# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_jane_05072019_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2008416'
loop_
_audit_author_name
_audit_author_address
'Gyeongjin Park'
;Texas AM university
United States of America
;
_audit_update_record
;
2020-06-06 deposited with the CCDC. 2020-08-28 downloaded from the CCDC.
;
_audit_creation_date 2020-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic BrC30Cl2SSb
_chemical_formula_moiety 'C30 H24 Br S Sb, C H2 Cl2'
_chemical_formula_sum 'C31 H26 Br Cl2 S Sb'
_chemical_formula_weight 703.14
_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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Sb Sb -0.5866 1.5461 '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 9.1739(16)
_cell_length_b 11.503(2)
_cell_length_c 14.471(3)
_cell_angle_alpha 91.549(4)
_cell_angle_beta 92.383(4)
_cell_angle_gamma 113.406(4)
_cell_volume 1398.6(4)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9687
_cell_measurement_temperature 110(2)
_cell_measurement_theta_max 27.56
_cell_measurement_theta_min 2.83
_shelx_estimated_absorpt_T_max 0.443
_shelx_estimated_absorpt_T_min 0.411
_exptl_absorpt_coefficient_mu 2.700
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.5771
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1010 before and 0.0754 after correction.
The Ratio of minimum to maximum transmission is 0.7740.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.670
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 696
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.39
_exptl_crystal_size_min 0.36
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0615
_diffrn_reflns_av_unetI/netI 0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 66623
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.583
_diffrn_reflns_theta_min 2.445
_diffrn_ambient_temperature 109.98
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5811
_reflns_number_total 6426
_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 V8.38A (?, 2016)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max 1.182
_refine_diff_density_min -1.150
_refine_diff_density_rms 0.110
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.055
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 265
_refine_ls_number_reflns 6426
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0403
_refine_ls_R_factor_gt 0.0339
_refine_ls_restrained_S_all 1.055
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+4.6266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0773
_refine_ls_wR_factor_ref 0.0819
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C12(H12), C8(H8), C9(H9), C10(H10), C11(H11),
C14(H14), C18(H18), C17(H17), C16(H16), C15(H15), C24(H24), C23(H23), C22(H22),
C21(H21), C20(H20), C26(H26), C30(H30), C29(H29), C28(H28), C27(H27)
2.c Fitted hexagon refined as free rotating group:
C1(C2,C3,C4,C5,C6), C12(C7,C8,C9,C10,C11), C14(C13,C18,C17,C16,C15), C19(C24,
C23,C22,C21,C20), C26(C25,C30,C29,C28,C27)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary iterative
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb Sb 0.63896(2) 0.83011(2) 0.74271(2) 0.01631(6) Uani 1 1 d . . . . .
Br Br 0.89323(4) 1.09106(3) 0.74645(2) 0.02488(9) Uani 1 1 d . . . . .
S S 0.60062(10) 0.89155(8) 0.96827(6) 0.02211(16) Uani 1 1 d . . . . .
C1 C 0.7899(2) 0.8223(2) 0.85613(11) 0.0191(6) Uani 1 1 d . . . . .
C2 C 0.7596(2) 0.8451(2) 0.94668(13) 0.0193(6) Uani 1 1 d G . . . .
C3 C 0.8571(3) 0.8361(2) 1.01981(10) 0.0235(7) Uani 1 1 d G . . . .
H3 H 0.836418 0.851624 1.081699 0.028 Uiso 1 1 calc R . . . .
C4 C 0.9850(2) 0.8044(2) 1.00241(12) 0.0254(7) Uani 1 1 d G . . . .
H4 H 1.051714 0.798291 1.052390 0.030 Uiso 1 1 calc R . . . .
C5 C 1.0154(2) 0.7817(2) 0.91186(14) 0.0246(7) Uani 1 1 d G . . . .
H5 H 1.102775 0.760037 0.899962 0.030 Uiso 1 1 calc R . . . .
C6 C 0.9178(2) 0.7906(2) 0.83872(10) 0.0232(6) Uani 1 1 d G . . . .
H6 H 0.938538 0.775116 0.776841 0.028 Uiso 1 1 calc R . . . .
C12 C 0.51210(19) 0.54716(19) 0.77184(16) 0.0260(7) Uani 1 1 d . . . . .
H12 H 0.622767 0.565753 0.773220 0.031 Uiso 1 1 calc R . . . .
C7 C 0.4583(2) 0.64230(15) 0.75536(16) 0.0205(6) Uani 1 1 d G . . . .
C8 C 0.2963(2) 0.61509(18) 0.75333(16) 0.0266(7) Uani 1 1 d G . . . .
H8 H 0.259540 0.680111 0.742071 0.032 Uiso 1 1 calc R . . . .
C9 C 0.18824(18) 0.4927(2) 0.76779(18) 0.0348(9) Uani 1 1 d G . . . .
H9 H 0.077565 0.474146 0.766401 0.042 Uiso 1 1 calc R . . . .
C10 C 0.2421(2) 0.39760(16) 0.78426(17) 0.0344(9) Uani 1 1 d G . . . .
H10 H 0.168188 0.313983 0.794141 0.041 Uiso 1 1 calc R . . . .
C11 C 0.4040(3) 0.42481(17) 0.78629(17) 0.0311(8) Uani 1 1 d G . . . .
H11 H 0.440788 0.359785 0.797551 0.037 Uiso 1 1 calc R . . . .
C14 C 0.61986(19) 0.69610(19) 0.55749(14) 0.0218(6) Uani 1 1 d . . . . .
H14 H 0.513512 0.651034 0.574071 0.026 Uiso 1 1 calc R . . . .
C13 C 0.7262(2) 0.79237(19) 0.61666(11) 0.0186(6) Uani 1 1 d G . . . .
C18 C 0.8818(2) 0.85830(18) 0.59240(14) 0.0243(7) Uani 1 1 d G . . . .
H18 H 0.954445 0.924095 0.632843 0.029 Uiso 1 1 calc R . . . .
C17 C 0.9311(2) 0.8280(2) 0.50896(15) 0.0302(8) Uani 1 1 d G . . . .
H17 H 1.037404 0.873023 0.492372 0.036 Uiso 1 1 calc R . . . .
C16 C 0.8247(3) 0.7317(2) 0.44978(12) 0.0308(8) Uani 1 1 d G . . . .
H16 H 0.858419 0.710957 0.392749 0.037 Uiso 1 1 calc R . . . .
C15 C 0.6691(2) 0.66576(19) 0.47404(13) 0.0289(7) Uani 1 1 d G . . . .
H15 H 0.596473 0.599962 0.433597 0.035 Uiso 1 1 calc R . . . .
C19 C 0.4971(2) 0.9350(2) 0.71970(14) 0.0199(6) Uani 1 1 d . . . . .
C24 C 0.5201(3) 1.0047(2) 0.64059(14) 0.0291(7) Uani 1 1 d G . . . .
H24 H 0.600418 1.007045 0.600388 0.035 Uiso 1 1 calc R . . . .
C23 C 0.4256(3) 1.0708(2) 0.62029(14) 0.0366(9) Uani 1 1 d G . . . .
H23 H 0.441262 1.118363 0.566213 0.044 Uiso 1 1 calc R . . . .
C22 C 0.3080(3) 1.0673(2) 0.67910(16) 0.0312(8) Uani 1 1 d G . . . .
H22 H 0.243412 1.112467 0.665224 0.037 Uiso 1 1 calc R . . . .
C21 C 0.2850(2) 0.9976(2) 0.75822(14) 0.0256(7) Uani 1 1 d G . . . .
H21 H 0.204718 0.995255 0.798412 0.031 Uiso 1 1 calc R . . . .
C20 C 0.3796(2) 0.9315(2) 0.77852(12) 0.0233(6) Uani 1 1 d G . . . .
H20 H 0.363874 0.883937 0.832590 0.028 Uiso 1 1 calc R . . . .
C26 C 0.4241(3) 0.63431(19) 0.99250(14) 0.0257(7) Uani 1 1 d . . . . .
H26 H 0.483453 0.616894 0.945822 0.031 Uiso 1 1 calc R . . . .
C25 C 0.4589(2) 0.75889(16) 1.02218(14) 0.0199(6) Uani 1 1 d G . . . .
C30 C 0.3721(3) 0.78437(14) 1.09048(15) 0.0226(6) Uani 1 1 d G . . . .
H30 H 0.395865 0.869518 1.110770 0.027 Uiso 1 1 calc R . . . .
C29 C 0.2505(3) 0.68526(19) 1.12910(15) 0.0284(7) Uani 1 1 d G . . . .
H29 H 0.191186 0.702672 1.175783 0.034 Uiso 1 1 calc R . . . .
C28 C 0.2157(2) 0.56067(17) 1.09942(16) 0.0289(7) Uani 1 1 d G . . . .
H28 H 0.132638 0.492937 1.125815 0.035 Uiso 1 1 calc R . . . .
C27 C 0.3025(3) 0.53520(14) 1.03112(16) 0.0293(7) Uani 1 1 d G . . . .
H27 H 0.278770 0.450046 1.010835 0.035 Uiso 1 1 calc R . . . .
Cl1 Cl 1.23211(19) 0.7090(2) 0.51728(11) 0.0786(5) Uani 1 1 d . . . . .
Cl2 Cl 1.1959(3) 0.5238(2) 0.36740(12) 0.0996(7) Uani 1 1 d . . . . .
C31 C 1.1537(15) 0.6430(8) 0.4091(6) 0.139(5) Uani 1 1 d . . . . .
H31A H 1.036481 0.612319 0.409695 0.167 Uiso 1 1 calc R . . . .
H31B H 1.189311 0.711476 0.364702 0.167 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb 0.01559(10) 0.01703(11) 0.01539(10) 0.00001(7) 0.00156(7) 0.00551(8)
Br 0.02310(16) 0.02032(16) 0.02675(18) -0.00290(13) 0.00124(12) 0.00420(13)
S 0.0275(4) 0.0188(4) 0.0225(4) 0.0042(3) 0.0057(3) 0.0113(3)
C1 0.0185(14) 0.0158(14) 0.0198(15) -0.0005(11) -0.0018(11) 0.0037(12)
C2 0.0209(15) 0.0159(14) 0.0207(15) 0.0025(12) 0.0010(12) 0.0068(12)
C3 0.0306(17) 0.0220(16) 0.0172(15) 0.0008(12) -0.0005(12) 0.0097(14)
C4 0.0250(16) 0.0219(16) 0.0264(17) 0.0028(13) -0.0047(13) 0.0069(13)
C5 0.0185(15) 0.0229(16) 0.0302(18) 0.0041(13) 0.0009(13) 0.0058(13)
C6 0.0198(15) 0.0252(16) 0.0229(16) 0.0013(13) 0.0039(12) 0.0070(13)
C12 0.0312(17) 0.0211(16) 0.0213(16) -0.0003(13) 0.0010(13) 0.0058(14)
C7 0.0203(15) 0.0175(15) 0.0167(14) -0.0009(11) 0.0005(11) 0.0004(12)
C8 0.0220(16) 0.0288(18) 0.0242(17) -0.0002(14) 0.0008(13) 0.0051(14)
C9 0.0202(16) 0.037(2) 0.0303(19) -0.0008(16) 0.0004(14) -0.0058(15)
C10 0.040(2) 0.0227(18) 0.0216(17) 0.0015(14) -0.0014(15) -0.0074(15)
C11 0.047(2) 0.0175(16) 0.0204(17) 0.0004(13) -0.0032(15) 0.0052(15)
C14 0.0245(16) 0.0189(15) 0.0210(16) 0.0005(12) 0.0001(12) 0.0077(13)
C13 0.0243(15) 0.0175(14) 0.0153(14) 0.0011(11) 0.0024(11) 0.0095(12)
C18 0.0254(16) 0.0200(16) 0.0247(17) -0.0019(13) 0.0051(13) 0.0059(13)
C17 0.0328(18) 0.0291(18) 0.0289(18) 0.0023(15) 0.0133(15) 0.0115(15)
C16 0.049(2) 0.0275(18) 0.0210(17) 0.0006(14) 0.0093(15) 0.0196(17)
C15 0.043(2) 0.0235(17) 0.0204(16) -0.0047(13) -0.0017(14) 0.0140(16)
C19 0.0183(14) 0.0180(15) 0.0228(15) -0.0013(12) -0.0018(12) 0.0071(12)
C24 0.0300(18) 0.0353(19) 0.0267(18) 0.0074(15) 0.0082(14) 0.0168(16)
C23 0.042(2) 0.040(2) 0.036(2) 0.0162(17) 0.0064(17) 0.0223(18)
C22 0.0262(17) 0.0287(18) 0.042(2) 0.0023(16) -0.0028(15) 0.0143(15)
C21 0.0179(15) 0.0271(17) 0.0300(18) -0.0038(14) -0.0004(13) 0.0077(13)
C20 0.0202(15) 0.0217(16) 0.0245(16) 0.0005(13) 0.0001(12) 0.0048(13)
C26 0.0365(19) 0.0216(16) 0.0199(16) -0.0005(13) 0.0064(13) 0.0122(14)
C25 0.0216(15) 0.0170(15) 0.0198(15) 0.0017(12) -0.0006(12) 0.0065(12)
C30 0.0240(15) 0.0187(15) 0.0270(17) -0.0004(12) 0.0026(13) 0.0104(13)
C29 0.0278(17) 0.0289(18) 0.0331(19) 0.0052(15) 0.0103(14) 0.0154(15)
C28 0.0256(17) 0.0220(17) 0.038(2) 0.0067(14) 0.0062(14) 0.0076(14)
C27 0.0377(19) 0.0180(16) 0.0297(18) -0.0009(13) 0.0004(15) 0.0088(15)
Cl1 0.0591(8) 0.1297(15) 0.0643(9) 0.0034(9) -0.0104(7) 0.0573(10)
Cl2 0.1572(19) 0.1506(18) 0.0615(9) 0.0205(10) 0.0212(10) 0.1335(17)
C31 0.245(13) 0.088(6) 0.097(6) -0.028(5) -0.102(7) 0.093(7)
_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
Sb Br 2.9785(6) . ?
Sb C1 2.1301(14) . ?
Sb C7 2.1565(15) . ?
Sb C13 2.1237(14) . ?
Sb C19 2.1199(15) . ?
S C2 1.7774(16) . ?
S C25 1.7889(17) . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C12 C7 1.3900 . ?
C12 C11 1.3900 . ?
C7 C8 1.3900 . ?
C8 C9 1.3900 . ?
C9 C10 1.3900 . ?
C10 C11 1.3900 . ?
C14 C13 1.3900 . ?
C14 C15 1.3900 . ?
C13 C18 1.3900 . ?
C18 C17 1.3900 . ?
C17 C16 1.3900 . ?
C16 C15 1.3900 . ?
C19 C24 1.3900 . ?
C19 C20 1.3900 . ?
C24 C23 1.3900 . ?
C23 C22 1.3900 . ?
C22 C21 1.3900 . ?
C21 C20 1.3900 . ?
C26 C25 1.3900 . ?
C26 C27 1.3900 . ?
C25 C30 1.3900 . ?
C30 C29 1.3900 . ?
C29 C28 1.3900 . ?
C28 C27 1.3900 . ?
Cl1 C31 1.719(7) . ?
Cl2 C31 1.669(9) . ?
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
C1 Sb Br 79.22(6) . . ?
C1 Sb C7 95.91(8) . . ?
C7 Sb Br 174.08(6) . . ?
C13 Sb Br 87.86(6) . . ?
C13 Sb C1 109.56(8) . . ?
C13 Sb C7 97.00(8) . . ?
C19 Sb Br 80.31(6) . . ?
C19 Sb C1 133.58(8) . . ?
C19 Sb C7 100.99(8) . . ?
C19 Sb C13 110.79(8) . . ?
C2 S C25 104.23(11) . . ?
C2 C1 Sb 120.96(10) . . ?
C2 C1 C6 120.0 . . ?
C6 C1 Sb 119.01(10) . . ?
C1 C2 S 119.79(11) . . ?
C3 C2 S 120.16(11) . . ?
C3 C2 C1 120.0 . . ?
C4 C3 C2 120.0 . . ?
C3 C4 C5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C5 C6 C1 120.0 . . ?
C7 C12 C11 120.0 . . ?
C12 C7 Sb 116.22(11) . . ?
C12 C7 C8 120.0 . . ?
C8 C7 Sb 123.66(11) . . ?
C9 C8 C7 120.0 . . ?
C8 C9 C10 120.0 . . ?
C11 C10 C9 120.0 . . ?
C10 C11 C12 120.0 . . ?
C13 C14 C15 120.0 . . ?
C14 C13 Sb 116.91(10) . . ?
C14 C13 C18 120.0 . . ?
C18 C13 Sb 123.09(10) . . ?
C17 C18 C13 120.0 . . ?
C18 C17 C16 120.0 . . ?
C15 C16 C17 120.0 . . ?
C16 C15 C14 120.0 . . ?
C24 C19 Sb 117.74(11) . . ?
C24 C19 C20 120.0 . . ?
C20 C19 Sb 122.20(11) . . ?
C19 C24 C23 120.0 . . ?
C22 C23 C24 120.0 . . ?
C23 C22 C21 120.0 . . ?
C20 C21 C22 120.0 . . ?
C21 C20 C19 120.0 . . ?
C25 C26 C27 120.0 . . ?
C26 C25 S 122.41(12) . . ?
C26 C25 C30 120.0 . . ?
C30 C25 S 117.33(12) . . ?
C25 C30 C29 120.0 . . ?
C28 C29 C30 120.0 . . ?
C27 C28 C29 120.0 . . ?
C28 C27 C26 120.0 . . ?
Cl2 C31 Cl1 118.5(5) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sb C1 C2 S -4.19(16) . . . . ?
Sb C1 C2 C3 178.25(15) . . . . ?
Sb C1 C6 C5 -178.29(15) . . . . ?
Sb C7 C8 C9 -175.96(16) . . . . ?
Sb C13 C18 C17 179.58(16) . . . . ?
Sb C19 C24 C23 177.30(16) . . . . ?
Sb C19 C20 C21 -177.18(16) . . . . ?
S C2 C3 C4 -177.54(17) . . . . ?
S C25 C30 C29 174.30(17) . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C2 S C25 C26 -40.95(16) . . . . ?
C2 S C25 C30 144.90(13) . . . . ?
C2 C1 C6 C5 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C1 0.0 . . . . ?
C6 C1 C2 S 177.55(16) . . . . ?
C6 C1 C2 C3 0.0 . . . . ?
C12 C7 C8 C9 0.0 . . . . ?
C7 C12 C11 C10 0.0 . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C8 C9 C10 C11 0.0 . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C11 C12 C7 Sb 176.25(15) . . . . ?
C11 C12 C7 C8 0.0 . . . . ?
C14 C13 C18 C17 0.0 . . . . ?
C13 C14 C15 C16 0.0 . . . . ?
C13 C18 C17 C16 0.0 . . . . ?
C18 C17 C16 C15 0.0 . . . . ?
C17 C16 C15 C14 0.0 . . . . ?
C15 C14 C13 Sb -179.61(15) . . . . ?
C15 C14 C13 C18 0.0 . . . . ?
C19 C24 C23 C22 0.0 . . . . ?
C24 C19 C20 C21 0.0 . . . . ?
C24 C23 C22 C21 0.0 . . . . ?
C23 C22 C21 C20 0.0 . . . . ?
C22 C21 C20 C19 0.0 . . . . ?
C20 C19 C24 C23 0.0 . . . . ?
C26 C25 C30 C29 0.0 . . . . ?
C25 S C2 C1 111.78(13) . . . . ?
C25 S C2 C3 -70.67(14) . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C25 C30 C29 C28 0.0 . . . . ?
C30 C29 C28 C27 0.0 . . . . ?
C29 C28 C27 C26 0.0 . . . . ?
C27 C26 C25 S -174.00(18) . . . . ?
C27 C26 C25 C30 0.0 . . . . ?
_shelx_res_file
;
TITL Jane_05072019_0m_a.res in P-1
jane_05072019_0m_a.res
created by SHELXL-2018/3 at 15:11:23 on 04-May-2020
REM Jane_05072019_0m_a.res in P-1
REM wR2 = 0.154034, GooF = S = 1.29945, Restrained GooF = 1.29945 for all data
REM 325 parameters refined using 0 restraints
CELL 0.71073 9.1739 11.5028 14.4707 91.549 92.383 113.406
ZERR 2 0.0016 0.002 0.0025 0.004 0.004 0.004
LATT 1
SFAC C H Br Cl S Sb
UNIT 62 52 2 4 2 2
L.S. 4
PLAN 1 0 0
SIZE 0.36 0.39 0.4
TEMP -163.17
HTAB
CONF
fmap 2
acta
OMIT -1 1 1
REM
REM
REM
WGHT 0.027000 4.626600
FVAR 0.45924
SB 6 0.638965 0.830113 0.742706 11.00000 0.01559 0.01703 =
0.01539 0.00001 0.00156 0.00551
BR 3 0.893231 1.091056 0.746454 11.00000 0.02310 0.02032 =
0.02675 -0.00290 0.00124 0.00420
S 5 0.600623 0.891553 0.968272 11.00000 0.02752 0.01885 =
0.02251 0.00425 0.00566 0.01133
AFIX 66
C1 1 0.789916 0.822329 0.856134 11.00000 0.01855 0.01581 =
0.01977 -0.00048 -0.00181 0.00372
C2 1 0.759587 0.845052 0.946680 11.00000 0.02087 0.01594 =
0.02067 0.00246 0.00104 0.00676
C3 1 0.857147 0.836094 1.019815 11.00000 0.03056 0.02196 =
0.01715 0.00082 -0.00049 0.00972
AFIX 43
H3 2 0.836418 0.851624 1.081699 11.00000 -1.20000
AFIX 65
C4 1 0.985037 0.804413 1.002405 11.00000 0.02501 0.02191 =
0.02635 0.00282 -0.00468 0.00685
AFIX 43
H4 2 1.051714 0.798291 1.052390 11.00000 -1.20000
AFIX 65
C5 1 1.015368 0.781689 0.911860 11.00000 0.01848 0.02289 =
0.03025 0.00414 0.00092 0.00577
AFIX 43
H5 2 1.102775 0.760037 0.899962 11.00000 -1.20000
AFIX 65
C6 1 0.917809 0.790647 0.838724 11.00000 0.01984 0.02522 =
0.02287 0.00129 0.00394 0.00705
AFIX 43
H6 2 0.938538 0.775116 0.776841 11.00000 -1.20000
AFIX 66
C12 1 0.512095 0.547158 0.771836 11.00000 0.03115 0.02106 =
0.02127 -0.00026 0.00105 0.00582
AFIX 43
H12 2 0.622767 0.565753 0.773220 11.00000 -1.20000
AFIX 65
C7 1 0.458262 0.642296 0.755358 11.00000 0.02028 0.01755 =
0.01667 -0.00094 0.00050 0.00042
C8 1 0.296333 0.615088 0.753333 11.00000 0.02204 0.02876 =
0.02417 -0.00019 0.00082 0.00508
AFIX 43
H8 2 0.259540 0.680111 0.742071 11.00000 -1.20000
AFIX 65
C9 1 0.188236 0.492741 0.767785 11.00000 0.02015 0.03734 =
0.03029 -0.00079 0.00039 -0.00582
AFIX 43
H9 2 0.077565 0.474146 0.766401 11.00000 -1.20000
AFIX 65
C10 1 0.242068 0.397602 0.784263 11.00000 0.03993 0.02267 =
0.02160 0.00150 -0.00144 -0.00739
AFIX 43
H10 2 0.168188 0.313983 0.794141 11.00000 -1.20000
AFIX 65
C11 1 0.403996 0.424808 0.786289 11.00000 0.04741 0.01751 =
0.02043 0.00044 -0.00317 0.00522
AFIX 43
H11 2 0.440788 0.359785 0.797551 11.00000 -1.20000
AFIX 66
C14 1 0.619857 0.696096 0.557487 11.00000 0.02445 0.01890 =
0.02101 0.00051 0.00015 0.00775
AFIX 43
H14 2 0.513512 0.651034 0.574071 11.00000 -1.20000
AFIX 65
C13 1 0.726179 0.792366 0.616663 11.00000 0.02429 0.01751 =
0.01534 0.00112 0.00237 0.00952
C18 1 0.881779 0.858298 0.592398 11.00000 0.02540 0.01995 =
0.02473 -0.00194 0.00507 0.00590
AFIX 43
H18 2 0.954445 0.924095 0.632843 11.00000 -1.20000
AFIX 65
C17 1 0.931058 0.827961 0.508956 11.00000 0.03278 0.02915 =
0.02888 0.00230 0.01325 0.01147
AFIX 43
H17 2 1.037404 0.873023 0.492372 11.00000 -1.20000
AFIX 65
C16 1 0.824738 0.731691 0.449778 11.00000 0.04865 0.02749 =
0.02095 0.00059 0.00931 0.01958
AFIX 43
H16 2 0.858419 0.710957 0.392749 11.00000 -1.20000
AFIX 65
C15 1 0.669138 0.665758 0.474042 11.00000 0.04298 0.02349 =
0.02037 -0.00466 -0.00171 0.01399
AFIX 43
H15 2 0.596473 0.599962 0.433597 11.00000 -1.20000
AFIX 66
C19 1 0.497112 0.935025 0.719702 11.00000 0.01830 0.01802 =
0.02281 -0.00128 -0.00175 0.00708
C24 1 0.520095 1.004652 0.640586 11.00000 0.02996 0.03532 =
0.02667 0.00743 0.00825 0.01676
AFIX 43
H24 2 0.600418 1.007045 0.600388 11.00000 -1.20000
AFIX 65
C23 1 0.425553 1.070776 0.620285 11.00000 0.04156 0.03956 =
0.03555 0.01616 0.00635 0.02229
AFIX 43
H23 2 0.441262 1.118363 0.566213 11.00000 -1.20000
AFIX 65
C22 1 0.308027 1.067274 0.679100 11.00000 0.02618 0.02872 =
0.04155 0.00227 -0.00281 0.01431
AFIX 43
H22 2 0.243412 1.112467 0.665224 11.00000 -1.20000
AFIX 65
C21 1 0.285042 0.997648 0.758215 11.00000 0.01791 0.02715 =
0.03002 -0.00380 -0.00044 0.00766
AFIX 43
H21 2 0.204718 0.995255 0.798412 11.00000 -1.20000
AFIX 65
C20 1 0.379583 0.931523 0.778517 11.00000 0.02022 0.02167 =
0.02447 0.00049 0.00015 0.00479
AFIX 43
H20 2 0.363874 0.883937 0.832590 11.00000 -1.20000
AFIX 66
C26 1 0.424125 0.634306 0.992502 11.00000 0.03649 0.02165 =
0.01994 -0.00049 0.00637 0.01225
AFIX 43
H26 2 0.483453 0.616894 0.945822 11.00000 -1.20000
AFIX 65
C25 1 0.458902 0.758892 1.022184 11.00000 0.02156 0.01705 =
0.01979 0.00167 -0.00060 0.00654
C30 1 0.372096 0.784369 1.090484 11.00000 0.02395 0.01874 =
0.02702 -0.00044 0.00264 0.01041
AFIX 43
H30 2 0.395865 0.869518 1.110770 11.00000 -1.20000
AFIX 65
C29 1 0.250513 0.685260 1.129102 11.00000 0.02783 0.02894 =
0.03313 0.00523 0.01028 0.01539
AFIX 43
H29 2 0.191186 0.702672 1.175783 11.00000 -1.20000
AFIX 65
C28 1 0.215735 0.560673 1.099421 11.00000 0.02559 0.02197 =
0.03814 0.00673 0.00625 0.00756
AFIX 43
H28 2 0.132638 0.492937 1.125815 11.00000 -1.20000
AFIX 65
C27 1 0.302539 0.535195 1.031121 11.00000 0.03768 0.01801 =
0.02969 -0.00088 0.00045 0.00881
AFIX 43
H27 2 0.278770 0.450046 1.010835 11.00000 -1.20000
AFIX 0
CL1 4 1.232107 0.709021 0.517275 11.00000 0.05912 0.12969 =
0.06434 0.00341 -0.01045 0.05725
CL2 4 1.195853 0.523825 0.367397 11.00000 0.15719 0.15065 =
0.06145 0.02051 0.02124 0.13346
C31 1 1.153672 0.642957 0.409055 11.00000 0.24529 0.08750 =
0.09681 -0.02843 -0.10212 0.09315
AFIX 23
H31A 2 1.036481 0.612319 0.409695 11.00000 -1.20000
H31B 2 1.189311 0.711476 0.364702 11.00000 -1.20000
AFIX 0
HKLF 4
REM Jane_05072019_0m_a.res in P-1
REM wR2 = 0.0819, GooF = S = 1.055, Restrained GooF = 1.055 for all data
REM R1 = 0.0339 for 5811 Fo > 4sig(Fo) and 0.0403 for all 6426 data
REM 265 parameters refined using 0 restraints
END
WGHT 0.0270 4.6266
REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, -y+2, -z+2
HTAB C30 S_$1
EQIV $2 -x+2, -y+2, -z+1
HTAB C31 Br_$2
REM Highest difference peak 1.182, deepest hole -1.150, 1-sigma level 0.110
Q1 1 1.1223 0.4847 0.3464 11.00000 0.05 1.18
;
_shelx_res_checksum 30458
_olex2_submission_original_sample_id J
_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_jj_bf4_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2008417'
loop_
_audit_author_name
_audit_author_address
'Gyeongjin Park'
;Texas AM university
United States of America
;
_audit_update_record
;
2020-06-06 deposited with the CCDC. 2020-08-28 downloaded from the CCDC.
;
_audit_creation_date 2020-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic C30H24SBF4Sb
_chemical_formula_moiety 'C30 H24 S Sb, B F4'
_chemical_formula_sum 'C30 H24 B F4 S Sb'
_chemical_formula_weight 625.11
_chemical_absolute_configuration ?
_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'
F F 0.0171 0.0103 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
_cell_length_a 7.9877(11)
_cell_length_b 15.558(2)
_cell_length_c 21.445(3)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2665.0(7)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9824
_cell_measurement_temperature 110(2)
_cell_measurement_theta_max 27.57
_cell_measurement_theta_min 2.62
_shelx_estimated_absorpt_T_max 0.855
_shelx_estimated_absorpt_T_min 0.716
_exptl_absorpt_coefficient_mu 1.159
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.6596
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1791 before and 0.0723 after correction.
The Ratio of minimum to maximum transmission is 0.8847.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.558
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1248
_exptl_crystal_size_max 0.3088
_exptl_crystal_size_mid 0.1806
_exptl_crystal_size_min 0.1395
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0425
_diffrn_reflns_av_unetI/netI 0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_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 37617
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.527
_diffrn_reflns_theta_min 2.618
_diffrn_ambient_temperature 110.01
_diffrn_detector 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker SMART APEX2 area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.769
_reflns_Friedel_fraction_full 0.998
_reflns_Friedel_fraction_max 0.997
_reflns_number_gt 5875
_reflns_number_total 6122
_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. Completness statistics refer to single and
composite reflections containing twin component 1 only.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT V8.38A (?, 2016)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max 1.504
_refine_diff_density_min -0.464
_refine_diff_density_rms 0.076
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.49(3)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.072
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 335
_refine_ls_number_reflns 6122
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0312
_refine_ls_R_factor_gt 0.0289
_refine_ls_restrained_S_all 1.072
_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^)+(0.0453P)^2^+1.2439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0750
_refine_ls_wR_factor_ref 0.0770
_refine_special_details
;
Refined as a 2-component inversion twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.51(3)
0.49(3)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_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
Sb Sb 0.47451(3) 0.40506(2) 0.68044(2) 0.02621(9) Uani 1 1 d . . . . .
S S 0.76252(17) 0.53993(8) 0.62994(6) 0.0364(3) Uani 1 1 d . . . . .
C1 C 0.6258(6) 0.3827(3) 0.60219(19) 0.0261(9) Uani 1 1 d . . . . .
C2 C 0.7383(6) 0.4466(3) 0.5839(2) 0.0284(9) Uani 1 1 d . . . . .
C3 C 0.8371(7) 0.4327(3) 0.5313(2) 0.0379(11) Uani 1 1 d . . . . .
H3 H 0.914587 0.475344 0.518154 0.045 Uiso 1 1 calc R . . . .
C4 C 0.8223(8) 0.3573(4) 0.4984(2) 0.0447(13) Uani 1 1 d . . . . .
H4 H 0.887251 0.348959 0.461746 0.054 Uiso 1 1 calc R . . . .
C5 C 0.7143(8) 0.2937(3) 0.5179(2) 0.0436(12) Uani 1 1 d . . . . .
H5 H 0.707744 0.241251 0.495358 0.052 Uiso 1 1 calc R . . . .
C6 C 0.6152(6) 0.3059(3) 0.5700(2) 0.0329(10) Uani 1 1 d . . . . .
H6 H 0.540872 0.262051 0.583604 0.039 Uiso 1 1 calc R . . . .
C7 C 0.3078(5) 0.3007(3) 0.6819(2) 0.0275(8) Uani 1 1 d . . . . .
C8 C 0.3478(7) 0.2259(3) 0.7142(2) 0.0394(11) Uani 1 1 d . . . . .
H8 H 0.446064 0.223448 0.739096 0.047 Uiso 1 1 calc R . . . .
C9 C 0.2435(8) 0.1549(3) 0.7098(3) 0.0454(13) Uani 1 1 d . . . . .
H9 H 0.269973 0.103775 0.731906 0.054 Uiso 1 1 calc R . . . .
C10 C 0.1013(7) 0.1585(3) 0.6735(2) 0.0400(11) Uani 1 1 d . . . . .
H10 H 0.031054 0.109477 0.670094 0.048 Uiso 1 1 calc R . . . .
C11 C 0.0604(7) 0.2328(3) 0.6421(2) 0.0411(11) Uani 1 1 d . . . . .
H11 H -0.039099 0.235320 0.617848 0.049 Uiso 1 1 calc R . . . .
C12 C 0.1645(6) 0.3040(3) 0.6458(2) 0.0360(10) Uani 1 1 d . . . . .
H12 H 0.137503 0.354966 0.623536 0.043 Uiso 1 1 calc R . . . .
C13 C 0.3348(6) 0.5183(3) 0.6710(2) 0.0323(10) Uani 1 1 d . . . . .
C14 C 0.2732(7) 0.5382(4) 0.6124(3) 0.0420(12) Uani 1 1 d . . . . .
H14 H 0.287283 0.499660 0.578471 0.050 Uiso 1 1 calc R . . . .
C15 C 0.1902(8) 0.6159(4) 0.6044(3) 0.0549(15) Uani 1 1 d . . . . .
H15 H 0.146957 0.630736 0.564555 0.066 Uiso 1 1 calc R . . . .
C16 C 0.1704(8) 0.6712(4) 0.6535(4) 0.0623(19) Uani 1 1 d . . . . .
H16 H 0.115397 0.724626 0.647163 0.075 Uiso 1 1 calc R . . . .
C17 C 0.2295(8) 0.6501(4) 0.7123(4) 0.0559(16) Uani 1 1 d . . . . .
H17 H 0.212480 0.688257 0.746336 0.067 Uiso 1 1 calc R . . . .
C18 C 0.3137(8) 0.5732(3) 0.7214(3) 0.0441(13) Uani 1 1 d . . . . .
H18 H 0.356117 0.558314 0.761313 0.053 Uiso 1 1 calc R . . . .
C19 C 0.6306(6) 0.4059(3) 0.75868(19) 0.0327(9) Uani 1 1 d . . . . .
C20 C 0.5655(8) 0.4275(3) 0.8173(2) 0.0463(12) Uani 1 1 d . . . . .
H20 H 0.448365 0.434661 0.822955 0.056 Uiso 1 1 calc R . . . .
C21 C 0.6747(10) 0.4381(4) 0.8667(3) 0.0569(17) Uani 1 1 d . . . . .
H21 H 0.632800 0.452343 0.906833 0.068 Uiso 1 1 calc R . . . .
C22 C 0.8458(10) 0.4278(4) 0.8576(3) 0.062(2) Uani 1 1 d . . . . .
H22 H 0.920415 0.436956 0.891481 0.074 Uiso 1 1 calc R . . . .
C23 C 0.9090(7) 0.4046(4) 0.8002(3) 0.0518(13) Uani 1 1 d . . . . .
H23 H 1.025879 0.395966 0.794913 0.062 Uiso 1 1 calc R . . . .
C24 C 0.8003(7) 0.3938(4) 0.7499(2) 0.0396(11) Uani 1 1 d . . . . .
H24 H 0.842477 0.378368 0.710009 0.047 Uiso 1 1 calc R . . . .
C25 C 0.6693(7) 0.6219(3) 0.5839(2) 0.0389(11) Uani 1 1 d . . . . .
C26 C 0.5778(7) 0.6070(3) 0.5300(2) 0.0409(11) Uani 1 1 d . . . . .
H26 H 0.571522 0.550620 0.513127 0.049 Uiso 1 1 calc R . . . .
C27 C 0.4953(9) 0.6744(4) 0.5006(3) 0.0526(15) Uani 1 1 d . . . . .
H27 H 0.430701 0.663599 0.464217 0.063 Uiso 1 1 calc R . . . .
C28 C 0.5066(10) 0.7561(4) 0.5237(3) 0.0630(19) Uani 1 1 d . . . . .
H28 H 0.447511 0.801829 0.504282 0.076 Uiso 1 1 calc R . . . .
C29 C 0.6058(10) 0.7714(4) 0.5760(3) 0.065(2) Uani 1 1 d . . . . .
H29 H 0.618538 0.828611 0.590771 0.079 Uiso 1 1 calc R . . . .
C30 C 0.6860(9) 0.7050(3) 0.6069(3) 0.0528(15) Uani 1 1 d . . . . .
H30 H 0.751271 0.715961 0.643077 0.063 Uiso 1 1 calc R . . . .
F1 F 1.3462(7) 0.6035(3) 0.8991(2) 0.0902(15) Uani 1 1 d . . . . .
F2 F 1.1128(8) 0.5642(3) 0.9528(2) 0.0927(16) Uani 1 1 d . . . . .
F3 F 1.2081(5) 0.4867(3) 0.8726(2) 0.0741(12) Uani 1 1 d . . . . .
F4 F 1.3529(6) 0.4838(3) 0.9598(2) 0.0722(11) Uani 1 1 d . . . . .
B B 1.2559(9) 0.5384(4) 0.9236(3) 0.0486(15) 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
Sb 0.03006(14) 0.02537(13) 0.02321(13) -0.00090(10) 0.00271(10) -0.00235(11)
S 0.0425(7) 0.0324(6) 0.0343(6) -0.0011(5) 0.0005(5) -0.0095(5)
C1 0.030(2) 0.024(2) 0.0245(19) -0.0014(15) 0.0006(15) 0.0011(16)
C2 0.031(2) 0.028(2) 0.026(2) 0.0010(16) 0.0015(16) 0.0002(18)
C3 0.037(3) 0.038(2) 0.039(3) 0.0093(19) 0.012(2) 0.005(2)
C4 0.055(3) 0.048(3) 0.032(2) 0.002(2) 0.014(2) 0.021(3)
C5 0.062(3) 0.037(3) 0.032(2) -0.012(2) 0.002(2) 0.012(3)
C6 0.043(3) 0.025(2) 0.031(2) -0.0025(17) -0.0012(19) 0.0010(19)
C7 0.0301(19) 0.0269(19) 0.0254(18) -0.0026(17) 0.0042(19) -0.0045(16)
C8 0.042(3) 0.034(3) 0.042(3) 0.009(2) -0.008(2) -0.004(2)
C9 0.057(3) 0.029(2) 0.050(3) 0.015(2) -0.003(3) -0.007(2)
C10 0.042(3) 0.034(2) 0.043(3) -0.003(2) 0.007(2) -0.011(2)
C11 0.038(3) 0.039(3) 0.045(3) -0.001(2) -0.004(2) -0.004(2)
C12 0.036(3) 0.031(2) 0.041(3) 0.0064(19) -0.005(2) -0.001(2)
C13 0.029(2) 0.028(2) 0.039(3) 0.0055(18) 0.0095(18) -0.0011(17)
C14 0.035(3) 0.040(3) 0.051(3) 0.011(2) 0.003(2) 0.003(2)
C15 0.043(3) 0.050(3) 0.072(4) 0.024(3) 0.002(3) 0.004(3)
C16 0.040(3) 0.037(3) 0.110(6) 0.013(3) 0.014(3) 0.008(3)
C17 0.044(3) 0.043(3) 0.081(5) -0.014(3) 0.015(3) 0.001(3)
C18 0.047(3) 0.037(3) 0.048(3) -0.005(2) 0.013(2) -0.002(2)
C19 0.046(2) 0.029(2) 0.0239(19) 0.0017(18) -0.0007(16) -0.007(2)
C20 0.065(3) 0.046(3) 0.028(2) -0.002(2) 0.005(2) -0.010(2)
C21 0.087(5) 0.058(3) 0.026(2) -0.001(2) 0.001(3) -0.017(3)
C22 0.097(5) 0.052(4) 0.037(3) 0.010(2) -0.026(3) -0.036(3)
C23 0.052(3) 0.056(3) 0.047(3) 0.016(3) -0.017(2) -0.016(3)
C24 0.046(3) 0.042(3) 0.031(2) 0.0040(19) -0.0061(18) -0.009(2)
C25 0.046(3) 0.031(2) 0.039(3) 0.0025(18) 0.016(2) -0.006(2)
C26 0.053(3) 0.033(2) 0.037(2) 0.0038(19) 0.009(2) 0.005(2)
C27 0.064(4) 0.053(3) 0.041(3) 0.014(2) 0.018(3) 0.016(3)
C28 0.086(5) 0.046(3) 0.057(3) 0.020(3) 0.031(4) 0.021(3)
C29 0.095(5) 0.028(3) 0.073(4) 0.000(3) 0.039(4) 0.000(3)
C30 0.078(4) 0.029(3) 0.052(3) -0.006(2) 0.025(3) -0.009(3)
F1 0.119(4) 0.051(2) 0.101(3) 0.011(2) 0.017(3) -0.022(3)
F2 0.126(4) 0.073(3) 0.079(3) 0.004(2) 0.042(3) 0.027(3)
F3 0.059(2) 0.088(3) 0.076(3) -0.013(2) -0.012(2) -0.009(2)
F4 0.081(3) 0.062(2) 0.073(3) 0.005(2) -0.014(2) 0.008(2)
B 0.043(3) 0.043(3) 0.060(4) 0.007(3) -0.014(3) -0.010(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
Sb C1 2.097(4) . ?
Sb C7 2.100(4) . ?
Sb C13 2.095(5) . ?
Sb C19 2.090(4) . ?
S C2 1.766(5) . ?
S C25 1.775(6) . ?
C1 C2 1.396(6) . ?
C1 C6 1.382(6) . ?
C2 C3 1.395(6) . ?
C3 C4 1.374(8) . ?
C4 C5 1.378(8) . ?
C5 C6 1.384(7) . ?
C7 C8 1.391(6) . ?
C7 C12 1.383(6) . ?
C8 C9 1.386(8) . ?
C9 C10 1.379(8) . ?
C10 C11 1.377(7) . ?
C11 C12 1.388(7) . ?
C13 C14 1.386(7) . ?
C13 C18 1.386(7) . ?
C14 C15 1.388(8) . ?
C15 C16 1.369(10) . ?
C16 C17 1.387(11) . ?
C17 C18 1.386(9) . ?
C19 C20 1.400(7) . ?
C19 C24 1.382(7) . ?
C20 C21 1.383(8) . ?
C21 C22 1.390(11) . ?
C22 C23 1.379(10) . ?
C23 C24 1.395(7) . ?
C25 C26 1.388(8) . ?
C25 C30 1.390(7) . ?
C26 C27 1.389(7) . ?
C27 C28 1.367(9) . ?
C28 C29 1.395(11) . ?
C29 C30 1.385(10) . ?
F1 B 1.351(8) . ?
F2 B 1.364(9) . ?
F3 B 1.411(8) . ?
F4 B 1.386(8) . ?
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
C1 Sb C7 104.44(17) . . ?
C13 Sb C1 111.68(17) . . ?
C13 Sb C7 108.30(17) . . ?
C19 Sb C1 107.45(17) . . ?
C19 Sb C7 111.77(18) . . ?
C19 Sb C13 112.9(2) . . ?
C2 S C25 103.5(2) . . ?
C2 C1 Sb 118.5(3) . . ?
C6 C1 Sb 120.5(3) . . ?
C6 C1 C2 121.0(4) . . ?
C1 C2 S 120.0(3) . . ?
C3 C2 S 121.2(4) . . ?
C3 C2 C1 118.8(4) . . ?
C4 C3 C2 120.0(5) . . ?
C3 C4 C5 120.7(5) . . ?
C4 C5 C6 120.4(5) . . ?
C1 C6 C5 119.1(5) . . ?
C8 C7 Sb 120.6(3) . . ?
C12 C7 Sb 119.1(3) . . ?
C12 C7 C8 120.0(4) . . ?
C9 C8 C7 119.6(5) . . ?
C10 C9 C8 120.1(5) . . ?
C11 C10 C9 120.4(5) . . ?
C10 C11 C12 120.0(5) . . ?
C7 C12 C11 119.9(4) . . ?
C14 C13 Sb 117.7(4) . . ?
C14 C13 C18 121.7(5) . . ?
C18 C13 Sb 120.5(4) . . ?
C13 C14 C15 118.5(6) . . ?
C16 C15 C14 120.5(6) . . ?
C15 C16 C17 120.8(6) . . ?
C18 C17 C16 119.8(6) . . ?
C13 C18 C17 118.8(6) . . ?
C20 C19 Sb 120.0(4) . . ?
C24 C19 Sb 118.3(3) . . ?
C24 C19 C20 121.3(5) . . ?
C21 C20 C19 118.8(6) . . ?
C20 C21 C22 120.0(6) . . ?
C23 C22 C21 121.0(5) . . ?
C22 C23 C24 119.6(6) . . ?
C19 C24 C23 119.3(5) . . ?
C26 C25 S 124.4(4) . . ?
C26 C25 C30 120.1(5) . . ?
C30 C25 S 115.5(5) . . ?
C25 C26 C27 120.2(5) . . ?
C28 C27 C26 120.4(6) . . ?
C27 C28 C29 119.2(6) . . ?
C30 C29 C28 121.3(6) . . ?
C29 C30 C25 118.7(7) . . ?
F1 B F2 113.9(6) . . ?
F1 B F3 105.7(6) . . ?
F1 B F4 112.3(6) . . ?
F2 B F3 107.3(5) . . ?
F2 B F4 113.1(6) . . ?
F4 B F3 103.7(5) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sb C1 C2 S 4.9(5) . . . . ?
Sb C1 C2 C3 -178.9(3) . . . . ?
Sb C1 C6 C5 178.7(4) . . . . ?
Sb C7 C8 C9 -174.0(4) . . . . ?
Sb C7 C12 C11 174.5(4) . . . . ?
Sb C13 C14 C15 -175.6(4) . . . . ?
Sb C13 C18 C17 175.9(4) . . . . ?
Sb C19 C20 C21 -172.0(4) . . . . ?
Sb C19 C24 C23 172.2(4) . . . . ?
S C2 C3 C4 176.3(4) . . . . ?
S C25 C26 C27 173.5(4) . . . . ?
S C25 C30 C29 -175.2(5) . . . . ?
C1 C2 C3 C4 0.1(7) . . . . ?
C2 S C25 C26 9.2(5) . . . . ?
C2 S C25 C30 -173.9(4) . . . . ?
C2 C1 C6 C5 -2.1(7) . . . . ?
C2 C3 C4 C5 -2.0(8) . . . . ?
C3 C4 C5 C6 1.9(9) . . . . ?
C4 C5 C6 C1 0.2(8) . . . . ?
C6 C1 C2 S -174.3(4) . . . . ?
C6 C1 C2 C3 1.9(7) . . . . ?
C7 C8 C9 C10 0.2(9) . . . . ?
C8 C7 C12 C11 0.4(7) . . . . ?
C8 C9 C10 C11 -1.0(9) . . . . ?
C9 C10 C11 C12 1.4(8) . . . . ?
C10 C11 C12 C7 -1.1(8) . . . . ?
C12 C7 C8 C9 0.1(8) . . . . ?
C13 C14 C15 C16 0.0(8) . . . . ?
C14 C13 C18 C17 -0.5(8) . . . . ?
C14 C15 C16 C17 -1.3(10) . . . . ?
C15 C16 C17 C18 1.7(10) . . . . ?
C16 C17 C18 C13 -0.8(9) . . . . ?
C18 C13 C14 C15 0.9(8) . . . . ?
C19 C20 C21 C22 0.4(9) . . . . ?
C20 C19 C24 C23 -1.0(8) . . . . ?
C20 C21 C22 C23 -2.0(10) . . . . ?
C21 C22 C23 C24 2.1(9) . . . . ?
C22 C23 C24 C19 -0.6(9) . . . . ?
C24 C19 C20 C21 1.1(8) . . . . ?
C25 S C2 C1 -109.4(4) . . . . ?
C25 S C2 C3 74.5(4) . . . . ?
C25 C26 C27 C28 1.5(9) . . . . ?
C26 C25 C30 C29 1.9(8) . . . . ?
C26 C27 C28 C29 1.9(9) . . . . ?
C27 C28 C29 C30 -3.4(10) . . . . ?
C28 C29 C30 C25 1.4(9) . . . . ?
C30 C25 C26 C27 -3.4(8) . . . . ?
_shelx_res_file
;
TITL JJ_BF4_0ma_a.res in P2(1)2(1)2(1)
jj_bf4_0ma_a.res
created by SHELXL-2018/3 at 15:18:04 on 04-May-2020
REM JJ_BF4_0ma_a.res in P2(1)2(1)2(1)
REM wR2 = 0.116634, GooF = S = 1.00869, Restrained GooF = 1.00869 for all data
REM 334 parameters refined using 0 restraints
CELL 0.71073 7.9877 15.5576 21.4453 90 90 90
ZERR 4 0.0011 0.0023 0.0031 0 0 0
LATT -1
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5-X,-Y,0.5+Z
SFAC C H B F S Sb
UNIT 120 96 4 16 4 4
L.S. 4
PLAN 1 0 0
SIZE 0.1395 0.1806 0.3088
TEMP -163.14
HTAB
CONF
MORE -1
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
OMIT 1 0 5
OMIT 0 1 2
OMIT 0 2 8
OMIT 0 8 2
OMIT 2 1 5
OMIT -1 3 3
OMIT 0 3 10
OMIT 2 0 7
OMIT 0 0 12
OMIT 0 1 8
OMIT -1 5 2
OMIT 2 0 3
OMIT 1 5 2
OMIT 3 1 0
OMIT 2 1 2
OMIT 0 5 8
OMIT 0 9 2
OMIT 1 5 14
REM
REM
REM
WGHT 0.045300 1.243900
BASF 0.48688
FVAR 0.43814
SB 6 0.474512 0.405064 0.680439 11.00000 0.03006 0.02537 =
0.02321 -0.00090 0.00271 -0.00235
S 5 0.762521 0.539929 0.629936 11.00000 0.04248 0.03238 =
0.03435 -0.00113 0.00051 -0.00950
C1 1 0.625805 0.382697 0.602191 11.00000 0.02965 0.02403 =
0.02451 -0.00137 0.00064 0.00107
C2 1 0.738302 0.446576 0.583936 11.00000 0.03098 0.02787 =
0.02644 0.00105 0.00146 0.00015
C3 1 0.837092 0.432694 0.531265 11.00000 0.03676 0.03835 =
0.03856 0.00926 0.01208 0.00535
AFIX 43
H3 2 0.914587 0.475344 0.518154 11.00000 -1.20000
AFIX 0
C4 1 0.822293 0.357329 0.498354 11.00000 0.05475 0.04777 =
0.03156 0.00221 0.01417 0.02147
AFIX 43
H4 2 0.887251 0.348959 0.461746 11.00000 -1.20000
AFIX 0
C5 1 0.714256 0.293741 0.517863 11.00000 0.06189 0.03662 =
0.03235 -0.01171 0.00193 0.01154
AFIX 43
H5 2 0.707744 0.241251 0.495358 11.00000 -1.20000
AFIX 0
C6 1 0.615197 0.305908 0.570049 11.00000 0.04286 0.02468 =
0.03101 -0.00251 -0.00119 0.00100
AFIX 43
H6 2 0.540872 0.262051 0.583604 11.00000 -1.20000
AFIX 0
C7 1 0.307789 0.300684 0.681931 11.00000 0.03010 0.02693 =
0.02536 -0.00261 0.00422 -0.00449
C8 1 0.347800 0.225891 0.714203 11.00000 0.04216 0.03443 =
0.04167 0.00918 -0.00832 -0.00439
AFIX 43
H8 2 0.446064 0.223448 0.739096 11.00000 -1.20000
AFIX 0
C9 1 0.243463 0.154938 0.709831 11.00000 0.05700 0.02910 =
0.05011 0.01515 -0.00258 -0.00680
AFIX 43
H9 2 0.269973 0.103775 0.731906 11.00000 -1.20000
AFIX 0
C10 1 0.101263 0.158543 0.673483 11.00000 0.04246 0.03438 =
0.04315 -0.00282 0.00683 -0.01081
AFIX 43
H10 2 0.031054 0.109477 0.670094 11.00000 -1.20000
AFIX 0
C11 1 0.060375 0.232820 0.642061 11.00000 0.03843 0.03941 =
0.04540 -0.00070 -0.00440 -0.00387
AFIX 43
H11 2 -0.039099 0.235320 0.617848 11.00000 -1.20000
AFIX 0
C12 1 0.164540 0.304018 0.645782 11.00000 0.03570 0.03092 =
0.04128 0.00641 -0.00511 -0.00101
AFIX 43
H12 2 0.137503 0.354966 0.623536 11.00000 -1.20000
AFIX 0
C13 1 0.334849 0.518306 0.671036 11.00000 0.02944 0.02842 =
0.03914 0.00552 0.00952 -0.00112
C14 1 0.273156 0.538237 0.612404 11.00000 0.03526 0.03967 =
0.05103 0.01137 0.00302 0.00304
AFIX 43
H14 2 0.287283 0.499660 0.578471 11.00000 -1.20000
AFIX 0
C15 1 0.190222 0.615883 0.604387 11.00000 0.04277 0.04970 =
0.07217 0.02432 0.00164 0.00419
AFIX 43
H15 2 0.146957 0.630736 0.564555 11.00000 -1.20000
AFIX 0
C16 1 0.170365 0.671179 0.653477 11.00000 0.03998 0.03706 =
0.10999 0.01306 0.01361 0.00775
AFIX 43
H16 2 0.115397 0.724626 0.647163 11.00000 -1.20000
AFIX 0
C17 1 0.229549 0.650109 0.712335 11.00000 0.04371 0.04337 =
0.08073 -0.01411 0.01476 0.00091
AFIX 43
H17 2 0.212480 0.688257 0.746336 11.00000 -1.20000
AFIX 0
C18 1 0.313699 0.573172 0.721355 11.00000 0.04659 0.03711 =
0.04846 -0.00541 0.01313 -0.00189
AFIX 43
H18 2 0.356117 0.558314 0.761313 11.00000 -1.20000
AFIX 0
C19 1 0.630554 0.405929 0.758684 11.00000 0.04557 0.02863 =
0.02393 0.00169 -0.00074 -0.00749
C20 1 0.565478 0.427463 0.817268 11.00000 0.06530 0.04573 =
0.02798 -0.00228 0.00486 -0.01041
AFIX 43
H20 2 0.448365 0.434661 0.822955 11.00000 -1.20000
AFIX 0
C21 1 0.674704 0.438064 0.866690 11.00000 0.08736 0.05761 =
0.02579 -0.00125 0.00087 -0.01743
AFIX 43
H21 2 0.632800 0.452343 0.906833 11.00000 -1.20000
AFIX 0
C22 1 0.845836 0.427820 0.857616 11.00000 0.09657 0.05167 =
0.03703 0.01031 -0.02623 -0.03598
AFIX 43
H22 2 0.920415 0.436956 0.891481 11.00000 -1.20000
AFIX 0
C23 1 0.908992 0.404592 0.800185 11.00000 0.05189 0.05612 =
0.04724 0.01642 -0.01689 -0.01598
AFIX 43
H23 2 1.025879 0.395966 0.794913 11.00000 -1.20000
AFIX 0
C24 1 0.800284 0.393835 0.749878 11.00000 0.04613 0.04188 =
0.03068 0.00403 -0.00614 -0.00940
AFIX 43
H24 2 0.842477 0.378368 0.710009 11.00000 -1.20000
AFIX 0
C25 1 0.669289 0.621850 0.583934 11.00000 0.04641 0.03107 =
0.03928 0.00250 0.01592 -0.00605
C26 1 0.577781 0.606995 0.529989 11.00000 0.05323 0.03257 =
0.03680 0.00381 0.00868 0.00475
AFIX 43
H26 2 0.571522 0.550620 0.513127 11.00000 -1.20000
AFIX 0
C27 1 0.495302 0.674369 0.500582 11.00000 0.06428 0.05274 =
0.04074 0.01390 0.01759 0.01554
AFIX 43
H27 2 0.430701 0.663599 0.464217 11.00000 -1.20000
AFIX 0
C28 1 0.506567 0.756053 0.523666 11.00000 0.08579 0.04589 =
0.05744 0.02006 0.03060 0.02136
AFIX 43
H28 2 0.447511 0.801829 0.504282 11.00000 -1.20000
AFIX 0
C29 1 0.605760 0.771415 0.576005 11.00000 0.09495 0.02844 =
0.07289 -0.00023 0.03869 -0.00011
AFIX 43
H29 2 0.618538 0.828611 0.590771 11.00000 -1.20000
AFIX 0
C30 1 0.686049 0.704954 0.606904 11.00000 0.07754 0.02908 =
0.05188 -0.00569 0.02452 -0.00869
AFIX 43
H30 2 0.751271 0.715961 0.643077 11.00000 -1.20000
AFIX 0
F1 4 1.346224 0.603547 0.899134 11.00000 0.11893 0.05073 =
0.10088 0.01060 0.01701 -0.02246
F2 4 1.112806 0.564187 0.952822 11.00000 0.12617 0.07299 =
0.07894 0.00401 0.04246 0.02689
F3 4 1.208056 0.486679 0.872614 11.00000 0.05906 0.08759 =
0.07566 -0.01321 -0.01170 -0.00861
F4 4 1.352874 0.483837 0.959812 11.00000 0.08108 0.06214 =
0.07340 0.00482 -0.01410 0.00836
B 3 1.255935 0.538371 0.923636 11.00000 0.04336 0.04257 =
0.05983 0.00725 -0.01402 -0.00960
HKLF 4
REM JJ_BF4_0ma_a.res in P2(1)2(1)2(1)
REM wR2 = 0.0770, GooF = S = 1.072, Restrained GooF = 1.072 for all data
REM R1 = 0.0289 for 5875 Fo > 4sig(Fo) and 0.0312 for all 6122 data
REM 335 parameters refined using 0 restraints
END
WGHT 0.0453 1.2516
REM Instructions for potential hydrogen bonds
EQIV $1 -x+5/2, -y+1, z-1/2
HTAB C3 F4_$1
REM Highest difference peak 1.504, deepest hole -0.464, 1-sigma level 0.076
Q1 1 1.0073 0.3980 0.6773 11.00000 0.05 1.50
;
_shelx_res_checksum 7385
_olex2_submission_original_sample_id JJ_BF4
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.51(3)
2 0.49(3)
#######################################################################
#
# 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_phssb(ptol)3br
_database_code_depnum_ccdc_archive 'CCDC 2021695'
loop_
_audit_author_name
_audit_author_address
'Gyeongjin Park'
;Texas AM university
United States of America
;
_audit_update_record
;
2020-08-05 deposited with the CCDC. 2020-08-28 downloaded from the CCDC.
;
_audit_creation_date 2020-08-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C33 H30 Br S Sb'
_chemical_formula_sum 'C33 H30 Br S Sb'
_chemical_formula_weight 660.29
_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'
Br Br -0.2901 2.4595 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 16.7041(12)
_cell_length_b 10.2829(7)
_cell_length_c 17.9121(13)
_cell_angle_alpha 90
_cell_angle_beta 107.860(2)
_cell_angle_gamma 90
_cell_volume 2928.4(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9322
_cell_measurement_temperature 110
_cell_measurement_theta_max 30.657
_cell_measurement_theta_min 2.313
_shelx_estimated_absorpt_T_max 0.702
_shelx_estimated_absorpt_T_min 0.511
_exptl_absorpt_coefficient_mu 2.397
_exptl_absorpt_correction_T_max 0.7462
_exptl_absorpt_correction_T_min 0.5782
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1042 before and 0.0673 after correction. The Ratio of minimum to maximum transmission is 0.7749. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.498
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1320
_exptl_crystal_size_max 0.323
_exptl_crystal_size_mid 0.2515
_exptl_crystal_size_min 0.1585
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0750
_diffrn_reflns_av_unetI/netI 0.0379
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 110270
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 31.063
_diffrn_reflns_theta_min 2.002
_diffrn_ambient_temperature 110.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7431
_reflns_number_total 9366
_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 V8.38A (?, 2016)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max 1.672
_refine_diff_density_min -1.284
_refine_diff_density_rms 0.156
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.160
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 328
_refine_ls_number_reflns 9366
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0698
_refine_ls_R_factor_gt 0.0490
_refine_ls_restrained_S_all 1.160
_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^)+(0.0288P)^2^+16.4567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1124
_refine_ls_wR_factor_ref 0.1207
_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:
C5(H5), C15(H15), C18(H18), C6(H6), C9(H9), C19(H19), C8(H8), C16(H16),
C22(H22), C4(H4), C26(H26), C12(H12), C25(H25), C11(H11), C3(H3), C23(H23),
C29(H29), C33(H33), C32(H32), C30(H30), C31(H31)
2.b Idealised Me refined as rotating group:
C13(H13A,H13B,H13C), C27(H27A,H27B,H27C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_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
Sb Sb 0.49967(2) 0.38634(3) 0.68730(2) 0.01469(7) Uani 1 1 d . . . . .
Br Br 0.63702(3) 0.37335(4) 0.83251(2) 0.02132(9) Uani 1 1 d . . . . .
S S 0.41892(7) 0.64805(12) 0.74701(7) 0.0254(2) Uani 1 1 d . . . . .
C5 C 0.6472(3) 0.7267(5) 0.6666(3) 0.0258(9) Uani 1 1 d . . . . .
H5 H 0.694429 0.742866 0.648929 0.031 Uiso 1 1 calc R . . . .
C1 C 0.5496(2) 0.5771(4) 0.6946(2) 0.0166(7) Uani 1 1 d . . . . .
C14 C 0.5643(3) 0.2606(4) 0.6315(2) 0.0166(7) Uani 1 1 d . . . . .
C21 C 0.4393(2) 0.2731(4) 0.7526(2) 0.0175(7) Uani 1 1 d . . . . .
C15 C 0.5226(3) 0.2252(4) 0.5532(2) 0.0204(8) Uani 1 1 d . . . . .
H15 H 0.467593 0.257241 0.527831 0.024 Uiso 1 1 calc R . . . .
C18 C 0.6829(3) 0.1324(4) 0.6256(3) 0.0230(8) Uani 1 1 d . . . . .
H18 H 0.737983 0.100368 0.650589 0.028 Uiso 1 1 calc R . . . .
C10 C 0.2512(3) 0.4730(4) 0.4574(2) 0.0213(8) Uani 1 1 d . . . . .
C7 C 0.3909(2) 0.4241(4) 0.5894(2) 0.0156(7) Uani 1 1 d . . . . .
C6 C 0.6182(3) 0.6000(4) 0.6679(2) 0.0217(8) Uani 1 1 d . . . . .
H6 H 0.645031 0.529812 0.650658 0.026 Uiso 1 1 calc R . . . .
C9 C 0.3148(3) 0.5637(4) 0.4829(2) 0.0241(9) Uani 1 1 d . . . . .
H9 H 0.310907 0.643792 0.455544 0.029 Uiso 1 1 calc R . . . .
C19 C 0.6453(3) 0.2129(4) 0.6669(2) 0.0187(7) Uani 1 1 d . . . . .
H19 H 0.674704 0.235847 0.719513 0.022 Uiso 1 1 calc R . . . .
C8 C 0.3844(3) 0.5400(4) 0.5477(2) 0.0207(8) Uani 1 1 d . . . . .
H8 H 0.427795 0.603184 0.563721 0.025 Uiso 1 1 calc R . . . .
C16 C 0.5611(3) 0.1445(4) 0.5133(2) 0.0231(8) Uani 1 1 d . . . . .
H16 H 0.531704 0.120533 0.460842 0.028 Uiso 1 1 calc R . . . .
C22 C 0.4733(3) 0.1524(4) 0.7784(3) 0.0231(8) Uani 1 1 d . . . . .
H22 H 0.523759 0.125492 0.769023 0.028 Uiso 1 1 calc R . . . .
C4 C 0.6078(3) 0.8286(5) 0.6909(3) 0.0290(10) Uani 1 1 d . . . . .
H4 H 0.628081 0.914691 0.690038 0.035 Uiso 1 1 calc R . . . .
C17 C 0.6420(3) 0.0971(4) 0.5481(3) 0.0241(8) Uani 1 1 d . . . . .
C24 C 0.3602(3) 0.1077(5) 0.8323(3) 0.0259(9) Uani 1 1 d . . . . .
C26 C 0.3646(3) 0.3111(4) 0.7645(3) 0.0227(8) Uani 1 1 d . . . . .
H26 H 0.339848 0.392349 0.745062 0.027 Uiso 1 1 calc R . . . .
C12 C 0.3261(2) 0.3326(4) 0.5644(2) 0.0182(7) Uani 1 1 d . . . . .
H12 H 0.329028 0.253727 0.592664 0.022 Uiso 1 1 calc R . . . .
C25 C 0.3263(3) 0.2297(5) 0.8050(3) 0.0269(9) Uani 1 1 d . . . . .
H25 H 0.275930 0.257186 0.814408 0.032 Uiso 1 1 calc R . . . .
C2 C 0.5097(3) 0.6799(4) 0.7190(2) 0.0192(8) Uani 1 1 d . . . . .
C13 C 0.1760(3) 0.5002(5) 0.3867(3) 0.0300(10) Uani 1 1 d . . . . .
H13A H 0.124888 0.501856 0.402650 0.045 Uiso 1 1 calc GR . . . .
H13B H 0.171070 0.431762 0.347428 0.045 Uiso 1 1 calc GR . . . .
H13C H 0.183207 0.584535 0.364105 0.045 Uiso 1 1 calc GR . . . .
C11 C 0.2580(3) 0.3560(4) 0.4988(2) 0.0206(8) Uani 1 1 d . . . . .
H11 H 0.215280 0.291950 0.481641 0.025 Uiso 1 1 calc R . . . .
C3 C 0.5389(3) 0.8068(5) 0.7165(3) 0.0277(10) Uani 1 1 d . . . . .
H3 H 0.511538 0.877688 0.732420 0.033 Uiso 1 1 calc R . . . .
C23 C 0.4339(3) 0.0704(5) 0.8179(3) 0.0266(9) Uani 1 1 d . . . . .
H23 H 0.457775 -0.012238 0.835260 0.032 Uiso 1 1 calc R . . . .
C28 C 0.4535(3) 0.6600(5) 0.8513(3) 0.0272(9) Uani 1 1 d . . . . .
C29 C 0.3923(3) 0.6377(5) 0.8880(3) 0.0345(11) Uani 1 1 d . . . . .
H29 H 0.336129 0.618253 0.857777 0.041 Uiso 1 1 calc R . . . .
C33 C 0.5358(4) 0.6868(5) 0.8953(3) 0.0346(11) Uani 1 1 d . . . . .
H33 H 0.578146 0.698173 0.870627 0.042 Uiso 1 1 calc R . . . .
C27 C 0.3205(3) 0.0217(6) 0.8788(3) 0.0376(12) Uani 1 1 d . . . . .
H27A H 0.354818 0.022536 0.934010 0.056 Uiso 1 1 calc GR . . . .
H27B H 0.316834 -0.067386 0.858487 0.056 Uiso 1 1 calc GR . . . .
H27C H 0.263901 0.053671 0.874090 0.056 Uiso 1 1 calc GR . . . .
C20 C 0.6842(4) 0.0117(5) 0.5026(3) 0.0378(12) Uani 1 1 d . . . . .
H20A H 0.731041 0.059219 0.493102 0.057 Uiso 1 1 calc GR . . . .
H20B H 0.643400 -0.012260 0.452322 0.057 Uiso 1 1 calc GR . . . .
H20C H 0.705640 -0.067131 0.532876 0.057 Uiso 1 1 calc GR . . . .
C32 C 0.5551(4) 0.6966(6) 0.9768(3) 0.0439(14) Uani 1 1 d . . . . .
H32 H 0.610556 0.719307 1.007544 0.053 Uiso 1 1 calc R . . . .
C30 C 0.4142(4) 0.6440(6) 0.9688(3) 0.0426(14) Uani 1 1 d . . . . .
H30 H 0.372715 0.627340 0.993957 0.051 Uiso 1 1 calc R . . . .
C31 C 0.4946(4) 0.6738(6) 1.0132(3) 0.0441(14) Uani 1 1 d . . . . .
H31 H 0.508599 0.678663 1.068737 0.053 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb 0.01384(11) 0.01633(12) 0.01280(11) 0.00047(9) 0.00249(8) -0.00111(9)
Br 0.01936(18) 0.0256(2) 0.01588(18) 0.00027(15) 0.00079(14) -0.00069(15)
S 0.0274(5) 0.0271(5) 0.0243(5) -0.0025(4) 0.0116(4) 0.0001(4)
C5 0.024(2) 0.034(2) 0.0174(19) 0.0011(17) 0.0033(16) -0.0117(18)
C1 0.0180(17) 0.0168(17) 0.0123(16) 0.0011(13) 0.0008(13) -0.0023(14)
C14 0.0183(17) 0.0151(17) 0.0165(17) 0.0012(14) 0.0054(14) 0.0001(14)
C21 0.0180(18) 0.0219(19) 0.0120(17) 0.0005(14) 0.0036(14) -0.0019(14)
C15 0.0190(18) 0.023(2) 0.0181(18) -0.0010(15) 0.0043(15) -0.0011(15)
C18 0.0233(19) 0.023(2) 0.023(2) 0.0036(16) 0.0077(16) 0.0078(16)
C10 0.0203(19) 0.025(2) 0.0149(18) -0.0026(15) 0.0006(15) 0.0024(16)
C7 0.0137(16) 0.0199(18) 0.0111(15) 0.0007(13) 0.0009(13) 0.0014(13)
C6 0.0179(18) 0.024(2) 0.0220(19) 0.0005(16) 0.0051(15) -0.0026(16)
C9 0.031(2) 0.023(2) 0.0134(17) 0.0035(15) -0.0011(16) -0.0031(17)
C19 0.0203(18) 0.0183(18) 0.0159(17) 0.0009(14) 0.0031(14) 0.0006(15)
C8 0.0233(19) 0.0217(19) 0.0130(17) -0.0003(14) -0.0002(15) -0.0055(15)
C16 0.028(2) 0.023(2) 0.0167(18) -0.0044(15) 0.0053(16) -0.0029(16)
C22 0.023(2) 0.024(2) 0.024(2) 0.0007(16) 0.0105(16) -0.0003(16)
C4 0.042(3) 0.023(2) 0.020(2) -0.0005(16) 0.0065(19) -0.0146(19)
C17 0.032(2) 0.0169(19) 0.025(2) 0.0003(16) 0.0108(17) 0.0019(16)
C24 0.026(2) 0.032(2) 0.0209(19) 0.0061(18) 0.0081(16) -0.0069(18)
C26 0.0198(19) 0.024(2) 0.024(2) 0.0013(16) 0.0055(16) 0.0022(16)
C12 0.0183(18) 0.0171(18) 0.0197(18) -0.0003(14) 0.0067(15) -0.0023(14)
C25 0.020(2) 0.033(2) 0.030(2) 0.0007(19) 0.0104(18) -0.0017(17)
C2 0.0238(19) 0.0189(19) 0.0142(17) -0.0013(14) 0.0048(14) -0.0030(15)
C13 0.027(2) 0.030(2) 0.022(2) -0.0023(18) -0.0084(17) 0.0022(18)
C11 0.0180(18) 0.0199(19) 0.0207(19) -0.0034(15) 0.0012(15) -0.0026(14)
C3 0.044(3) 0.021(2) 0.0176(19) -0.0024(16) 0.0084(19) -0.0052(19)
C23 0.029(2) 0.024(2) 0.027(2) 0.0056(17) 0.0089(18) -0.0019(17)
C28 0.040(3) 0.021(2) 0.024(2) -0.0003(17) 0.0150(19) 0.0024(19)
C29 0.037(3) 0.036(3) 0.035(3) -0.002(2) 0.019(2) 0.006(2)
C33 0.046(3) 0.036(3) 0.023(2) -0.003(2) 0.014(2) -0.009(2)
C27 0.035(3) 0.042(3) 0.040(3) 0.013(2) 0.016(2) -0.008(2)
C20 0.046(3) 0.035(3) 0.033(3) -0.005(2) 0.014(2) 0.016(2)
C32 0.056(4) 0.050(3) 0.026(3) -0.011(2) 0.012(2) -0.008(3)
C30 0.062(4) 0.040(3) 0.039(3) 0.002(2) 0.035(3) 0.010(3)
C31 0.070(4) 0.044(3) 0.023(2) -0.004(2) 0.021(3) 0.005(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
Sb Br 2.8960(5) . ?
Sb C1 2.120(4) . ?
Sb C14 2.121(4) . ?
Sb C21 2.114(4) . ?
Sb C7 2.139(4) . ?
S C2 1.768(4) . ?
S C28 1.782(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(6) . ?
C5 C4 1.378(7) . ?
C1 C6 1.390(6) . ?
C1 C2 1.390(6) . ?
C14 C15 1.409(6) . ?
C14 C19 1.394(5) . ?
C21 C22 1.384(6) . ?
C21 C26 1.383(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.377(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.383(6) . ?
C18 C17 1.393(6) . ?
C10 C9 1.382(6) . ?
C10 C13 1.511(6) . ?
C10 C11 1.399(6) . ?
C7 C8 1.392(6) . ?
C7 C12 1.399(5) . ?
C6 H6 0.9500 . ?
C9 H9 0.9500 . ?
C9 C8 1.390(6) . ?
C19 H19 0.9500 . ?
C8 H8 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.392(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.388(6) . ?
C4 H4 0.9500 . ?
C4 C3 1.380(7) . ?
C17 C20 1.512(6) . ?
C24 C25 1.401(7) . ?
C24 C23 1.387(7) . ?
C24 C27 1.501(6) . ?
C26 H26 0.9500 . ?
C26 C25 1.386(6) . ?
C12 H12 0.9500 . ?
C12 C11 1.384(6) . ?
C25 H25 0.9500 . ?
C2 C3 1.398(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C11 H11 0.9500 . ?
C3 H3 0.9500 . ?
C23 H23 0.9500 . ?
C28 C29 1.394(7) . ?
C28 C33 1.386(7) . ?
C29 H29 0.9500 . ?
C29 C30 1.381(8) . ?
C33 H33 0.9500 . ?
C33 C32 1.400(7) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C32 H32 0.9500 . ?
C32 C31 1.381(8) . ?
C30 H30 0.9500 . ?
C30 C31 1.370(9) . ?
C31 H31 0.9500 . ?
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
C1 Sb Br 78.40(10) . . ?
C1 Sb C14 110.21(15) . . ?
C1 Sb C7 95.84(15) . . ?
C14 Sb Br 91.00(11) . . ?
C14 Sb C7 98.72(15) . . ?
C21 Sb Br 81.86(10) . . ?
C21 Sb C1 136.16(15) . . ?
C21 Sb C14 108.88(15) . . ?
C21 Sb C7 97.14(15) . . ?
C7 Sb Br 169.98(11) . . ?
C2 S C28 104.7(2) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.2(4) . . ?
C6 C1 Sb 119.1(3) . . ?
C6 C1 C2 120.3(4) . . ?
C2 C1 Sb 120.3(3) . . ?
C15 C14 Sb 117.3(3) . . ?
C19 C14 Sb 124.3(3) . . ?
C19 C14 C15 118.5(4) . . ?
C22 C21 Sb 117.5(3) . . ?
C26 C21 Sb 122.4(3) . . ?
C26 C21 C22 119.9(4) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 C14 120.3(4) . . ?
C16 C15 H15 119.8 . . ?
C19 C18 H18 119.2 . . ?
C19 C18 C17 121.6(4) . . ?
C17 C18 H18 119.2 . . ?
C9 C10 C13 120.6(4) . . ?
C9 C10 C11 118.4(4) . . ?
C11 C10 C13 120.9(4) . . ?
C8 C7 Sb 120.1(3) . . ?
C8 C7 C12 118.6(4) . . ?
C12 C7 Sb 121.3(3) . . ?
C5 C6 H6 120.2 . . ?
C1 C6 C5 119.5(4) . . ?
C1 C6 H6 120.2 . . ?
C10 C9 H9 119.4 . . ?
C10 C9 C8 121.3(4) . . ?
C8 C9 H9 119.4 . . ?
C14 C19 H19 119.9 . . ?
C18 C19 C14 120.3(4) . . ?
C18 C19 H19 119.9 . . ?
C7 C8 H8 119.8 . . ?
C9 C8 C7 120.4(4) . . ?
C9 C8 H8 119.8 . . ?
C15 C16 H16 119.2 . . ?
C15 C16 C17 121.6(4) . . ?
C17 C16 H16 119.2 . . ?
C21 C22 H22 119.9 . . ?
C21 C22 C23 120.2(4) . . ?
C23 C22 H22 119.9 . . ?
C5 C4 H4 119.7 . . ?
C5 C4 C3 120.6(4) . . ?
C3 C4 H4 119.7 . . ?
C18 C17 C20 121.4(4) . . ?
C16 C17 C18 117.8(4) . . ?
C16 C17 C20 120.8(4) . . ?
C25 C24 C27 121.4(4) . . ?
C23 C24 C25 118.0(4) . . ?
C23 C24 C27 120.6(5) . . ?
C21 C26 H26 120.2 . . ?
C21 C26 C25 119.5(4) . . ?
C25 C26 H26 120.2 . . ?
C7 C12 H12 119.7 . . ?
C11 C12 C7 120.6(4) . . ?
C11 C12 H12 119.7 . . ?
C24 C25 H25 119.3 . . ?
C26 C25 C24 121.4(4) . . ?
C26 C25 H25 119.3 . . ?
C1 C2 S 119.0(3) . . ?
C1 C2 C3 119.6(4) . . ?
C3 C2 S 121.3(3) . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C11 H11 119.6 . . ?
C12 C11 C10 120.7(4) . . ?
C12 C11 H11 119.6 . . ?
C4 C3 C2 119.8(4) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C22 C23 H23 119.6 . . ?
C24 C23 C22 120.9(4) . . ?
C24 C23 H23 119.6 . . ?
C29 C28 S 115.8(4) . . ?
C33 C28 S 123.8(4) . . ?
C33 C28 C29 120.4(5) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 C28 119.4(5) . . ?
C30 C29 H29 120.3 . . ?
C28 C33 H33 120.7 . . ?
C28 C33 C32 118.6(5) . . ?
C32 C33 H33 120.7 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C33 C32 H32 119.6 . . ?
C31 C32 C33 120.8(6) . . ?
C31 C32 H32 119.6 . . ?
C29 C30 H30 119.5 . . ?
C31 C30 C29 121.1(5) . . ?
C31 C30 H30 119.5 . . ?
C32 C31 H31 120.2 . . ?
C30 C31 C32 119.6(5) . . ?
C30 C31 H31 120.2 . . ?
_shelx_res_file
;
TITL ssptol_br_0m_a.res in P2(1)/n
phssb(ptol)3br.res
created by SHELXL-2018/3 at 17:06:39 on 22-Jun-2020
REM Old TITL ssptol_br_0m in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.096, Rweak 0.005, Alpha 0.037, Orientation as input
REM Formula found by SHELXT: C33 Br S Sb
CELL 0.71073 16.7041 10.2829 17.9121 90 107.86 90
ZERR 4 0.0012 0.0007 0.0013 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Br S Sb
UNIT 132 120 4 4 4
L.S. 10
PLAN 1
SIZE 0.323 0.2515 0.1585
TEMP -163.15
BOND $H
LIST 6
fmap 2
acta
REM
REM
REM
WGHT 0.028800 16.456699
FVAR 0.27021
SB 5 0.499666 0.386342 0.687295 11.00000 0.01384 0.01633 =
0.01280 0.00047 0.00249 -0.00111
BR 3 0.637017 0.373351 0.832511 11.00000 0.01936 0.02558 =
0.01588 0.00027 0.00079 -0.00069
S 4 0.418917 0.648051 0.747007 11.00000 0.02736 0.02714 =
0.02434 -0.00253 0.01162 0.00005
C5 1 0.647241 0.726673 0.666612 11.00000 0.02363 0.03427 =
0.01736 0.00113 0.00326 -0.01172
AFIX 43
H5 2 0.694429 0.742866 0.648929 11.00000 -1.20000
AFIX 0
C1 1 0.549620 0.577090 0.694577 11.00000 0.01796 0.01678 =
0.01233 0.00106 0.00080 -0.00229
C14 1 0.564323 0.260561 0.631499 11.00000 0.01831 0.01513 =
0.01648 0.00117 0.00543 0.00008
C21 1 0.439251 0.273113 0.752649 11.00000 0.01799 0.02192 =
0.01201 0.00051 0.00359 -0.00191
C15 1 0.522572 0.225209 0.553215 11.00000 0.01898 0.02320 =
0.01811 -0.00096 0.00434 -0.00110
AFIX 43
H15 2 0.467593 0.257241 0.527831 11.00000 -1.20000
AFIX 0
C18 1 0.682917 0.132375 0.625550 11.00000 0.02325 0.02281 =
0.02327 0.00360 0.00771 0.00775
AFIX 43
H18 2 0.737983 0.100368 0.650589 11.00000 -1.20000
AFIX 0
C10 1 0.251206 0.472991 0.457363 11.00000 0.02034 0.02535 =
0.01490 -0.00256 0.00062 0.00244
C7 1 0.390895 0.424115 0.589384 11.00000 0.01370 0.01991 =
0.01111 0.00072 0.00089 0.00135
C6 1 0.618186 0.600020 0.667894 11.00000 0.01794 0.02439 =
0.02203 0.00053 0.00514 -0.00258
AFIX 43
H6 2 0.645031 0.529812 0.650658 11.00000 -1.20000
AFIX 0
C9 1 0.314816 0.563696 0.482864 11.00000 0.03070 0.02271 =
0.01339 0.00348 -0.00115 -0.00313
AFIX 43
H9 2 0.310907 0.643792 0.455544 11.00000 -1.20000
AFIX 0
C19 1 0.645280 0.212912 0.666855 11.00000 0.02028 0.01829 =
0.01594 0.00094 0.00305 0.00055
AFIX 43
H19 2 0.674704 0.235847 0.719513 11.00000 -1.20000
AFIX 0
C8 1 0.384407 0.539971 0.547726 11.00000 0.02329 0.02174 =
0.01304 -0.00030 -0.00018 -0.00554
AFIX 43
H8 2 0.427795 0.603184 0.563721 11.00000 -1.20000
AFIX 0
C16 1 0.561074 0.144467 0.513339 11.00000 0.02840 0.02297 =
0.01673 -0.00435 0.00535 -0.00293
AFIX 43
H16 2 0.531704 0.120533 0.460842 11.00000 -1.20000
AFIX 0
C22 1 0.473282 0.152381 0.778401 11.00000 0.02286 0.02402 =
0.02449 0.00068 0.01046 -0.00033
AFIX 43
H22 2 0.523759 0.125492 0.769023 11.00000 -1.20000
AFIX 0
C4 1 0.607755 0.828600 0.690915 11.00000 0.04210 0.02253 =
0.02022 -0.00049 0.00646 -0.01462
AFIX 43
H4 2 0.628081 0.914691 0.690038 11.00000 -1.20000
AFIX 0
C17 1 0.642010 0.097073 0.548117 11.00000 0.03198 0.01693 =
0.02476 0.00028 0.01077 0.00190
C24 1 0.360195 0.107723 0.832290 11.00000 0.02571 0.03165 =
0.02089 0.00607 0.00809 -0.00690
C26 1 0.364624 0.311085 0.764513 11.00000 0.01983 0.02399 =
0.02352 0.00130 0.00546 0.00218
AFIX 43
H26 2 0.339848 0.392349 0.745062 11.00000 -1.20000
AFIX 0
C12 1 0.326147 0.332618 0.564359 11.00000 0.01832 0.01708 =
0.01969 -0.00028 0.00669 -0.00229
AFIX 43
H12 2 0.329028 0.253727 0.592664 11.00000 -1.20000
AFIX 0
C25 1 0.326269 0.229698 0.804985 11.00000 0.02023 0.03255 =
0.02970 0.00075 0.01042 -0.00169
AFIX 43
H25 2 0.275930 0.257186 0.814408 11.00000 -1.20000
AFIX 0
C2 1 0.509694 0.679898 0.718991 11.00000 0.02383 0.01889 =
0.01417 -0.00127 0.00476 -0.00301
C13 1 0.175980 0.500176 0.386673 11.00000 0.02711 0.02998 =
0.02211 -0.00229 -0.00839 0.00219
AFIX 137
H13A 2 0.124888 0.501856 0.402650 11.00000 -1.50000
H13B 2 0.171070 0.431762 0.347428 11.00000 -1.50000
H13C 2 0.183207 0.584535 0.364105 11.00000 -1.50000
AFIX 0
C11 1 0.257973 0.356018 0.498763 11.00000 0.01801 0.01988 =
0.02071 -0.00340 0.00121 -0.00262
AFIX 43
H11 2 0.215280 0.291950 0.481641 11.00000 -1.20000
AFIX 0
C3 1 0.538941 0.806760 0.716523 11.00000 0.04360 0.02132 =
0.01756 -0.00241 0.00836 -0.00522
AFIX 43
H3 2 0.511538 0.877688 0.732420 11.00000 -1.20000
AFIX 0
C23 1 0.433917 0.070445 0.817881 11.00000 0.02889 0.02411 =
0.02705 0.00558 0.00894 -0.00191
AFIX 43
H23 2 0.457775 -0.012238 0.835260 11.00000 -1.20000
AFIX 0
C28 1 0.453471 0.660025 0.851272 11.00000 0.03986 0.02147 =
0.02389 -0.00031 0.01503 0.00243
C29 1 0.392324 0.637657 0.888021 11.00000 0.03719 0.03642 =
0.03506 -0.00159 0.01853 0.00622
AFIX 43
H29 2 0.336129 0.618253 0.857777 11.00000 -1.20000
AFIX 0
C33 1 0.535756 0.686767 0.895303 11.00000 0.04630 0.03644 =
0.02303 -0.00296 0.01358 -0.00857
AFIX 43
H33 2 0.578146 0.698173 0.870627 11.00000 -1.20000
AFIX 0
C27 1 0.320490 0.021665 0.878753 11.00000 0.03470 0.04183 =
0.03976 0.01275 0.01635 -0.00822
AFIX 137
H27A 2 0.354818 0.022536 0.934010 11.00000 -1.50000
H27B 2 0.316834 -0.067386 0.858487 11.00000 -1.50000
H27C 2 0.263901 0.053671 0.874090 11.00000 -1.50000
AFIX 0
C20 1 0.684236 0.011720 0.502602 11.00000 0.04625 0.03513 =
0.03318 -0.00482 0.01370 0.01569
AFIX 137
H20A 2 0.731041 0.059219 0.493102 11.00000 -1.50000
H20B 2 0.643400 -0.012260 0.452322 11.00000 -1.50000
H20C 2 0.705640 -0.067131 0.532876 11.00000 -1.50000
AFIX 0
C32 1 0.555098 0.696615 0.976849 11.00000 0.05576 0.04967 =
0.02615 -0.01104 0.01227 -0.00771
AFIX 43
H32 2 0.610556 0.719307 1.007544 11.00000 -1.20000
AFIX 0
C30 1 0.414150 0.643951 0.968804 11.00000 0.06246 0.03979 =
0.03893 0.00204 0.03510 0.00995
AFIX 43
H30 2 0.372715 0.627340 0.993957 11.00000 -1.20000
AFIX 0
C31 1 0.494562 0.673753 1.013247 11.00000 0.06966 0.04422 =
0.02269 -0.00387 0.02059 0.00514
AFIX 43
H31 2 0.508599 0.678663 1.068737 11.00000 -1.20000
AFIX 0
HKLF 4
REM ssptol_br_0m_a.res in P2(1)/n
REM wR2 = 0.1207, GooF = S = 1.160, Restrained GooF = 1.160 for all data
REM R1 = 0.0490 for 7431 Fo > 4sig(Fo) and 0.0698 for all 9366 data
REM 328 parameters refined using 0 restraints
END
WGHT 0.0288 16.4573
REM Highest difference peak 1.672, deepest hole -1.284, 1-sigma level 0.156
Q1 1 0.4605 0.9719 0.6923 11.00000 0.05 1.67
;
_shelx_res_checksum 44904
_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_phssb(ptol)3bf4
_database_code_depnum_ccdc_archive 'CCDC 2021710'
loop_
_audit_author_name
_audit_author_address
'Gyeongjin Park'
;Texas AM university
United States of America
;
_audit_update_record
;
2020-08-05 deposited with the CCDC. 2020-08-28 downloaded from the CCDC.
;
_audit_creation_date 2020-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C33 H30 S Sb, B F4'
_chemical_formula_sum 'C33 H30 B F4 S Sb'
_chemical_formula_weight 667.19
_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'
F F 0.0171 0.0103 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 20.555
_cell_length_b 12.162
_cell_length_c 24.558
_cell_angle_alpha 90
_cell_angle_beta 101.94
_cell_angle_gamma 90
_cell_volume 6006.3
_cell_formula_units_Z 8
_cell_measurement_reflns_used 9274
_cell_measurement_temperature 110
_cell_measurement_theta_max 30.493
_cell_measurement_theta_min 2.213
_shelx_estimated_absorpt_T_max 0.848
_shelx_estimated_absorpt_T_min 0.766
_exptl_absorpt_coefficient_mu 1.034
_exptl_absorpt_correction_T_max 0.7461
_exptl_absorpt_correction_T_min 0.6682
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0931 before and 0.0526 after correction. The Ratio of minimum to maximum transmission is 0.8956. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.476
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2688
_exptl_crystal_size_max 0.272
_exptl_crystal_size_mid 0.1781
_exptl_crystal_size_min 0.1649
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0421
_diffrn_reflns_av_unetI/netI 0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 35
_diffrn_reflns_limit_l_min -35
_diffrn_reflns_number 113069
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.549
_diffrn_reflns_theta_min 1.957
_diffrn_ambient_temperature 110.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7998
_reflns_number_total 9135
_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 V8.38A (?, 2016)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max 0.437
_refine_diff_density_min -0.351
_refine_diff_density_rms 0.063
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 364
_refine_ls_number_reflns 9135
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0298
_refine_ls_R_factor_gt 0.0219
_refine_ls_restrained_S_all 1.062
_refine_ls_shift/su_max 0.006
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0182P)^2^+6.4468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0465
_refine_ls_wR_factor_ref 0.0499
_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:
C3(H3), C5(H5), C6(H6), C4(H4), C22(H22), C12(H12), C8(H8), C11(H11),
C26(H26), C9(H9), C25(H25), C19(H19), C15(H15), C23(H23), C16(H16), C33(H33),
C18(H18), C29(H29), C32(H32), C31(H31), C30(H30)
2.b Idealised Me refined as rotating group:
C27(H27A,H27B,H27C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_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
Sb Sb 0.56243(2) 0.61126(2) 0.61790(2) 0.01606(3) Uani 1 1 d . . . . .
S S 0.71321(2) 0.50650(3) 0.65492(2) 0.02250(7) Uani 1 1 d . . . . .
F4 F 0.62389(4) 0.82161(7) 0.60513(4) 0.02588(18) Uani 1 1 d . . . . .
F1 F 0.63117(5) 0.93155(9) 0.53231(4) 0.0356(2) Uani 1 1 d . . . . .
F3 F 0.59174(5) 1.00035(8) 0.60487(4) 0.0333(2) Uani 1 1 d . . . . .
F2 F 0.70185(5) 0.95640(9) 0.61583(5) 0.0397(2) Uani 1 1 d . . . . .
C1 C 0.63216(7) 0.60440(11) 0.56607(6) 0.0179(2) Uani 1 1 d . . . . .
C3 C 0.74360(7) 0.56816(13) 0.55432(7) 0.0257(3) Uani 1 1 d . . . . .
H3 H 0.787260 0.541470 0.568500 0.031 Uiso 1 1 calc R . . . .
C21 C 0.58591(7) 0.68541(12) 0.69669(6) 0.0190(3) Uani 1 1 d . . . . .
C7 C 0.47689(7) 0.68155(11) 0.56809(6) 0.0179(2) Uani 1 1 d . . . . .
C14 C 0.53082(7) 0.45169(11) 0.63207(6) 0.0178(2) Uani 1 1 d . . . . .
C2 C 0.69596(7) 0.56492(11) 0.58731(6) 0.0197(3) Uani 1 1 d . . . . .
C5 C 0.66319(8) 0.64827(13) 0.47958(6) 0.0264(3) Uani 1 1 d . . . . .
H5 H 0.652124 0.676006 0.442651 0.032 Uiso 1 1 calc R . . . .
C24 C 0.61669(7) 0.78314(13) 0.80163(6) 0.0241(3) Uani 1 1 d . . . . .
C6 C 0.61525(7) 0.64587(12) 0.51198(6) 0.0218(3) Uani 1 1 d . . . . .
H6 H 0.571557 0.672107 0.497533 0.026 Uiso 1 1 calc R . . . .
C4 C 0.72710(8) 0.61046(13) 0.50073(7) 0.0289(3) Uani 1 1 d . . . . .
H4 H 0.759723 0.613523 0.478435 0.035 Uiso 1 1 calc R . . . .
C22 C 0.61695(8) 0.62413(12) 0.74267(6) 0.0236(3) Uani 1 1 d . . . . .
H22 H 0.627626 0.549024 0.738472 0.028 Uiso 1 1 calc R . . . .
C12 C 0.47572(7) 0.78745(12) 0.54602(6) 0.0221(3) Uani 1 1 d . . . . .
H12 H 0.513422 0.833998 0.556024 0.026 Uiso 1 1 calc R . . . .
C8 C 0.42087(7) 0.61494(12) 0.55397(6) 0.0196(3) Uani 1 1 d . . . . .
H8 H 0.420914 0.543386 0.569495 0.023 Uiso 1 1 calc R . . . .
C11 C 0.41924(7) 0.82452(13) 0.50939(6) 0.0232(3) Uani 1 1 d . . . . .
H11 H 0.418560 0.896942 0.494795 0.028 Uiso 1 1 calc R . . . .
C26 C 0.56919(7) 0.79466(12) 0.70292(6) 0.0235(3) Uani 1 1 d . . . . .
H26 H 0.547303 0.836203 0.671709 0.028 Uiso 1 1 calc R . . . .
C9 C 0.36464(7) 0.65347(12) 0.51696(6) 0.0214(3) Uani 1 1 d . . . . .
H9 H 0.326493 0.607733 0.507575 0.026 Uiso 1 1 calc R . . . .
C25 C 0.58484(8) 0.84230(13) 0.75528(6) 0.0255(3) Uani 1 1 d . . . . .
H25 H 0.573553 0.917091 0.759591 0.031 Uiso 1 1 calc R . . . .
C19 C 0.49069(8) 0.43637(13) 0.67077(6) 0.0259(3) Uani 1 1 d . . . . .
H19 H 0.480084 0.496915 0.691782 0.031 Uiso 1 1 calc R . . . .
C17 C 0.48151(8) 0.24243(13) 0.64869(7) 0.0275(3) Uani 1 1 d . . . . .
C28 C 0.76261(7) 0.60871(12) 0.69600(6) 0.0212(3) Uani 1 1 d . . . . .
C15 C 0.54621(7) 0.36228(12) 0.60177(6) 0.0203(3) Uani 1 1 d . . . . .
H15 H 0.573315 0.372129 0.575154 0.024 Uiso 1 1 calc R . . . .
C23 C 0.63218(8) 0.67370(14) 0.79472(6) 0.0265(3) Uani 1 1 d . . . . .
H23 H 0.653532 0.632002 0.826064 0.032 Uiso 1 1 calc R . . . .
C16 C 0.52191(8) 0.25848(12) 0.61045(6) 0.0246(3) Uani 1 1 d . . . . .
H16 H 0.533083 0.197602 0.589938 0.030 Uiso 1 1 calc R . . . .
C33 C 0.76120(7) 0.71875(13) 0.68080(6) 0.0246(3) Uani 1 1 d . . . . .
H33 H 0.735144 0.742208 0.646188 0.030 Uiso 1 1 calc R . . . .
C10 C 0.36358(7) 0.75755(13) 0.49365(6) 0.0216(3) Uani 1 1 d . . . . .
C27 C 0.63447(9) 0.83768(15) 0.85774(7) 0.0337(4) Uani 1 1 d . . . . .
H27A H 0.675517 0.880129 0.860282 0.051 Uiso 1 1 calc GR . . . .
H27B H 0.641113 0.781445 0.886951 0.051 Uiso 1 1 calc GR . . . .
H27C H 0.598370 0.886994 0.862541 0.051 Uiso 1 1 calc GR . . . .
C18 C 0.46623(8) 0.33223(14) 0.67855(7) 0.0307(3) Uani 1 1 d . . . . .
H18 H 0.438588 0.322406 0.704746 0.037 Uiso 1 1 calc R . . . .
C29 C 0.80056(8) 0.57384(14) 0.74693(6) 0.0263(3) Uani 1 1 d . . . . .
H29 H 0.801254 0.498432 0.757123 0.032 Uiso 1 1 calc R . . . .
C13 C 0.30437(8) 0.79621(15) 0.45092(7) 0.0315(3) Uani 1 1 d . . . . .
H13A H 0.292056 0.870574 0.460387 0.047 Uiso 1 1 calc GR . . . .
H13B H 0.266865 0.746247 0.450531 0.047 Uiso 1 1 calc GR . . . .
H13C H 0.315704 0.796919 0.414074 0.047 Uiso 1 1 calc GR . . . .
C32 C 0.79844(8) 0.79421(13) 0.71693(7) 0.0281(3) Uani 1 1 d . . . . .
H32 H 0.797777 0.869709 0.706914 0.034 Uiso 1 1 calc R . . . .
C31 C 0.83659(8) 0.76005(14) 0.76756(7) 0.0299(3) Uani 1 1 d . . . . .
H31 H 0.862200 0.811934 0.791904 0.036 Uiso 1 1 calc R . . . .
C30 C 0.83719(8) 0.65016(15) 0.78246(7) 0.0307(3) Uani 1 1 d . . . . .
H30 H 0.862897 0.626986 0.817266 0.037 Uiso 1 1 calc R . . . .
B B 0.63779(8) 0.92901(14) 0.58969(7) 0.0226(3) Uani 1 1 d . . . . .
C20 C 0.45545(11) 0.12937(15) 0.65753(10) 0.0459(5) Uani 1 1 d . . . . .
H20A H 0.436435 0.096087 0.621406 0.069 Uiso 1 1 calc GR . . . .
H20B H 0.421025 0.135156 0.679670 0.069 Uiso 1 1 calc GR . . . .
H20C H 0.491957 0.083382 0.677278 0.069 Uiso 1 1 calc GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb 0.01451(4) 0.01714(4) 0.01635(4) 0.00071(3) 0.00274(3) 0.00116(3)
S 0.01849(16) 0.01912(16) 0.02840(18) 0.00241(13) 0.00138(13) 0.00089(12)
F4 0.0267(4) 0.0181(4) 0.0321(5) 0.0028(3) 0.0045(4) -0.0007(3)
F1 0.0407(6) 0.0403(6) 0.0279(5) 0.0086(4) 0.0119(4) 0.0124(5)
F3 0.0384(5) 0.0246(5) 0.0379(5) -0.0034(4) 0.0100(4) 0.0086(4)
F2 0.0262(5) 0.0329(5) 0.0543(7) 0.0081(5) -0.0050(4) -0.0079(4)
C1 0.0165(6) 0.0169(6) 0.0207(6) -0.0018(5) 0.0048(5) -0.0016(5)
C3 0.0182(6) 0.0240(7) 0.0363(8) -0.0051(6) 0.0092(6) -0.0025(5)
C21 0.0186(6) 0.0209(6) 0.0175(6) -0.0001(5) 0.0036(5) -0.0005(5)
C7 0.0150(6) 0.0203(6) 0.0183(6) 0.0002(5) 0.0031(5) 0.0026(5)
C14 0.0163(6) 0.0188(6) 0.0177(6) 0.0022(5) 0.0021(5) -0.0003(5)
C2 0.0182(6) 0.0167(6) 0.0242(7) -0.0031(5) 0.0043(5) -0.0021(5)
C5 0.0336(8) 0.0252(7) 0.0230(7) -0.0014(6) 0.0113(6) -0.0063(6)
C24 0.0219(7) 0.0303(8) 0.0212(7) -0.0034(6) 0.0071(5) -0.0086(6)
C6 0.0225(7) 0.0211(6) 0.0218(7) -0.0004(5) 0.0049(5) -0.0020(5)
C4 0.0291(8) 0.0271(7) 0.0352(8) -0.0060(7) 0.0177(7) -0.0075(6)
C22 0.0267(7) 0.0214(7) 0.0224(7) 0.0019(5) 0.0044(5) 0.0012(5)
C12 0.0188(6) 0.0219(7) 0.0249(7) 0.0030(5) 0.0030(5) -0.0022(5)
C8 0.0194(6) 0.0180(6) 0.0209(6) -0.0011(5) 0.0031(5) 0.0016(5)
C11 0.0210(7) 0.0243(7) 0.0245(7) 0.0065(6) 0.0049(5) 0.0014(5)
C26 0.0251(7) 0.0229(7) 0.0225(7) 0.0008(5) 0.0049(5) 0.0032(6)
C9 0.0171(6) 0.0229(7) 0.0233(7) -0.0015(5) 0.0022(5) -0.0006(5)
C25 0.0270(7) 0.0230(7) 0.0273(7) -0.0038(6) 0.0076(6) -0.0013(6)
C19 0.0258(7) 0.0280(8) 0.0264(7) -0.0021(6) 0.0113(6) -0.0006(6)
C17 0.0267(7) 0.0256(7) 0.0295(8) 0.0069(6) 0.0039(6) -0.0046(6)
C28 0.0150(6) 0.0236(7) 0.0244(7) 0.0000(6) 0.0024(5) 0.0017(5)
C15 0.0214(6) 0.0213(6) 0.0186(6) 0.0033(5) 0.0053(5) 0.0026(5)
C23 0.0282(8) 0.0309(8) 0.0193(7) 0.0038(6) 0.0026(6) -0.0016(6)
C16 0.0280(7) 0.0215(7) 0.0236(7) 0.0011(5) 0.0036(6) -0.0001(6)
C33 0.0209(7) 0.0240(7) 0.0260(7) 0.0004(6) -0.0018(5) 0.0025(6)
C10 0.0172(6) 0.0281(7) 0.0193(6) 0.0021(5) 0.0031(5) 0.0036(5)
C27 0.0389(9) 0.0397(9) 0.0229(7) -0.0067(7) 0.0078(7) -0.0148(8)
C18 0.0288(8) 0.0346(9) 0.0323(8) 0.0054(7) 0.0147(6) -0.0047(7)
C29 0.0227(7) 0.0275(7) 0.0275(7) 0.0070(6) 0.0025(6) 0.0019(6)
C13 0.0210(7) 0.0402(9) 0.0300(8) 0.0096(7) -0.0021(6) 0.0023(6)
C32 0.0262(7) 0.0229(7) 0.0331(8) -0.0023(6) 0.0010(6) 0.0007(6)
C31 0.0257(8) 0.0347(9) 0.0272(8) -0.0066(6) 0.0004(6) -0.0011(6)
C30 0.0264(8) 0.0401(9) 0.0231(7) 0.0028(7) -0.0003(6) 0.0017(7)
B 0.0216(7) 0.0194(7) 0.0266(8) 0.0020(6) 0.0046(6) 0.0009(6)
C20 0.0536(12) 0.0299(9) 0.0578(13) 0.0078(8) 0.0203(10) -0.0125(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
Sb C1 2.1060(13) . ?
Sb C21 2.0986(14) . ?
Sb C7 2.1044(13) . ?
Sb C14 2.0983(14) . ?
S C2 1.7731(15) . ?
S C28 1.7805(15) . ?
F4 B 1.4058(19) . ?
F1 B 1.388(2) . ?
F3 B 1.3905(19) . ?
F2 B 1.3811(19) . ?
C1 C2 1.3926(19) . ?
C1 C6 1.3960(19) . ?
C3 H3 0.9500 . ?
C3 C2 1.395(2) . ?
C3 C4 1.388(2) . ?
C21 C22 1.393(2) . ?
C21 C26 1.389(2) . ?
C7 C12 1.396(2) . ?
C7 C8 1.3920(19) . ?
C14 C19 1.394(2) . ?
C14 C15 1.3906(19) . ?
C5 H5 0.9500 . ?
C5 C6 1.389(2) . ?
C5 C4 1.387(2) . ?
C24 C25 1.391(2) . ?
C24 C23 1.387(2) . ?
C24 C27 1.505(2) . ?
C6 H6 0.9500 . ?
C4 H4 0.9500 . ?
C22 H22 0.9500 . ?
C22 C23 1.389(2) . ?
C12 H12 0.9500 . ?
C12 C11 1.389(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.3952(19) . ?
C11 H11 0.9500 . ?
C11 C10 1.392(2) . ?
C26 H26 0.9500 . ?
C26 C25 1.386(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.388(2) . ?
C25 H25 0.9500 . ?
C19 H19 0.9500 . ?
C19 C18 1.390(2) . ?
C17 C16 1.390(2) . ?
C17 C18 1.387(2) . ?
C17 C20 1.508(2) . ?
C28 C33 1.388(2) . ?
C28 C29 1.396(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.390(2) . ?
C23 H23 0.9500 . ?
C16 H16 0.9500 . ?
C33 H33 0.9500 . ?
C33 C32 1.391(2) . ?
C10 C13 1.508(2) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C18 H18 0.9500 . ?
C29 H29 0.9500 . ?
C29 C30 1.385(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C32 H32 0.9500 . ?
C32 C31 1.389(2) . ?
C31 H31 0.9500 . ?
C31 C30 1.385(2) . ?
C30 H30 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 Sb C1 121.25(5) . . ?
C21 Sb C7 111.50(5) . . ?
C7 Sb C1 104.83(5) . . ?
C14 Sb C1 109.66(5) . . ?
C14 Sb C21 105.34(5) . . ?
C14 Sb C7 102.83(5) . . ?
C2 S C28 103.36(7) . . ?
C2 C1 Sb 119.55(10) . . ?
C2 C1 C6 120.70(13) . . ?
C6 C1 Sb 119.62(10) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C4 C3 C2 119.87(14) . . ?
C22 C21 Sb 119.80(10) . . ?
C26 C21 Sb 119.86(10) . . ?
C26 C21 C22 120.32(13) . . ?
C12 C7 Sb 123.08(10) . . ?
C8 C7 Sb 117.20(10) . . ?
C8 C7 C12 119.57(13) . . ?
C19 C14 Sb 118.95(11) . . ?
C15 C14 Sb 121.45(10) . . ?
C15 C14 C19 119.51(13) . . ?
C1 C2 S 118.63(11) . . ?
C1 C2 C3 119.53(14) . . ?
C3 C2 S 121.79(11) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C4 C5 C6 120.50(15) . . ?
C25 C24 C27 120.38(15) . . ?
C23 C24 C25 118.51(14) . . ?
C23 C24 C27 121.11(15) . . ?
C1 C6 H6 120.4 . . ?
C5 C6 C1 119.10(14) . . ?
C5 C6 H6 120.4 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.29(14) . . ?
C5 C4 H4 119.9 . . ?
C21 C22 H22 120.3 . . ?
C23 C22 C21 119.48(14) . . ?
C23 C22 H22 120.3 . . ?
C7 C12 H12 120.1 . . ?
C11 C12 C7 119.74(13) . . ?
C11 C12 H12 120.1 . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.86(13) . . ?
C9 C8 H8 120.1 . . ?
C12 C11 H11 119.4 . . ?
C12 C11 C10 121.25(14) . . ?
C10 C11 H11 119.4 . . ?
C21 C26 H26 120.4 . . ?
C25 C26 C21 119.14(14) . . ?
C25 C26 H26 120.4 . . ?
C8 C9 H9 119.5 . . ?
C10 C9 C8 121.02(13) . . ?
C10 C9 H9 119.5 . . ?
C24 C25 H25 119.2 . . ?
C26 C25 C24 121.52(14) . . ?
C26 C25 H25 119.2 . . ?
C14 C19 H19 120.1 . . ?
C18 C19 C14 119.82(14) . . ?
C18 C19 H19 120.1 . . ?
C16 C17 C20 120.34(16) . . ?
C18 C17 C16 118.60(14) . . ?
C18 C17 C20 121.05(15) . . ?
C33 C28 S 122.89(11) . . ?
C33 C28 C29 120.70(14) . . ?
C29 C28 S 116.30(12) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 119.95(13) . . ?
C16 C15 H15 120.0 . . ?
C24 C23 C22 121.01(14) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C17 C16 C15 120.99(14) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C28 C33 H33 120.4 . . ?
C28 C33 C32 119.11(14) . . ?
C32 C33 H33 120.4 . . ?
C11 C10 C13 120.61(14) . . ?
C9 C10 C11 118.51(13) . . ?
C9 C10 C13 120.86(14) . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C19 C18 H18 119.4 . . ?
C17 C18 C19 121.12(14) . . ?
C17 C18 H18 119.4 . . ?
C28 C29 H29 120.3 . . ?
C30 C29 C28 119.41(15) . . ?
C30 C29 H29 120.3 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C33 C32 H32 119.7 . . ?
C31 C32 C33 120.52(15) . . ?
C31 C32 H32 119.7 . . ?
C32 C31 H31 120.1 . . ?
C30 C31 C32 119.83(15) . . ?
C30 C31 H31 120.1 . . ?
C29 C30 C31 120.42(15) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
F1 B F4 108.17(13) . . ?
F1 B F3 109.22(13) . . ?
F3 B F4 108.65(13) . . ?
F2 B F4 109.04(12) . . ?
F2 B F1 110.51(13) . . ?
F2 B F3 111.18(14) . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
_shelx_res_file
;
TITL SbpTolS_0m_a.res in C2/c
phssb(ptol)3bf4.res
created by SHELXL-2018/3 at 11:15:02 on 19-Jun-2020
REM Old TITL Integration of SbpTolS
REM SHELXT solution in C2/c
REM R1 0.052, Rweak 0.003, Alpha 0.033, Orientation as input
REM Formula found by SHELXT: C33 B Cl F4 Sb
CELL 0.71073 20.5548 12.1617 24.5585 90 101.941 90
ZERR 8 0 0 0 0 0 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H B F S Sb
UNIT 264 240 8 32 8 8
L.S. 10
PLAN 1
SIZE 0.272 0.1649 0.1781
TEMP -163.15
BOND $H
LIST 6
fmap 2
acta
OMIT -2 0 2
OMIT 10 0 4
OMIT 7 3 2
OMIT 9 3 3
OMIT 10 2 3
OMIT 9 5 1
OMIT 1 1 5
OMIT -2 2 13
OMIT 1 7 2
OMIT 0 4 5
OMIT -11 1 8
OMIT -5 5 3
OMIT -4 2 14
OMIT 5 1 5
OMIT -12 0 8
OMIT -12 2 2
OMIT -8 2 12
OMIT -14 0 14
OMIT 10 2 6
OMIT 10 2 4
OMIT 12 6 7
OMIT -5 1 4
OMIT 5 5 5
OMIT 4 4 8
OMIT 6 4 5
OMIT 2 6 11
OMIT -1 7 4
OMIT -12 2 11
OMIT 4 6 0
OMIT 15 5 1
OMIT -2 2 12
OMIT 11 3 14
OMIT 15 3 5
OMIT 0 2 10
OMIT -7 5 5
OMIT 0 4 11
OMIT 7 5 3
OMIT 8 0 6
OMIT -1 5 9
OMIT 0 4 4
OMIT -2 4 8
OMIT -8 2 9
OMIT -3 5 5
OMIT 0 2 5
OMIT -2 4 7
OMIT -9 1 2
OMIT 5 3 9
OMIT 2 6 0
OMIT -1 7 1
OMIT -10 0 6
REM
REM
REM
WGHT 0.018200 6.446800
FVAR 0.18084
SB 6 0.562433 0.611257 0.617896 11.00000 0.01451 0.01714 =
0.01635 0.00071 0.00274 0.00116
S 5 0.713211 0.506498 0.654920 11.00000 0.01849 0.01912 =
0.02840 0.00241 0.00138 0.00089
F4 4 0.623889 0.821612 0.605131 11.00000 0.02671 0.01808 =
0.03213 0.00281 0.00446 -0.00069
F1 4 0.631171 0.931549 0.532312 11.00000 0.04070 0.04034 =
0.02785 0.00859 0.01193 0.01238
F3 4 0.591738 1.000345 0.604871 11.00000 0.03837 0.02456 =
0.03793 -0.00341 0.00999 0.00855
F2 4 0.701853 0.956404 0.615830 11.00000 0.02625 0.03288 =
0.05427 0.00808 -0.00498 -0.00794
C1 1 0.632156 0.604402 0.566074 11.00000 0.01646 0.01693 =
0.02068 -0.00183 0.00482 -0.00157
C3 1 0.743604 0.568155 0.554321 11.00000 0.01819 0.02400 =
0.03633 -0.00513 0.00925 -0.00254
AFIX 43
H3 2 0.787260 0.541470 0.568500 11.00000 -1.20000
AFIX 0
C21 1 0.585911 0.685415 0.696686 11.00000 0.01859 0.02088 =
0.01746 -0.00006 0.00364 -0.00053
C7 1 0.476895 0.681550 0.568085 11.00000 0.01505 0.02031 =
0.01828 0.00021 0.00314 0.00264
C14 1 0.530822 0.451693 0.632074 11.00000 0.01627 0.01884 =
0.01765 0.00217 0.00209 -0.00028
C2 1 0.695956 0.564916 0.587307 11.00000 0.01820 0.01668 =
0.02417 -0.00308 0.00432 -0.00213
C5 1 0.663190 0.648268 0.479576 11.00000 0.03359 0.02517 =
0.02296 -0.00144 0.01132 -0.00625
AFIX 43
H5 2 0.652124 0.676006 0.442651 11.00000 -1.20000
AFIX 0
C24 1 0.616685 0.783145 0.801633 11.00000 0.02187 0.03035 =
0.02123 -0.00338 0.00707 -0.00862
C6 1 0.615252 0.645875 0.511984 11.00000 0.02253 0.02109 =
0.02181 -0.00045 0.00487 -0.00196
AFIX 43
H6 2 0.571557 0.672107 0.497533 11.00000 -1.20000
AFIX 0
C4 1 0.727104 0.610456 0.500726 11.00000 0.02912 0.02711 =
0.03516 -0.00599 0.01767 -0.00748
AFIX 43
H4 2 0.759723 0.613523 0.478435 11.00000 -1.20000
AFIX 0
C22 1 0.616951 0.624132 0.742669 11.00000 0.02674 0.02136 =
0.02243 0.00189 0.00440 0.00125
AFIX 43
H22 2 0.627626 0.549024 0.738472 11.00000 -1.20000
AFIX 0
C12 1 0.475724 0.787449 0.546023 11.00000 0.01884 0.02189 =
0.02487 0.00298 0.00304 -0.00225
AFIX 43
H12 2 0.513422 0.833998 0.556024 11.00000 -1.20000
AFIX 0
C8 1 0.420867 0.614937 0.553966 11.00000 0.01938 0.01798 =
0.02088 -0.00105 0.00313 0.00157
AFIX 43
H8 2 0.420914 0.543386 0.569495 11.00000 -1.20000
AFIX 0
C11 1 0.419240 0.824516 0.509393 11.00000 0.02103 0.02425 =
0.02450 0.00646 0.00486 0.00136
AFIX 43
H11 2 0.418560 0.896942 0.494795 11.00000 -1.20000
AFIX 0
C26 1 0.569188 0.794662 0.702922 11.00000 0.02512 0.02287 =
0.02253 0.00076 0.00490 0.00320
AFIX 43
H26 2 0.547303 0.836203 0.671709 11.00000 -1.20000
AFIX 0
C9 1 0.364641 0.653465 0.516960 11.00000 0.01707 0.02293 =
0.02333 -0.00149 0.00218 -0.00065
AFIX 43
H9 2 0.326493 0.607733 0.507575 11.00000 -1.20000
AFIX 0
C25 1 0.584840 0.842303 0.755277 11.00000 0.02703 0.02303 =
0.02727 -0.00381 0.00761 -0.00131
AFIX 43
H25 2 0.573553 0.917091 0.759591 11.00000 -1.20000
AFIX 0
C19 1 0.490692 0.436369 0.670774 11.00000 0.02584 0.02799 =
0.02638 -0.00205 0.01127 -0.00060
AFIX 43
H19 2 0.480084 0.496915 0.691782 11.00000 -1.20000
AFIX 0
C17 1 0.481512 0.242431 0.648689 11.00000 0.02666 0.02556 =
0.02952 0.00686 0.00390 -0.00463
C28 1 0.762608 0.608707 0.696004 11.00000 0.01499 0.02361 =
0.02444 0.00002 0.00244 0.00174
C15 1 0.546214 0.362284 0.601768 11.00000 0.02141 0.02129 =
0.01858 0.00332 0.00529 0.00263
AFIX 43
H15 2 0.573315 0.372129 0.575154 11.00000 -1.20000
AFIX 0
C23 1 0.632179 0.673699 0.794721 11.00000 0.02821 0.03087 =
0.01932 0.00376 0.00255 -0.00158
AFIX 43
H23 2 0.653532 0.632002 0.826064 11.00000 -1.20000
AFIX 0
C16 1 0.521912 0.258482 0.610449 11.00000 0.02803 0.02148 =
0.02362 0.00113 0.00358 -0.00015
AFIX 43
H16 2 0.533083 0.197602 0.589938 11.00000 -1.20000
AFIX 0
C33 1 0.761197 0.718751 0.680805 11.00000 0.02090 0.02404 =
0.02603 0.00039 -0.00178 0.00248
AFIX 43
H33 2 0.735144 0.742208 0.646188 11.00000 -1.20000
AFIX 0
C10 1 0.363581 0.757548 0.493653 11.00000 0.01715 0.02805 =
0.01933 0.00209 0.00310 0.00363
C27 1 0.634472 0.837682 0.857743 11.00000 0.03895 0.03975 =
0.02291 -0.00672 0.00776 -0.01483
AFIX 137
H27A 2 0.675517 0.880129 0.860282 11.00000 -1.50000
H27B 2 0.641113 0.781445 0.886951 11.00000 -1.50000
H27C 2 0.598370 0.886994 0.862541 11.00000 -1.50000
AFIX 0
C18 1 0.466233 0.332232 0.678545 11.00000 0.02878 0.03463 =
0.03233 0.00536 0.01472 -0.00469
AFIX 43
H18 2 0.438588 0.322406 0.704746 11.00000 -1.20000
AFIX 0
C29 1 0.800561 0.573842 0.746929 11.00000 0.02272 0.02751 =
0.02754 0.00697 0.00249 0.00194
AFIX 43
H29 2 0.801254 0.498432 0.757123 11.00000 -1.20000
AFIX 0
C13 1 0.304365 0.796208 0.450919 11.00000 0.02100 0.04023 =
0.03001 0.00959 -0.00210 0.00230
AFIX 137
H13A 2 0.292056 0.870574 0.460387 11.00000 -1.50000
H13B 2 0.266865 0.746247 0.450531 11.00000 -1.50000
H13C 2 0.315704 0.796919 0.414074 11.00000 -1.50000
AFIX 0
C32 1 0.798435 0.794208 0.716934 11.00000 0.02619 0.02295 =
0.03306 -0.00229 0.00099 0.00070
AFIX 43
H32 2 0.797777 0.869709 0.706914 11.00000 -1.20000
AFIX 0
C31 1 0.836588 0.760047 0.767561 11.00000 0.02570 0.03468 =
0.02725 -0.00657 0.00036 -0.00115
AFIX 43
H31 2 0.862200 0.811934 0.791904 11.00000 -1.20000
AFIX 0
C30 1 0.837191 0.650157 0.782456 11.00000 0.02636 0.04010 =
0.02315 0.00278 -0.00031 0.00171
AFIX 43
H30 2 0.862897 0.626986 0.817266 11.00000 -1.20000
AFIX 0
B 3 0.637787 0.929011 0.589691 11.00000 0.02156 0.01944 =
0.02665 0.00203 0.00456 0.00085
C20 1 0.455452 0.129373 0.657535 11.00000 0.05360 0.02994 =
0.05785 0.00784 0.02032 -0.01254
AFIX 137
H20A 2 0.436435 0.096087 0.621406 11.00000 -1.50000
H20B 2 0.421025 0.135156 0.679670 11.00000 -1.50000
H20C 2 0.491957 0.083382 0.677278 11.00000 -1.50000
AFIX 0
HKLF 4
REM SbpTolS_0m_a.res in C2/c
REM wR2 = 0.0499, GooF = S = 1.062, Restrained GooF = 1.062 for all data
REM R1 = 0.0219 for 7998 Fo > 4sig(Fo) and 0.0298 for all 9135 data
REM 364 parameters refined using 0 restraints
END
WGHT 0.0182 6.4468
REM Highest difference peak 0.437, deepest hole -0.351, 1-sigma level 0.063
Q1 1 0.6874 0.9568 0.6434 11.00000 0.05 0.44
;
_shelx_res_checksum 31751
_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_me_2_bf4_0ma
_database_code_depnum_ccdc_archive 'CCDC 2008418'
loop_
_audit_author_name
_audit_author_address
'Gyeongjin Park'
;Texas AM university
United States of America
;
_audit_update_record
;
2020-06-06 deposited with the CCDC. 2020-08-28 downloaded from the CCDC.
;
_audit_creation_date 2020-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic J_Me_BF4
_chemical_formula_moiety 'C62 H54 F S2 Sb2, 2(C H2 Cl2), 3(B F4)'
_chemical_formula_sum 'C64 H58 B3 Cl4 F13 S2 Sb2'
_chemical_formula_weight 1555.95
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 13
_space_group_name_H-M_alt 'P 1 2/n 1'
_space_group_name_Hall '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'
_cell_length_a 15.494(2)
_cell_length_b 10.9891(16)
_cell_length_c 19.761(3)
_cell_angle_alpha 90
_cell_angle_beta 110.566(7)
_cell_angle_gamma 90
_cell_volume 3150.3(8)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9203
_cell_measurement_temperature 110
_cell_measurement_theta_max 27.46
_cell_measurement_theta_min 2.77
_shelx_estimated_absorpt_T_max 0.962
_shelx_estimated_absorpt_T_min 0.758
_exptl_absorpt_coefficient_mu 1.173
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.6448
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1184 before and 0.0631 after correction. The Ratio of minimum to maximum transmission is 0.8648. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.640
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1552
_exptl_crystal_preparation 'In DCM and pentane mixture'
_exptl_crystal_recrystallization_method 'In air and at room temperature'
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.033
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1577
_diffrn_reflns_av_unetI/netI 0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 84174
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.489
_diffrn_reflns_theta_min 2.156
_diffrn_ambient_temperature 109.98
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type 'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6476
_reflns_number_total 7231
_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 V8.38A (?, 2016)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 1.164
_refine_diff_density_min -1.329
_refine_diff_density_rms 0.139
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.110
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 413
_refine_ls_number_reflns 7231
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0471
_refine_ls_R_factor_gt 0.0405
_refine_ls_restrained_S_all 1.110
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+8.5472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1013
_refine_ls_wR_factor_ref 0.1100
_refine_special_details
'the boron (B1) is located in the other side of the inversion center.The other boron should be in the opposit from the inversion center.'
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Others
Fixed Sof: F6(0.5) F7(0.5) F8(0.5)
3.a Secondary CH2 refined with riding coordinates:
C32(H32A,H32B)
3.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
3.c Idealised Me refined as rotating group:
C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.78180(2) 0.43485(2) 0.36890(2) 0.01281(8) Uani 1 1 d . . . . .
S1 S 0.70978(5) 0.26133(7) 0.48371(4) 0.01460(15) Uani 1 1 d . . . . .
Cl2 Cl 1.12727(9) 0.05294(11) 0.30608(6) 0.0457(3) Uani 1 1 d . . . . .
Cl1 Cl 1.11578(10) 0.10582(12) 0.15823(6) 0.0530(3) Uani 1 1 d . . . . .
F1 F 0.750000 0.3875(2) 0.250000 0.0162(5) Uani 1 2 d S T P . .
F4 F 0.63744(17) 0.0389(2) 0.40936(14) 0.0370(5) Uani 1 1 d . . . . .
F5 F 0.6454(2) -0.1458(2) 0.36108(17) 0.0535(8) Uani 1 1 d . . . . .
F2 F 0.6883(2) 0.0213(3) 0.31529(14) 0.0553(8) Uani 1 1 d . . . . .
F3 F 0.7765(2) -0.0437(3) 0.42616(17) 0.0620(9) Uani 1 1 d . . . . .
C19 C 0.8679(2) 0.2799(3) 0.39164(16) 0.0155(6) Uani 1 1 d . . . . .
C13 C 0.6371(2) 0.4451(3) 0.33147(16) 0.0170(6) Uani 1 1 d . . . . .
C1 C 0.7921(2) 0.4803(3) 0.47894(15) 0.0150(5) Uani 1 1 d . . . . .
C7 C 0.8560(2) 0.5815(3) 0.34884(16) 0.0149(5) Uani 1 1 d . . . . .
C2 C 0.7543(2) 0.4074(3) 0.51973(15) 0.0142(5) Uani 1 1 d . . . . .
C12 C 0.9454(2) 0.5597(3) 0.35088(17) 0.0177(6) Uani 1 1 d . . . . .
H12 H 0.971638 0.480720 0.361637 0.021 Uiso 1 1 calc R . . . .
C24 C 0.9350(2) 0.2752(3) 0.46060(16) 0.0187(6) Uani 1 1 d . . . . .
H24 H 0.935832 0.334613 0.495742 0.022 Uiso 1 1 calc R . . . .
C11 C 0.9959(2) 0.6551(3) 0.33693(17) 0.0211(6) Uani 1 1 d . . . . .
H11 H 1.057142 0.641341 0.338596 0.025 Uiso 1 1 calc R . . . .
C18 C 0.5992(2) 0.5538(3) 0.34498(17) 0.0202(6) Uani 1 1 d . . . . .
H18 H 0.638332 0.619732 0.367637 0.024 Uiso 1 1 calc R . . . .
C20 C 0.8667(2) 0.1941(3) 0.33970(17) 0.0185(6) Uani 1 1 d . . . . .
H20 H 0.820651 0.197247 0.292862 0.022 Uiso 1 1 calc R . . . .
C25 C 0.6028(2) 0.2531(3) 0.49831(16) 0.0175(6) Uani 1 1 d . . . . .
C8 C 0.8177(2) 0.6975(3) 0.33378(17) 0.0192(6) Uani 1 1 d . . . . .
H8 H 0.757197 0.712323 0.333612 0.023 Uiso 1 1 calc R . . . .
C3 C 0.7511(2) 0.4446(3) 0.58620(17) 0.0186(6) Uani 1 1 d . . . . .
H3 H 0.725293 0.392998 0.612724 0.022 Uiso 1 1 calc R . . . .
C14 C 0.5815(2) 0.3481(3) 0.29883(17) 0.0230(7) Uani 1 1 d . . . . .
H14 H 0.607560 0.274456 0.289740 0.028 Uiso 1 1 calc R . . . .
C16 C 0.4486(2) 0.4682(4) 0.29263(19) 0.0314(8) Uani 1 1 d . . . . .
H16 H 0.383593 0.475641 0.279101 0.038 Uiso 1 1 calc R . . . .
C23 C 1.0006(2) 0.1828(3) 0.47763(18) 0.0223(6) Uani 1 1 d . . . . .
H23 H 1.045750 0.177944 0.524799 0.027 Uiso 1 1 calc R . . . .
C17 C 0.5045(3) 0.5650(3) 0.32524(19) 0.0277(8) Uani 1 1 d . . . . .
H17 H 0.478292 0.638768 0.334075 0.033 Uiso 1 1 calc R . . . .
C10 C 0.9574(2) 0.7700(3) 0.32064(18) 0.0227(7) Uani 1 1 d . . . . .
H10 H 0.991891 0.834496 0.310560 0.027 Uiso 1 1 calc R . . . .
C22 C 1.0000(2) 0.0982(3) 0.42568(19) 0.0244(7) Uani 1 1 d . . . . .
H22 H 1.045431 0.036006 0.437058 0.029 Uiso 1 1 calc R . . . .
C4 C 0.7859(2) 0.5573(3) 0.61304(17) 0.0199(6) Uani 1 1 d . . . . .
H4 H 0.782665 0.584681 0.657703 0.024 Uiso 1 1 calc R . . . .
C30 C 0.5402(2) 0.3456(3) 0.46807(18) 0.0216(6) Uani 1 1 d . . . . .
H30 H 0.555857 0.410991 0.443096 0.026 Uiso 1 1 calc R . . . .
C9 C 0.8684(2) 0.7909(3) 0.31906(19) 0.0251(7) Uani 1 1 d . . . . .
H9 H 0.842107 0.869775 0.307818 0.030 Uiso 1 1 calc R . . . .
C21 C 0.9334(2) 0.1037(3) 0.35702(19) 0.0235(7) Uani 1 1 d . . . . .
H21 H 0.933588 0.045178 0.321657 0.028 Uiso 1 1 calc R . . . .
C5 C 0.8256(2) 0.6308(3) 0.57481(17) 0.0225(6) Uani 1 1 d . . . . .
H5 H 0.850538 0.707663 0.593784 0.027 Uiso 1 1 calc R . . . .
C6 C 0.8288(2) 0.5918(3) 0.50855(17) 0.0196(6) Uani 1 1 d . . . . .
H6 H 0.856662 0.642565 0.483118 0.024 Uiso 1 1 calc R . . . .
C15 C 0.4862(2) 0.3603(4) 0.27943(19) 0.0308(8) Uani 1 1 d . . . . .
H15 H 0.446973 0.294271 0.257059 0.037 Uiso 1 1 calc R . . . .
C26 C 0.5807(2) 0.1550(3) 0.53343(18) 0.0222(6) Uani 1 1 d . . . . .
H26 H 0.623877 0.091526 0.553046 0.027 Uiso 1 1 calc R . . . .
C28 C 0.4311(2) 0.2443(4) 0.5102(2) 0.0279(7) Uani 1 1 d . . . . .
H28 H 0.371913 0.241203 0.514455 0.034 Uiso 1 1 calc R . . . .
C29 C 0.4539(2) 0.3408(4) 0.4751(2) 0.0280(7) Uani 1 1 d . . . . .
H29 H 0.410552 0.404177 0.455584 0.034 Uiso 1 1 calc R . . . .
C27 C 0.4939(3) 0.1519(3) 0.53921(19) 0.0271(7) Uani 1 1 d . . . . .
H27 H 0.477609 0.085780 0.563280 0.033 Uiso 1 1 calc R . . . .
C31 C 0.7840(2) 0.1586(3) 0.54932(17) 0.0201(6) Uani 1 1 d . . . . .
H31A H 0.779140 0.174457 0.596668 0.030 Uiso 1 1 calc GR . . . .
H31B H 0.847835 0.170841 0.552256 0.030 Uiso 1 1 calc GR . . . .
H31C H 0.765381 0.074562 0.534823 0.030 Uiso 1 1 calc GR . . . .
C32 C 1.0835(5) 0.0049(6) 0.2151(3) 0.0656(16) Uani 1 1 d . . . . .
H32A H 1.015461 0.000238 0.198796 0.079 Uiso 1 1 calc R . . . .
H32B H 1.107173 -0.077607 0.211331 0.079 Uiso 1 1 calc R . . . .
B1 B 0.6873(3) -0.0327(4) 0.3776(2) 0.0277(8) Uani 1 1 d . . . . .
F9 F 0.750000 0.4023(3) 0.750000 0.0368(8) Uani 1 2 d S T P . .
B2 B 0.750000 0.2771(6) 0.750000 0.0408(17) Uani 1 2 d S T P . .
F6 F 0.8363(3) 0.2525(4) 0.7255(3) 0.0339(10) Uani 0.5 1 d . . . . .
F7 F 0.7360(4) 0.2114(4) 0.6945(2) 0.0357(11) Uani 0.5 1 d . . . . .
F8 F 0.6810(4) 0.2472(5) 0.6861(2) 0.0368(11) Uani 0.5 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
Sb1 0.01311(11) 0.01276(12) 0.01323(11) 0.00019(6) 0.00544(8) -0.00066(6)
S1 0.0152(3) 0.0136(3) 0.0164(3) 0.0003(3) 0.0073(3) -0.0004(3)
Cl2 0.0552(7) 0.0469(6) 0.0372(5) 0.0056(4) 0.0190(5) 0.0101(5)
Cl1 0.0745(9) 0.0499(7) 0.0427(6) 0.0048(5) 0.0307(6) 0.0086(6)
F1 0.0181(12) 0.0146(12) 0.0162(11) 0.000 0.0064(9) 0.000
F4 0.0347(12) 0.0310(12) 0.0543(14) -0.0191(11) 0.0269(11) -0.0088(10)
F5 0.076(2) 0.0288(13) 0.0774(19) -0.0214(13) 0.0545(17) -0.0168(13)
F2 0.071(2) 0.0647(19) 0.0382(14) 0.0022(13) 0.0290(14) -0.0220(16)
F3 0.0393(16) 0.089(2) 0.0519(17) -0.0152(16) 0.0086(13) 0.0183(16)
C19 0.0151(13) 0.0126(13) 0.0202(14) 0.0030(11) 0.0078(11) 0.0014(11)
C13 0.0137(14) 0.0229(16) 0.0148(13) 0.0016(11) 0.0056(11) 0.0002(11)
C1 0.0124(13) 0.0158(14) 0.0170(13) -0.0014(11) 0.0054(10) -0.0011(11)
C7 0.0163(14) 0.0145(13) 0.0149(13) 0.0010(11) 0.0067(11) -0.0015(11)
C2 0.0122(13) 0.0147(13) 0.0134(13) -0.0003(11) 0.0014(10) -0.0004(11)
C12 0.0185(15) 0.0173(15) 0.0174(14) -0.0003(11) 0.0064(12) -0.0006(11)
C24 0.0152(14) 0.0222(15) 0.0191(14) 0.0020(12) 0.0066(11) -0.0007(12)
C11 0.0172(14) 0.0251(16) 0.0217(15) -0.0014(12) 0.0076(12) -0.0033(12)
C18 0.0202(15) 0.0234(16) 0.0185(14) 0.0038(12) 0.0086(12) 0.0039(12)
C20 0.0196(14) 0.0151(14) 0.0205(14) 0.0011(12) 0.0068(11) -0.0006(12)
C25 0.0171(14) 0.0185(15) 0.0193(14) -0.0033(12) 0.0093(11) -0.0035(12)
C8 0.0196(14) 0.0178(15) 0.0232(15) 0.0024(12) 0.0111(12) 0.0008(12)
C3 0.0208(15) 0.0203(15) 0.0161(14) 0.0031(11) 0.0084(12) 0.0010(12)
C14 0.0178(15) 0.0294(18) 0.0218(15) -0.0046(13) 0.0072(12) -0.0017(13)
C16 0.0148(15) 0.053(2) 0.0253(17) 0.0029(16) 0.0052(13) 0.0052(16)
C23 0.0153(14) 0.0246(16) 0.0251(15) 0.0104(13) 0.0049(12) 0.0016(12)
C17 0.0238(18) 0.036(2) 0.0240(16) 0.0080(14) 0.0089(14) 0.0124(14)
C10 0.0243(16) 0.0210(16) 0.0245(15) 0.0000(13) 0.0106(13) -0.0073(13)
C22 0.0206(15) 0.0177(15) 0.0356(18) 0.0081(14) 0.0108(14) 0.0021(13)
C4 0.0212(15) 0.0229(16) 0.0157(14) -0.0039(11) 0.0068(12) 0.0000(12)
C30 0.0180(15) 0.0215(16) 0.0262(16) 0.0004(13) 0.0089(12) 0.0012(12)
C9 0.0288(18) 0.0164(15) 0.0313(17) 0.0036(13) 0.0120(14) -0.0008(13)
C21 0.0251(16) 0.0137(14) 0.0328(17) -0.0001(13) 0.0117(14) -0.0007(13)
C5 0.0252(16) 0.0211(16) 0.0206(15) -0.0041(12) 0.0074(12) -0.0036(13)
C6 0.0207(15) 0.0189(14) 0.0195(14) -0.0010(12) 0.0074(12) -0.0044(12)
C15 0.0184(16) 0.044(2) 0.0281(17) -0.0056(16) 0.0054(13) -0.0080(15)
C26 0.0229(16) 0.0205(16) 0.0254(16) 0.0007(13) 0.0111(13) -0.0026(13)
C28 0.0213(16) 0.036(2) 0.0318(18) -0.0095(15) 0.0162(14) -0.0048(14)
C29 0.0196(16) 0.0303(19) 0.0346(18) -0.0059(15) 0.0104(14) 0.0030(14)
C27 0.0283(18) 0.0278(18) 0.0298(17) -0.0030(14) 0.0161(14) -0.0082(14)
C31 0.0199(15) 0.0153(14) 0.0247(15) 0.0044(12) 0.0073(12) 0.0025(12)
C32 0.100(5) 0.050(3) 0.041(3) 0.003(2) 0.017(3) 0.002(3)
B1 0.031(2) 0.0255(19) 0.034(2) -0.0060(17) 0.0197(17) -0.0044(17)
F9 0.047(2) 0.0205(15) 0.058(2) 0.000 0.0374(17) 0.000
B2 0.050(4) 0.017(3) 0.035(3) 0.000 -0.011(3) 0.000
F6 0.031(2) 0.033(2) 0.046(3) -0.002(2) 0.023(2) 0.0040(19)
F7 0.056(3) 0.029(2) 0.024(2) -0.0049(18) 0.017(2) 0.002(2)
F8 0.036(3) 0.040(3) 0.026(2) -0.003(2) 0.001(2) -0.007(2)
_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
Sb1 F1 2.2849(7) . ?
Sb1 C19 2.112(3) . ?
Sb1 C13 2.103(3) . ?
Sb1 C1 2.182(3) . ?
Sb1 C7 2.097(3) . ?
S1 C2 1.793(3) . ?
S1 C25 1.782(3) . ?
S1 C31 1.797(3) . ?
Cl2 C32 1.765(5) . ?
Cl1 C32 1.772(6) . ?
F4 B1 1.397(5) . ?
F5 B1 1.387(5) . ?
F2 B1 1.372(5) . ?
F3 B1 1.384(5) . ?
C19 C24 1.395(4) . ?
C19 C20 1.389(4) . ?
C13 C18 1.396(4) . ?
C13 C14 1.380(5) . ?
C1 C2 1.403(4) . ?
C1 C6 1.390(4) . ?
C7 C12 1.393(4) . ?
C7 C8 1.393(4) . ?
C2 C3 1.393(4) . ?
C12 C11 1.392(4) . ?
C24 C23 1.392(5) . ?
C11 C10 1.385(5) . ?
C18 C17 1.385(5) . ?
C20 C21 1.388(5) . ?
C25 C30 1.387(5) . ?
C25 C26 1.389(4) . ?
C8 C9 1.385(5) . ?
C3 C4 1.381(5) . ?
C14 C15 1.394(5) . ?
C16 C17 1.381(6) . ?
C16 C15 1.387(6) . ?
C23 C22 1.382(5) . ?
C10 C9 1.387(5) . ?
C22 C21 1.387(5) . ?
C4 C5 1.388(5) . ?
C30 C29 1.393(5) . ?
C5 C6 1.395(4) . ?
C26 C27 1.389(5) . ?
C28 C29 1.380(5) . ?
C28 C27 1.384(6) . ?
F9 B2 1.376(7) . ?
B2 F6 1.597(4) . ?
B2 F6 1.597(4) 2_656 ?
B2 F7 1.266(6) 2_656 ?
B2 F7 1.267(6) . ?
B2 F8 1.378(5) . ?
B2 F8 1.378(5) 2_656 ?
F6 F7 1.525(7) . ?
F7 F8 0.900(6) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C19 Sb1 F1 85.82(9) . . ?
C19 Sb1 C1 98.81(11) . . ?
C13 Sb1 F1 80.36(8) . . ?
C13 Sb1 C19 129.34(12) . . ?
C13 Sb1 C1 91.93(11) . . ?
C1 Sb1 F1 172.27(8) . . ?
C7 Sb1 F1 85.14(9) . . ?
C7 Sb1 C19 108.23(12) . . ?
C7 Sb1 C13 118.67(12) . . ?
C7 Sb1 C1 99.17(11) . . ?
C2 S1 C31 102.51(15) . . ?
C25 S1 C2 103.35(14) . . ?
C25 S1 C31 104.30(15) . . ?
Sb1 F1 Sb1 153.66(12) 2_655 . ?
C24 C19 Sb1 115.9(2) . . ?
C20 C19 Sb1 123.1(2) . . ?
C20 C19 C24 120.6(3) . . ?
C18 C13 Sb1 116.5(2) . . ?
C14 C13 Sb1 122.4(2) . . ?
C14 C13 C18 121.0(3) . . ?
C2 C1 Sb1 122.9(2) . . ?
C6 C1 Sb1 119.8(2) . . ?
C6 C1 C2 117.0(3) . . ?
C12 C7 Sb1 117.9(2) . . ?
C8 C7 Sb1 121.5(2) . . ?
C8 C7 C12 120.6(3) . . ?
C1 C2 S1 117.6(2) . . ?
C3 C2 S1 120.1(2) . . ?
C3 C2 C1 122.3(3) . . ?
C11 C12 C7 119.1(3) . . ?
C23 C24 C19 119.6(3) . . ?
C10 C11 C12 120.4(3) . . ?
C17 C18 C13 119.8(3) . . ?
C21 C20 C19 119.2(3) . . ?
C30 C25 S1 116.3(2) . . ?
C30 C25 C26 121.8(3) . . ?
C26 C25 S1 121.8(3) . . ?
C9 C8 C7 119.5(3) . . ?
C4 C3 C2 119.1(3) . . ?
C13 C14 C15 118.8(3) . . ?
C17 C16 C15 120.7(3) . . ?
C22 C23 C24 119.8(3) . . ?
C16 C17 C18 119.5(3) . . ?
C11 C10 C9 120.0(3) . . ?
C23 C22 C21 120.4(3) . . ?
C3 C4 C5 120.0(3) . . ?
C25 C30 C29 118.7(3) . . ?
C8 C9 C10 120.4(3) . . ?
C22 C21 C20 120.4(3) . . ?
C4 C5 C6 120.1(3) . . ?
C1 C6 C5 121.4(3) . . ?
C16 C15 C14 120.3(4) . . ?
C25 C26 C27 118.4(3) . . ?
C29 C28 C27 120.3(3) . . ?
C28 C29 C30 120.3(3) . . ?
C28 C27 C26 120.6(3) . . ?
Cl2 C32 Cl1 111.5(4) . . ?
F5 B1 F4 108.9(3) . . ?
F2 B1 F4 110.0(4) . . ?
F2 B1 F5 109.2(3) . . ?
F2 B1 F3 109.7(3) . . ?
F3 B1 F4 108.2(3) . . ?
F3 B1 F5 110.9(4) . . ?
F9 B2 F6 99.8(3) . 2_656 ?
F9 B2 F6 99.8(3) . . ?
F9 B2 F8 103.8(3) . 2_656 ?
F9 B2 F8 103.8(3) . . ?
F6 B2 F6 160.5(6) . 2_656 ?
F7 B2 F9 124.8(3) 2_656 . ?
F7 B2 F9 124.8(3) . . ?
F7 B2 F6 105.0(4) . 2_656 ?
F7 B2 F6 63.1(3) . . ?
F7 B2 F6 63.1(3) 2_656 2_656 ?
F7 B2 F6 105.0(4) 2_656 . ?
F7 B2 F7 110.5(7) 2_656 . ?
F7 B2 F8 39.5(3) . . ?
F7 B2 F8 120.0(5) 2_656 . ?
F7 B2 F8 39.5(3) 2_656 2_656 ?
F7 B2 F8 120.0(5) . 2_656 ?
F8 B2 F6 98.3(3) . . ?
F8 B2 F6 77.0(3) . 2_656 ?
F8 B2 F6 77.0(3) 2_656 . ?
F8 B2 F6 98.3(3) 2_656 2_656 ?
F8 B2 F8 152.4(7) . 2_656 ?
F7 F6 B2 47.8(3) . . ?
B2 F7 F6 69.1(3) . . ?
F8 F7 B2 76.9(5) . . ?
F8 F7 F6 135.3(6) . . ?
F7 F8 B2 63.6(4) . . ?
_shelx_res_file
;
TITL Me_2_BF4_0ma_a.res in P2/n
me_2_bf4_0ma.res
created by SHELXL-2018/3 at 15:22:09 on 04-May-2020
REM
REM {'C00U': 'AtomInfo()', 'C00T': 'AtomInfo()', 'C00W': 'AtomInfo()',
REM 'C00V': 'AtomInfo()', 'C00Q': 'AtomInfo()', 'C00P': 'AtomInfo()',
REM 'C00S': 'AtomInfo()', 'C00R': 'AtomInfo()', 'B017': 'AtomInfo()',
REM 'C00Y': 'AtomInfo()', 'C00X': 'AtomInfo()', 'C00Z': 'AtomInfo()',
REM 'C00E': 'AtomInfo()', 'C00D': 'AtomInfo()', 'C00G': 'AtomInfo()',
REM 'C00F': 'AtomInfo()', 'C00C': 'AtomInfo()', 'C00B': 'AtomInfo()',
REM 'C00M': 'AtomInfo()', 'C00L': 'AtomInfo()', 'C00O': 'AtomInfo()',
REM 'C00N': 'AtomInfo()', 'C00I': 'AtomInfo()', 'C00H': 'AtomInfo()',
REM 'C00K': 'AtomInfo()', 'C00J': 'AtomInfo()', 'F00A': 'AtomInfo()',
REM 'C018': 'AtomInfo()', 'C012': 'AtomInfo()', 'C013': 'AtomInfo()',
REM 'C010': 'AtomInfo()', 'C011': 'AtomInfo()', 'C016': 'AtomInfo()',
REM 'C014': 'AtomInfo()', 'C015': 'AtomInfo()', 'B019': 'AtomInfo()',
REM 'CL03': 'AtomInfo()', 'CL02': 'AtomInfo()', 'CL04': 'AtomInfo()',
REM 'F006': 'AtomInfo()', 'F007': 'AtomInfo()', 'F005': 'AtomInfo()',
REM 'SB01': 'AtomInfo()', 'B01A': 'AtomInfo()', 'F008': 'AtomInfo()',
REM 'F009': 'AtomInfo()'}
REM
CELL 0.71073 15.4944 10.9891 19.761 90 110.566 90
ZERR 2 0.0023 0.0016 0.0029 0 0.007 0
LATT 1
SYMM 0.5-X,+Y,0.5-Z
SFAC C H B Cl F S Sb
UNIT 128 116 6 8 26 4 4
L.S. 4
PLAN 5 0 0
SIZE 0.033 0.15 0.25
TEMP -163.17
fmap 2
acta
OMIT 2 0 0
OMIT -1 0 7
REM
REM
REM
WGHT 0.038100 8.547200
FVAR 0.32360
SB1 7 0.781797 0.434850 0.368896 11.00000 0.01311 0.01276 =
0.01323 0.00019 0.00544 -0.00066
S1 6 0.709782 0.261333 0.483711 11.00000 0.01522 0.01360 =
0.01636 0.00027 0.00728 -0.00039
CL2 4 1.127272 0.052936 0.306080 11.00000 0.05519 0.04687 =
0.03722 0.00562 0.01900 0.01006
CL1 4 1.115777 0.105816 0.158232 11.00000 0.07451 0.04994 =
0.04268 0.00484 0.03068 0.00865
F1 5 0.750000 0.387484 0.250000 10.50000 0.01814 0.01462 =
0.01624 0.00000 0.00637 0.00000
F4 5 0.637445 0.038863 0.409363 11.00000 0.03472 0.03102 =
0.05430 -0.01906 0.02689 -0.00875
F5 5 0.645395 -0.145781 0.361079 11.00000 0.07630 0.02883 =
0.07744 -0.02142 0.05448 -0.01681
F2 5 0.688308 0.021267 0.315285 11.00000 0.07090 0.06465 =
0.03819 0.00221 0.02901 -0.02199
F3 5 0.776539 -0.043712 0.426165 11.00000 0.03929 0.08898 =
0.05188 -0.01522 0.00862 0.01833
C19 1 0.867879 0.279917 0.391640 11.00000 0.01513 0.01257 =
0.02022 0.00299 0.00782 0.00144
C13 1 0.637087 0.445141 0.331475 11.00000 0.01368 0.02292 =
0.01482 0.00163 0.00559 0.00016
C1 1 0.792085 0.480341 0.478937 11.00000 0.01245 0.01576 =
0.01703 -0.00143 0.00538 -0.00106
C7 1 0.855994 0.581532 0.348839 11.00000 0.01625 0.01453 =
0.01493 0.00101 0.00668 -0.00155
C2 1 0.754278 0.407390 0.519734 11.00000 0.01215 0.01472 =
0.01340 -0.00032 0.00142 -0.00035
C12 1 0.945427 0.559686 0.350876 11.00000 0.01849 0.01732 =
0.01737 -0.00035 0.00636 -0.00057
AFIX 43
H12 2 0.971638 0.480720 0.361637 11.00000 -1.20000
AFIX 0
C24 1 0.934959 0.275177 0.460597 11.00000 0.01520 0.02224 =
0.01913 0.00204 0.00655 -0.00068
AFIX 43
H24 2 0.935832 0.334613 0.495742 11.00000 -1.20000
AFIX 0
C11 1 0.995899 0.655113 0.336932 11.00000 0.01720 0.02509 =
0.02172 -0.00138 0.00764 -0.00332
AFIX 43
H11 2 1.057142 0.641341 0.338596 11.00000 -1.20000
AFIX 0
C18 1 0.599242 0.553752 0.344979 11.00000 0.02019 0.02338 =
0.01855 0.00380 0.00856 0.00395
AFIX 43
H18 2 0.638332 0.619732 0.367637 11.00000 -1.20000
AFIX 0
C20 1 0.866665 0.194088 0.339697 11.00000 0.01958 0.01508 =
0.02051 0.00105 0.00682 -0.00059
AFIX 43
H20 2 0.820651 0.197247 0.292862 11.00000 -1.20000
AFIX 0
C25 1 0.602773 0.253122 0.498310 11.00000 0.01706 0.01849 =
0.01931 -0.00332 0.00934 -0.00346
C8 1 0.817674 0.697475 0.333781 11.00000 0.01958 0.01783 =
0.02318 0.00236 0.01113 0.00084
AFIX 43
H8 2 0.757197 0.712323 0.333612 11.00000 -1.20000
AFIX 0
C3 1 0.751079 0.444559 0.586201 11.00000 0.02084 0.02031 =
0.01607 0.00311 0.00840 0.00101
AFIX 43
H3 2 0.725293 0.392998 0.612724 11.00000 -1.20000
AFIX 0
C14 1 0.581455 0.348138 0.298828 11.00000 0.01778 0.02940 =
0.02184 -0.00459 0.00716 -0.00170
AFIX 43
H14 2 0.607560 0.274456 0.289740 11.00000 -1.20000
AFIX 0
C16 1 0.448565 0.468217 0.292631 11.00000 0.01478 0.05274 =
0.02530 0.00291 0.00518 0.00517
AFIX 43
H16 2 0.383593 0.475641 0.279101 11.00000 -1.20000
AFIX 0
C23 1 1.000644 0.182820 0.477629 11.00000 0.01532 0.02464 =
0.02506 0.01043 0.00486 0.00157
AFIX 43
H23 2 1.045750 0.177944 0.524799 11.00000 -1.20000
AFIX 0
C17 1 0.504531 0.565015 0.325241 11.00000 0.02379 0.03570 =
0.02400 0.00801 0.00886 0.01244
AFIX 43
H17 2 0.478292 0.638768 0.334075 11.00000 -1.20000
AFIX 0
C10 1 0.957375 0.770026 0.320643 11.00000 0.02427 0.02105 =
0.02450 -0.00002 0.01057 -0.00729
AFIX 43
H10 2 0.991891 0.834496 0.310560 11.00000 -1.20000
AFIX 0
C22 1 1.000007 0.098244 0.425677 11.00000 0.02062 0.01773 =
0.03559 0.00806 0.01081 0.00207
AFIX 43
H22 2 1.045431 0.036006 0.437058 11.00000 -1.20000
AFIX 0
C4 1 0.785882 0.557346 0.613042 11.00000 0.02124 0.02292 =
0.01566 -0.00390 0.00679 -0.00003
AFIX 43
H4 2 0.782665 0.584681 0.657703 11.00000 -1.20000
AFIX 0
C30 1 0.540178 0.345642 0.468070 11.00000 0.01796 0.02150 =
0.02617 0.00040 0.00894 0.00121
AFIX 43
H30 2 0.555857 0.410991 0.443096 11.00000 -1.20000
AFIX 0
C9 1 0.868391 0.790923 0.319061 11.00000 0.02875 0.01644 =
0.03127 0.00360 0.01197 -0.00079
AFIX 43
H9 2 0.842107 0.869775 0.307818 11.00000 -1.20000
AFIX 0
C21 1 0.933448 0.103675 0.357016 11.00000 0.02512 0.01366 =
0.03281 -0.00007 0.01168 -0.00066
AFIX 43
H21 2 0.933588 0.045178 0.321657 11.00000 -1.20000
AFIX 0
C5 1 0.825550 0.630770 0.574808 11.00000 0.02520 0.02111 =
0.02059 -0.00407 0.00744 -0.00358
AFIX 43
H5 2 0.850538 0.707663 0.593784 11.00000 -1.20000
AFIX 0
C6 1 0.828785 0.591824 0.508548 11.00000 0.02066 0.01889 =
0.01952 -0.00098 0.00737 -0.00440
AFIX 43
H6 2 0.856662 0.642565 0.483118 11.00000 -1.20000
AFIX 0
C15 1 0.486230 0.360271 0.279428 11.00000 0.01836 0.04370 =
0.02809 -0.00559 0.00538 -0.00804
AFIX 43
H15 2 0.446973 0.294271 0.257059 11.00000 -1.20000
AFIX 0
C26 1 0.580678 0.155000 0.533434 11.00000 0.02288 0.02050 =
0.02536 0.00070 0.01106 -0.00255
AFIX 43
H26 2 0.623877 0.091526 0.553046 11.00000 -1.20000
AFIX 0
C28 1 0.431058 0.244270 0.510178 11.00000 0.02133 0.03620 =
0.03178 -0.00952 0.01618 -0.00478
AFIX 43
H28 2 0.371913 0.241203 0.514455 11.00000 -1.20000
AFIX 0
C29 1 0.453875 0.340787 0.475065 11.00000 0.01964 0.03031 =
0.03462 -0.00587 0.01040 0.00299
AFIX 43
H29 2 0.410552 0.404177 0.455584 11.00000 -1.20000
AFIX 0
C27 1 0.493939 0.151879 0.539206 11.00000 0.02831 0.02785 =
0.02982 -0.00302 0.01605 -0.00817
AFIX 43
H27 2 0.477609 0.085780 0.563280 11.00000 -1.20000
AFIX 0
C31 1 0.783967 0.158625 0.549322 11.00000 0.01990 0.01534 =
0.02466 0.00436 0.00732 0.00251
AFIX 137
H31A 2 0.779140 0.174457 0.596668 11.00000 -1.50000
H31B 2 0.847835 0.170841 0.552256 11.00000 -1.50000
H31C 2 0.765381 0.074562 0.534823 11.00000 -1.50000
AFIX 0
C32 1 1.083534 0.004854 0.215113 11.00000 0.10017 0.04954 =
0.04057 0.00320 0.01659 0.00227
AFIX 23
H32A 2 1.015461 0.000238 0.198796 11.00000 -1.20000
H32B 2 1.107173 -0.077607 0.211331 11.00000 -1.20000
AFIX 0
B1 3 0.687292 -0.032732 0.377591 11.00000 0.03070 0.02546 =
0.03363 -0.00603 0.01971 -0.00444
F9 5 0.750000 0.402344 0.750000 10.50000 0.04708 0.02054 =
0.05788 0.00000 0.03741 0.00000
B2 3 0.750000 0.277107 0.750000 10.50000 0.04998 0.01681 =
0.03494 0.00000 -0.01103 0.00000
F6 5 0.836318 0.252451 0.725522 10.50000 0.03067 0.03306 =
0.04577 -0.00206 0.02314 0.00400
F7 5 0.735995 0.211384 0.694507 10.50000 0.05590 0.02931 =
0.02404 -0.00495 0.01665 0.00204
F8 5 0.680972 0.247222 0.686060 10.50000 0.03586 0.04028 =
0.02614 -0.00324 0.00077 -0.00653
HKLF 4
REM Me_2_BF4_0ma_a.res in P2/n
REM wR2 = 0.1100, GooF = S = 1.110, Restrained GooF = 1.110 for all data
REM R1 = 0.0405 for 6476 Fo > 4sig(Fo) and 0.0471 for all 7231 data
REM 413 parameters refined using 0 restraints
END
WGHT 0.0381 8.5470
REM Highest difference peak 1.164, deepest hole -1.329, 1-sigma level 0.139
Q1 1 0.7904 0.4566 0.4176 11.00000 0.05 1.16
Q2 1 1.2179 0.1562 0.1709 11.00000 0.05 1.13
Q3 1 0.7774 0.4049 0.3183 11.00000 0.05 1.05
Q4 1 0.7722 0.4634 0.3217 11.00000 0.05 1.03
Q5 1 0.7836 0.4081 0.4215 11.00000 0.05 0.96
;
_shelx_res_checksum 94333
_olex2_submission_special_instructions 'No special instructions were received'