137
H24A 2 0.923038 0.671237 0.237906 11.00000 -1.50000
H24B 2 0.909652 0.572822 0.292069 11.00000 -1.50000
H24C 2 0.857223 0.668072 0.335088 11.00000 -1.50000
AFIX 0
C16 1 0.214064 0.798672 0.141528 11.00000 0.04712 0.10737 =
0.05892 0.02260 0.01965 0.04787
AFIX 137
H16A 2 0.241565 0.823667 0.082720 11.00000 -1.50000
H16B 2 0.145038 0.832880 0.163558 11.00000 -1.50000
H16C 2 0.163170 0.721624 0.124516 11.00000 -1.50000
AFIX 0
C25 1 0.706442 0.494106 0.113580 11.00000 0.09634 0.03873 =
0.04728 0.00941 0.01854 0.03402
AFIX 137
H25A 2 0.605487 0.464132 0.066915 11.00000 -1.50000
H25B 2 0.739881 0.436552 0.134042 11.00000 -1.50000
H25C 2 0.779331 0.535831 0.080927 11.00000 -1.50000
AFIX 0
C23 1 0.697909 0.566825 0.207024 11.00000 0.02910 0.02360 =
0.03154 0.00854 0.01268 0.00693
C12 1 0.640170 0.788157 0.067250 11.00000 0.02331 0.02195 =
0.02894 0.00748 0.00699 0.00165
C9 1 0.521040 0.689550 0.222921 11.00000 0.02204 0.02313 =
0.03219 0.00593 0.00881 0.00133
C13 1 0.684748 0.705678 0.102530 11.00000 0.02278 0.02838 =
0.03013 0.00486 0.00879 0.00393
AFIX 43
H13 2 0.756324 0.683115 0.074693 11.00000 -1.20000
AFIX 0
C17 1 0.441149 0.951518 0.258544 11.00000 0.08344 0.04304 =
0.09534 0.02947 0.06544 0.03164
AFIX 137
H17A 2 0.535552 0.968928 0.310537 11.00000 -1.50000
H17B 2 0.372048 0.983261 0.284042 11.00000 -1.50000
H17C 2 0.464862 0.979529 0.200168 11.00000 -1.50000
AFIX 0
C34 1 -0.240328 0.233653 0.381452 11.00000 0.03278 0.05141 =
0.10140 0.02755 0.02611 -0.00126
PART 1
AFIX 43
H34 2 -0.334689 0.184405 0.383428 31.00000 -1.20000
AFIX 43
PART 0
PART 2
H34A 2 -0.338965 0.184923 0.375570 -31.00000 -1.20000
AFIX 0
PART 0
C26 1 0.610712 0.489838 0.265844 11.00000 0.09287 0.06315 =
0.09945 0.05784 0.07039 0.05441
AFIX 137
H26A 2 0.611593 0.530041 0.329933 11.00000 -1.50000
H26B 2 0.660451 0.437169 0.277634 11.00000 -1.50000
H26C 2 0.505104 0.453751 0.227060 11.00000 -1.50000
AFIX 0
C33 1 -0.134497 0.292872 0.464994 11.00000 0.05530 0.10459 =
0.06788 0.04108 0.02614 -0.01241
PART 1
AFIX 43
H33 2 -0.140928 0.285470 0.530834 41.00000 -1.20000
AFIX 43
PART 0
PART 2
H33A 2 -0.154217 0.289191 0.528776 -41.00000 -1.20000
AFIX 0
PART 0
B1 3 0.447614 0.632119 0.305259 11.00000 0.03262 0.02372 =
0.04044 0.01192 0.01716 0.01045
PART 1
S2A 5 -0.193933 0.252952 0.274660 31.00000 0.02392 0.03461 =
0.05563 0.00751 0.00922 0.00078
O1B 4 0.646404 0.770730 0.447888 21.00000 0.02344 0.02875 =
0.03075 0.00737 0.01371 -0.00262
C4B 1 0.695251 0.796684 0.550697 21.00000 0.02415 0.03091 =
0.03265 0.00606 0.01031 0.00601
C27B 1 0.816068 0.900619 0.593849 21.00000 0.02963 0.02865 =
0.03897 0.00638 0.01514 0.00771
C28B 1 0.848186 0.989345 0.550434 21.00000 0.03116 0.02932 =
0.04135 0.00389 0.01772 0.00705
AFIX 43
H28B 2 0.792283 0.992463 0.487345 21.00000 -1.20000
AFIX 0
C29B 1 0.978061 1.076536 0.613895 21.00000 0.03183 0.02626 =
0.05389 0.00413 0.01641 0.00173
AFIX 43
H29B 2 1.016311 1.143176 0.596186 21.00000 -1.20000
AFIX 0
C30B 1 1.039661 1.053560 0.701162 21.00000 0.03433 0.02907 =
0.04439 -0.00427 0.01120 -0.00375
AFIX 43
H30B 2 1.125109 1.101560 0.750595 21.00000 -1.20000
AFIX 0
PART 0
PART 2
O1A 4 0.689159 0.757471 0.446048 -21.00000 0.03442 0.05733 =
0.03413 0.00718 0.02727 0.00457
C32B 1 -0.165711 0.263031 0.302515 -31.00000 0.05243 0.07866 =
0.03996 -0.00475 -0.01896 0.04299
AFIX 43
H32B 2 -0.208683 0.227379 0.234860 -31.00000 -1.20000
AFIX 0
C4A 1 0.734489 0.777801 0.553973 -21.00000 0.03741
C30A 1 1.111519 1.020447 0.691948 -21.00000 0.05442 0.02023 =
0.04361 -0.00933 0.00610 -0.01703
AFIX 43
H30A 2 1.171930 1.085906 0.735943 -21.00000 -1.20000
AFIX 0
C27A 1 0.881402 0.862543 0.595724 -21.00000 0.07516 0.02486 =
0.05114 0.02617 0.03027 0.00132
C28A 1 1.004298 0.887699 0.548288 -21.00000 0.04187 0.04105 =
0.04164 0.01256 0.00122 0.00505
AFIX 43
H28A 2 1.002198 0.848232 0.486127 -21.00000 -1.20000
AFIX 0
C29A 1 1.136887 0.982605 0.606431 -21.00000 0.06233 0.02971 =
0.05467 0.00536 -0.00750 -0.00719
AFIX 43
H29A 2 1.226909 1.011819 0.585121 -21.00000 -1.20000
AFIX 0
PART 0
PART 1
C32A 1 -0.008183 0.370229 0.440224 41.00000 0.02704 0.11585 =
0.07671 0.03340 0.00969 -0.02110
AFIX 43
H32A 2 0.071336 0.425744 0.487476 41.00000 -1.20000
AFIX 0
PART 0
PART 2
S2B 5 0.026699 0.370302 0.454451 -41.00000 0.03833 0.06480 =
0.04660 0.02316 0.01395 -0.01400
HKLF 4
REM m18_a15sad_a.res in P-1
REM R1 = 0.0661 for 3415 Fo > 4sig(Fo) and 0.1247 for all 6097 data
REM 431 parameters refined using 8 restraints
END
WGHT 0.0872 0.0000
REM Highest difference peak 0.306, deepest hole -0.401, 1-sigma level 0.060
Q1 1 0.8790 0.8571 0.0052 11.00000 0.05 0.31
Q2 1 0.8632 0.6012 0.2006 11.00000 0.05 0.30
Q3 1 0.6028 0.4704 0.1188 11.00000 0.05 0.26
Q4 1 -0.2331 0.2214 0.2077 11.00000 0.05 0.25
Q5 1 0.4744 0.6541 0.3610 11.00000 0.05 0.24
Q6 1 1.0438 0.9352 0.8020 11.00000 0.05 0.24
Q7 1 0.5042 0.4162 0.0803 11.00000 0.05 0.24
Q8 1 0.5511 0.5096 0.3194 11.00000 0.05 0.23
Q9 1 0.4232 0.7465 -0.1250 11.00000 0.05 0.22
Q10 1 0.7722 0.5945 0.2409 11.00000 0.05 0.21
Q11 1 0.1240 0.3974 0.5179 11.00000 0.05 0.21
Q12 1 0.6929 0.5547 0.3259 11.00000 0.05 0.21
Q13 1 -0.2553 0.3141 0.2255 11.00000 0.05 0.20
Q14 1 0.9831 0.9927 0.7816 11.00000 0.05 0.20
Q15 1 0.6681 0.6050 0.1957 11.00000 0.05 0.20
Q16 1 0.5751 0.9583 0.3667 11.00000 0.05 0.20
Q17 1 -0.2593 0.2595 0.1667 11.00000 0.05 0.20
Q18 1 0.6239 0.9129 0.5905 11.00000 0.05 0.20
Q19 1 0.3545 0.5879 0.3000 11.00000 0.05 0.19
Q20 1 0.8795 0.9899 0.6797 11.00000 0.05 0.19
;
_shelx_res_checksum 12953
_olex2_submission_special_instructions 'No special instructions were received'