# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_1a
_database_code_depnum_ccdc_archive 'CCDC 1832429'
_audit_update_record
;
2018-03-26 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;
# mo_jhgla025_0m
# [Y(hfac)3(N,N'-pd)]Et2O
_audit_creation_date 2018-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C27 H9 F18 N2 O8 Y, C4 H10 O'
_chemical_formula_sum 'C31 H19 F18 N2 O9 Y'
_chemical_formula_weight 994.39
_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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 9.6263(3)
_cell_length_b 22.7963(8)
_cell_length_c 17.0279(6)
_cell_angle_alpha 90
_cell_angle_beta 99.1760(10)
_cell_angle_gamma 90
_cell_volume 3688.9(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9949
_cell_measurement_temperature 100
_cell_measurement_theta_max 27.48
_cell_measurement_theta_min 2.32
_shelx_estimated_absorpt_T_max 0.919
_shelx_estimated_absorpt_T_min 0.653
_exptl_absorpt_coefficient_mu 1.727
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.5540
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1028 before and 0.0482 after correction. The Ratio of minimum to maximum transmission is 0.7430. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour green
_exptl_crystal_colour_primary green
_exptl_crystal_density_diffrn 1.791
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description column
_exptl_crystal_F_000 1968
_exptl_crystal_size_max 0.27
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.05
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0313
_diffrn_reflns_av_unetI/netI 0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 25874
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.494
_diffrn_reflns_theta_min 2.322
_diffrn_ambient_temperature 100
_diffrn_detector 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type 'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 VENTURE'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_collimation 'focusing mirrors'
_diffrn_radiation_monochromator 'multilayer mirror optics'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed tube'
_diffrn_source_type 'INCOATEC I\ms 3.0'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6684
_reflns_number_total 8416
_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 V8.37A (Bruker-AXS, 2016)'
_computing_data_collection 'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction 'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'XT (Sheldrick, 2015)'
_refine_diff_density_max 0.768
_refine_diff_density_min -1.022
_refine_diff_density_rms 0.105
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.066
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 567
_refine_ls_number_reflns 8416
_refine_ls_number_restraints 7
_refine_ls_R_factor_all 0.0696
_refine_ls_R_factor_gt 0.0538
_refine_ls_restrained_S_all 1.066
_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^)+(0.0890P)^2^+5.8620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1530
_refine_ls_wR_factor_ref 0.1624
_refine_special_details
;
A molecule of Et2O in the lattice is partly disordered with the oxygen and one C2H5
modelled over 2 0.5 occupied sites. Distance restratins were applied and the oxygen
was modelled with isotropic adps.
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
O11-C2EA = O11-C3E = O10-C3E = O10-C2EB
1.43 with sigma of 0.01
C4E-C3E \\sim C2EA-C1EA \\sim C1EB-C2EB
with sigma of 0.02
3. Others
Fixed Sof: H3EC(0.5) H3ED(0.5) H3EA(0.5) H3EB(0.5) C1EA(0.5) H1EA(0.5)
H1EB(0.5) H1EC(0.5) O10(0.5) C2EA(0.5) H2EA(0.5) H2EB(0.5) O11(0.5) C1EB(0.5)
H1ED(0.5) H1EE(0.5) H1EF(0.5) C2EB(0.5) H2EC(0.5) H2ED(0.5)
4.a Secondary CH2 refined with riding coordinates:
C3E(H3EC,H3ED), C3E(H3EA,H3EB), C2EA(H2EA,H2EB), C2EB(H2EC,H2ED)
4.b Me refined with riding coordinates:
C4E(H4EA,H4EB,H4EC), C1EA(H1EA,H1EB,H1EC), C1EB(H1ED,H1EE,H1EF)
4.c Aromatic/amide H refined with riding coordinates:
C10(H10), C25(H25), C15(H15), C8(H8), C20(H20), C9(H9), C1(H1), C3(H3), C2(H2)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.22870(3) 0.57404(2) 0.70979(2) 0.01917(11) Uani 1 1 d . . . . .
F17 F 0.4205(3) 0.37968(11) 0.65399(14) 0.0373(6) Uani 1 1 d . . . . .
O5 O 0.3063(3) 0.55977(11) 0.58897(14) 0.0227(5) Uani 1 1 d . . . . .
F12 F -0.2064(3) 0.63470(14) 0.54812(15) 0.0494(7) Uani 1 1 d . . . . .
O8 O 0.3213(3) 0.48080(11) 0.71828(16) 0.0267(5) Uani 1 1 d . . . . .
F11 F -0.1406(3) 0.63941(13) 0.43521(14) 0.0446(6) Uani 1 1 d . . . . .
F7 F 0.3242(3) 0.61667(13) 0.40229(15) 0.0479(7) Uani 1 1 d . . . . .
O6 O 0.0318(3) 0.58301(12) 0.61327(15) 0.0254(5) Uani 1 1 d . . . . .
O3 O 0.1062(3) 0.64683(11) 0.76747(16) 0.0285(6) Uani 1 1 d . . . . .
O7 O 0.0623(3) 0.51442(11) 0.75232(15) 0.0272(6) Uani 1 1 d . . . . .
O4 O 0.2880(3) 0.66446(11) 0.66092(16) 0.0273(6) Uani 1 1 d . . . . .
F13 F -0.1018(3) 0.46870(12) 0.85547(16) 0.0480(7) Uani 1 1 d . . . . .
F8 F 0.4892(3) 0.59918(18) 0.49930(16) 0.0621(9) Uani 1 1 d . . . . .
F16 F 0.5019(3) 0.39182(14) 0.77640(17) 0.0611(9) Uani 1 1 d . . . . .
F9 F 0.3832(3) 0.52831(14) 0.43244(18) 0.0617(8) Uani 1 1 d . . . . .
O2 O 0.8728(3) 0.57527(13) 0.97087(19) 0.0395(7) Uani 1 1 d . . . . .
F4 F 0.2863(4) 0.81395(12) 0.6230(2) 0.0766(11) Uani 1 1 d . . . . .
F3 F 0.0364(4) 0.78561(13) 0.8352(2) 0.0750(11) Uani 1 1 d . . . . .
N2 N 0.4894(3) 0.58504(13) 0.75616(18) 0.0251(6) Uani 1 1 d . . . . .
F10 F -0.1995(3) 0.55671(13) 0.4785(2) 0.0717(11) Uani 1 1 d . . . . .
F15 F -0.1968(3) 0.45671(17) 0.7345(2) 0.0686(10) Uani 1 1 d . . . . .
O1 O 0.6850(3) 0.56819(13) 1.07618(18) 0.0418(8) Uani 1 1 d . . . . .
F18 F 0.3377(4) 0.32900(12) 0.7404(2) 0.0680(10) Uani 1 1 d . . . . .
N1 N 0.3064(3) 0.57240(12) 0.85849(17) 0.0223(6) Uani 1 1 d . . . . .
F6 F 0.2882(5) 0.74319(15) 0.54089(18) 0.0820(12) Uani 1 1 d . . . . .
F14 F -0.0936(4) 0.38418(13) 0.8028(3) 0.0945(15) Uani 1 1 d . . . . .
F5 F 0.4597(3) 0.75726(17) 0.6320(3) 0.0823(12) Uani 1 1 d . . . . .
C26 C 0.2769(4) 0.43073(16) 0.7309(2) 0.0261(8) Uani 1 1 d . . . . .
C12 C 0.4446(4) 0.57491(14) 0.8901(2) 0.0226(7) Uani 1 1 d . . . . .
C7 C 0.6896(4) 0.58314(16) 0.8605(2) 0.0275(8) Uani 1 1 d . . . . .
C11 C 0.5437(4) 0.58061(15) 0.8345(2) 0.0238(7) Uani 1 1 d . . . . .
F2 F -0.1162(4) 0.72231(19) 0.8002(3) 0.1111(18) Uani 1 1 d . . . . .
C4 C 0.4890(4) 0.57439(15) 0.9725(2) 0.0260(8) Uani 1 1 d . . . . .
F1 F 0.0415(7) 0.7032(2) 0.8939(2) 0.136(2) Uani 1 1 d . . . . .
C10 C 0.5790(4) 0.59209(19) 0.7042(2) 0.0322(9) Uani 1 1 d . . . . .
H10 H 0.541291 0.595071 0.649271 0.039 Uiso 1 1 calc R . . . .
C14 C 0.1050(4) 0.70170(17) 0.7667(2) 0.0279(8) Uani 1 1 d . . . . .
C25 C 0.1461(4) 0.41631(16) 0.7494(2) 0.0289(8) Uani 1 1 d . . . . .
H25 H 0.121573 0.376241 0.754035 0.035 Uiso 1 1 calc R . . . .
C22 C -0.1341(4) 0.60567(18) 0.4998(2) 0.0299(8) Uani 1 1 d . . . . .
C19 C 0.2586(4) 0.57794(16) 0.5207(2) 0.0253(7) Uani 1 1 d . . . . .
C6 C 0.7468(4) 0.57786(16) 0.9461(3) 0.0315(9) Uani 1 1 d . . . . .
C16 C 0.2555(4) 0.71669(16) 0.6693(2) 0.0253(7) Uani 1 1 d . . . . .
C21 C 0.0175(4) 0.59401(16) 0.5398(2) 0.0255(7) Uani 1 1 d . . . . .
C15 C 0.1711(4) 0.73934(17) 0.7206(2) 0.0305(8) Uani 1 1 d . . . . .
H15 H 0.158617 0.780535 0.724080 0.037 Uiso 1 1 calc R . . . .
C27 C 0.3849(4) 0.38214(17) 0.7260(2) 0.0322(8) Uani 1 1 d . . . . .
C8 C 0.7788(4) 0.5908(2) 0.8056(3) 0.0364(9) Uani 1 1 d . . . . .
H8 H 0.877640 0.592934 0.822368 0.044 Uiso 1 1 calc R . . . .
C20 C 0.1204(4) 0.59510(18) 0.4920(2) 0.0287(8) Uani 1 1 d . . . . .
H20 H 0.096884 0.607793 0.438373 0.034 Uiso 1 1 calc R . . . .
C9 C 0.7232(4) 0.5953(2) 0.7262(3) 0.0387(10) Uani 1 1 d . . . . .
H9 H 0.782848 0.600412 0.687302 0.046 Uiso 1 1 calc R . . . .
C24 C 0.0508(4) 0.45962(17) 0.7612(2) 0.0265(8) Uani 1 1 d . . . . .
C3E C 0.6124(5) 0.74447(17) 0.9412(3) 0.0420(10) Uani 1 1 d D . . . .
H3EC H 0.691998 0.756600 0.914551 0.050 Uiso 0.5 1 calc R . P A 2
H3ED H 0.588172 0.777548 0.974169 0.050 Uiso 0.5 1 calc R . P A 2
H3EA H 0.673832 0.771619 0.916993 0.050 Uiso 0.5 1 calc R . P B 1
H3EB H 0.579693 0.765077 0.986052 0.050 Uiso 0.5 1 calc R . P B 1
C1 C 0.2121(4) 0.57049(16) 0.9088(2) 0.0270(8) Uani 1 1 d . . . . .
H1 H 0.115191 0.567854 0.886845 0.032 Uiso 1 1 calc R . . . .
C3 C 0.3895(5) 0.57348(16) 1.0225(2) 0.0319(9) Uani 1 1 d . . . . .
H3 H 0.418246 0.573759 1.078545 0.038 Uiso 1 1 calc R . . . .
C5 C 0.6419(5) 0.57378(16) 1.0050(2) 0.0306(9) Uani 1 1 d . . . . .
C18 C 0.3650(4) 0.5806(2) 0.4629(2) 0.0355(9) Uani 1 1 d . . . . .
C2 C 0.2486(5) 0.57216(16) 0.9912(2) 0.0305(8) Uani 1 1 d . . . . .
H2 H 0.178631 0.572389 1.024723 0.037 Uiso 1 1 calc R . . . .
C23 C -0.0860(5) 0.4419(2) 0.7876(3) 0.0446(11) Uani 1 1 d . . . . .
C17 C 0.3201(5) 0.75871(19) 0.6147(3) 0.0404(10) Uani 1 1 d . . . . .
C13 C 0.0187(6) 0.7296(2) 0.8250(3) 0.0486(12) Uani 1 1 d . . . . .
C4E C 0.4888(5) 0.7283(2) 0.8808(3) 0.0490(12) Uani 1 1 d D . . . .
H4EA H 0.436752 0.763905 0.861876 0.074 Uiso 1 1 calc R . . . .
H4EB H 0.521088 0.708530 0.835986 0.074 Uiso 1 1 calc R . . . .
H4EC H 0.427042 0.701995 0.904977 0.074 Uiso 1 1 calc R . . . .
C1EA C 0.7821(12) 0.7265(6) 1.1062(6) 0.056(3) Uani 0.5 1 d D . P C 1
H1EA H 0.869992 0.736388 1.141190 0.085 Uiso 0.5 1 calc R . P C 1
H1EB H 0.719764 0.760769 1.100478 0.085 Uiso 0.5 1 calc R . P C 1
H1EC H 0.735824 0.693963 1.129374 0.085 Uiso 0.5 1 calc R . P C 1
O10 O 0.6509(6) 0.6935(2) 0.9905(3) 0.0272(12) Uiso 0.5 1 d D . P D 2
C2EA C 0.8134(11) 0.7090(4) 1.0270(5) 0.041(2) Uani 0.5 1 d D . P C 1
H2EA H 0.862463 0.741825 1.004947 0.049 Uiso 0.5 1 calc R . P C 1
H2EB H 0.878498 0.675123 1.033797 0.049 Uiso 0.5 1 calc R . P C 1
O11 O 0.6915(6) 0.6935(2) 0.9705(4) 0.0341(14) Uiso 0.5 1 d D . P C 1
C1EB C 0.8958(11) 0.7186(5) 1.0463(6) 0.047(2) Uani 0.5 1 d D . P D 2
H1ED H 0.955796 0.726833 1.097239 0.071 Uiso 0.5 1 calc R . P D 2
H1EE H 0.932488 0.684391 1.021414 0.071 Uiso 0.5 1 calc R . P D 2
H1EF H 0.895207 0.752658 1.011191 0.071 Uiso 0.5 1 calc R . P D 2
C2EB C 0.7485(10) 0.7061(4) 1.0604(5) 0.039(2) Uani 0.5 1 d D . P D 2
H2EC H 0.751064 0.672411 1.097239 0.047 Uiso 0.5 1 calc R . P D 2
H2ED H 0.713853 0.740549 1.087035 0.047 Uiso 0.5 1 calc R . P D 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Y1 0.01870(17) 0.02011(18) 0.01783(17) 0.00039(12) 0.00032(12) -0.00043(13)
F17 0.0392(13) 0.0417(14) 0.0318(12) -0.0038(10) 0.0082(10) 0.0121(11)
O5 0.0246(12) 0.0250(12) 0.0181(12) -0.0009(10) 0.0026(10) 0.0020(10)
F12 0.0351(13) 0.077(2) 0.0356(13) 0.0068(13) 0.0036(11) 0.0219(14)
O8 0.0260(13) 0.0232(12) 0.0303(13) 0.0020(11) 0.0022(11) 0.0004(10)
F11 0.0361(13) 0.0652(17) 0.0298(12) 0.0138(12) -0.0032(10) 0.0123(12)
F7 0.0405(14) 0.0735(19) 0.0314(13) 0.0212(13) 0.0106(11) 0.0064(13)
O6 0.0200(12) 0.0353(14) 0.0200(12) -0.0019(10) 0.0003(10) -0.0005(10)
O3 0.0282(13) 0.0258(13) 0.0301(14) 0.0066(11) 0.0002(11) 0.0036(11)
O7 0.0277(13) 0.0242(13) 0.0283(13) 0.0005(10) -0.0004(11) -0.0028(11)
O4 0.0266(13) 0.0229(13) 0.0326(14) -0.0024(11) 0.0054(11) -0.0020(10)
F13 0.0611(17) 0.0449(15) 0.0467(15) 0.0053(12) 0.0351(13) 0.0021(13)
F8 0.0298(13) 0.126(3) 0.0297(13) 0.0087(16) 0.0024(11) -0.0149(16)
F16 0.0597(18) 0.0672(19) 0.0448(16) -0.0164(14) -0.0268(14) 0.0357(16)
F9 0.075(2) 0.0634(19) 0.0546(18) -0.0059(15) 0.0357(16) 0.0197(17)
O2 0.0297(15) 0.0413(16) 0.0412(17) -0.0010(13) -0.0137(13) 0.0032(13)
F4 0.109(3) 0.0260(14) 0.111(3) 0.0150(16) 0.068(2) 0.0029(16)
F3 0.109(3) 0.0393(16) 0.091(3) -0.0196(16) 0.060(2) 0.0060(17)
N2 0.0235(15) 0.0273(15) 0.0225(15) -0.0008(12) -0.0026(12) -0.0004(12)
F10 0.0398(16) 0.0374(15) 0.122(3) -0.0002(17) -0.0361(18) -0.0074(13)
F15 0.0333(15) 0.102(3) 0.072(2) -0.027(2) 0.0106(14) -0.0266(16)
O1 0.0474(18) 0.0455(18) 0.0265(15) -0.0014(13) -0.0124(13) 0.0094(14)
F18 0.079(2) 0.0253(13) 0.112(3) 0.0206(15) 0.053(2) 0.0135(14)
N1 0.0264(15) 0.0194(14) 0.0191(14) -0.0001(11) -0.0019(12) 0.0017(12)
F6 0.145(4) 0.062(2) 0.0434(18) 0.0096(16) 0.028(2) -0.041(2)
F14 0.099(3) 0.0284(15) 0.182(4) -0.009(2) 0.102(3) -0.0203(16)
F5 0.0503(19) 0.075(2) 0.129(3) 0.022(2) 0.036(2) -0.0156(17)
C26 0.0294(18) 0.0252(18) 0.0212(17) 0.0023(14) -0.0032(14) 0.0017(15)
C12 0.0279(18) 0.0163(15) 0.0214(17) -0.0016(13) -0.0026(14) 0.0011(14)
C7 0.0224(17) 0.0250(18) 0.032(2) 0.0008(15) -0.0047(15) -0.0011(14)
C11 0.0254(17) 0.0189(16) 0.0247(18) -0.0003(13) -0.0033(14) 0.0011(14)
F2 0.063(2) 0.092(3) 0.196(5) -0.053(3) 0.076(3) -0.003(2)
C4 0.0334(19) 0.0205(16) 0.0219(17) 0.0001(13) -0.0019(15) 0.0015(15)
F1 0.266(7) 0.100(3) 0.063(2) 0.030(2) 0.095(3) 0.105(4)
C10 0.0233(18) 0.049(2) 0.0234(18) 0.0019(17) -0.0003(15) -0.0035(17)
C14 0.0323(19) 0.0303(19) 0.0204(17) -0.0025(15) 0.0023(15) 0.0089(16)
C25 0.039(2) 0.0218(17) 0.0250(18) -0.0033(14) 0.0021(16) -0.0050(16)
C22 0.0254(18) 0.036(2) 0.0266(19) 0.0037(16) -0.0014(15) -0.0008(16)
C19 0.0249(17) 0.0296(19) 0.0206(17) -0.0023(14) 0.0013(14) -0.0004(15)
C6 0.031(2) 0.0238(18) 0.036(2) -0.0004(16) -0.0085(17) 0.0002(15)
C16 0.0225(17) 0.0249(18) 0.0277(18) 0.0015(15) 0.0018(14) -0.0029(14)
C21 0.0261(18) 0.0250(17) 0.0230(17) -0.0006(14) -0.0035(14) -0.0011(15)
C15 0.033(2) 0.0247(18) 0.032(2) 0.0011(16) 0.0022(16) 0.0053(16)
C27 0.036(2) 0.0253(19) 0.035(2) 0.0028(16) 0.0040(17) 0.0036(16)
C8 0.0243(19) 0.042(2) 0.041(2) 0.0019(19) -0.0024(17) -0.0012(17)
C20 0.0259(18) 0.038(2) 0.0208(17) 0.0048(16) 0.0002(14) -0.0001(16)
C9 0.025(2) 0.058(3) 0.033(2) 0.005(2) 0.0055(17) -0.0015(19)
C24 0.0300(19) 0.0319(19) 0.0181(16) -0.0016(14) 0.0051(14) -0.0079(16)
C3E 0.046(3) 0.028(2) 0.049(3) 0.0016(19) -0.003(2) -0.0028(19)
C1 0.0298(19) 0.0265(18) 0.0255(18) 0.0032(15) 0.0065(15) 0.0027(15)
C3 0.046(2) 0.0261(19) 0.0211(18) 0.0009(15) -0.0009(17) 0.0037(17)
C5 0.040(2) 0.0234(18) 0.0245(19) -0.0027(14) -0.0083(16) 0.0037(16)
C18 0.031(2) 0.055(3) 0.0203(18) -0.0004(18) 0.0024(15) 0.0040(19)
C2 0.045(2) 0.0290(19) 0.0187(17) 0.0013(15) 0.0081(16) 0.0020(17)
C23 0.050(3) 0.034(2) 0.055(3) -0.011(2) 0.026(2) -0.013(2)
C17 0.049(3) 0.027(2) 0.049(3) 0.0002(19) 0.019(2) -0.0036(19)
C13 0.065(3) 0.040(3) 0.048(3) 0.010(2) 0.032(2) 0.018(2)
C4E 0.056(3) 0.031(2) 0.053(3) 0.000(2) -0.013(2) -0.001(2)
C1EA 0.050(6) 0.074(8) 0.044(6) 0.012(6) 0.006(5) -0.007(6)
C2EA 0.042(6) 0.038(5) 0.041(6) -0.005(4) 0.005(5) -0.006(5)
C1EB 0.039(5) 0.048(6) 0.050(6) -0.001(5) -0.008(5) -0.007(5)
C2EB 0.054(6) 0.044(5) 0.017(4) -0.001(4) -0.001(4) -0.017(5)
_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
Y1 O5 2.321(2) . ?
Y1 O8 2.301(3) . ?
Y1 O6 2.311(2) . ?
Y1 O3 2.341(3) . ?
Y1 O7 2.304(3) . ?
Y1 O4 2.328(3) . ?
Y1 N2 2.520(3) . ?
Y1 N1 2.523(3) . ?
F17 C27 1.327(5) . ?
O5 C19 1.251(4) . ?
F12 C22 1.335(5) . ?
O8 C26 1.250(4) . ?
F11 C22 1.336(4) . ?
F7 C18 1.330(5) . ?
O6 C21 1.262(4) . ?
O3 C14 1.251(5) . ?
O7 C24 1.265(5) . ?
O4 C16 1.245(4) . ?
F13 C23 1.337(5) . ?
F8 C18 1.325(5) . ?
F16 C27 1.321(5) . ?
F9 C18 1.322(5) . ?
O2 C6 1.221(5) . ?
F4 C17 1.314(5) . ?
F3 C13 1.296(6) . ?
N2 C11 1.357(5) . ?
N2 C10 1.341(5) . ?
F10 C22 1.304(5) . ?
F15 C23 1.327(6) . ?
O1 C5 1.223(5) . ?
F18 C27 1.330(5) . ?
N1 C12 1.354(5) . ?
N1 C1 1.344(5) . ?
F6 C17 1.294(6) . ?
F14 C23 1.346(6) . ?
F5 C17 1.329(6) . ?
C26 C25 1.385(6) . ?
C26 C27 1.530(5) . ?
C12 C11 1.453(5) . ?
C12 C4 1.400(5) . ?
C7 C11 1.405(5) . ?
C7 C6 1.478(6) . ?
C7 C8 1.378(6) . ?
F2 C13 1.310(7) . ?
C4 C3 1.379(6) . ?
C4 C5 1.488(6) . ?
F1 C13 1.305(6) . ?
C10 H10 0.9500 . ?
C10 C9 1.381(5) . ?
C14 C15 1.385(6) . ?
C14 C13 1.531(6) . ?
C25 H25 0.9500 . ?
C25 C24 1.384(6) . ?
C22 C21 1.532(5) . ?
C19 C20 1.398(5) . ?
C19 C18 1.530(6) . ?
C6 C5 1.536(6) . ?
C16 C15 1.383(6) . ?
C16 C17 1.535(6) . ?
C21 C20 1.380(5) . ?
C15 H15 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.376(6) . ?
C20 H20 0.9500 . ?
C9 H9 0.9500 . ?
C24 C23 1.512(6) . ?
C3E H3EC 0.9900 . ?
C3E H3ED 0.9900 . ?
C3E H3EA 0.9900 . ?
C3E H3EB 0.9900 . ?
C3E C4E 1.489(6) . ?
C3E O10 1.448(6) . ?
C3E O11 1.435(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.392(5) . ?
C3 H3 0.9500 . ?
C3 C2 1.376(6) . ?
C2 H2 0.9500 . ?
C4E H4EA 0.9800 . ?
C4E H4EB 0.9800 . ?
C4E H4EC 0.9800 . ?
C1EA H1EA 0.9800 . ?
C1EA H1EB 0.9800 . ?
C1EA H1EC 0.9800 . ?
C1EA C2EA 1.483(11) . ?
O10 C2EB 1.424(7) . ?
C2EA H2EA 0.9900 . ?
C2EA H2EB 0.9900 . ?
C2EA O11 1.437(8) . ?
C1EB H1ED 0.9800 . ?
C1EB H1EE 0.9800 . ?
C1EB H1EF 0.9800 . ?
C1EB C2EB 1.503(11) . ?
C2EB H2EC 0.9900 . ?
C2EB H2ED 0.9900 . ?
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
O5 Y1 O3 136.58(9) . . ?
O5 Y1 O4 71.05(9) . . ?
O5 Y1 N2 81.17(10) . . ?
O5 Y1 N1 143.28(9) . . ?
O8 Y1 O5 75.52(9) . . ?
O8 Y1 O6 113.08(9) . . ?
O8 Y1 O3 147.65(9) . . ?
O8 Y1 O7 73.57(9) . . ?
O8 Y1 O4 136.54(9) . . ?
O8 Y1 N2 73.48(10) . . ?
O8 Y1 N1 82.73(9) . . ?
O6 Y1 O5 74.06(9) . . ?
O6 Y1 O3 79.91(9) . . ?
O6 Y1 O4 83.54(9) . . ?
O6 Y1 N2 151.24(10) . . ?
O6 Y1 N1 142.48(10) . . ?
O3 Y1 N2 109.95(10) . . ?
O3 Y1 N1 71.22(9) . . ?
O7 Y1 O5 122.29(9) . . ?
O7 Y1 O6 75.13(9) . . ?
O7 Y1 O3 82.19(9) . . ?
O7 Y1 O4 149.01(9) . . ?
O7 Y1 N2 131.89(10) . . ?
O7 Y1 N1 77.61(9) . . ?
O4 Y1 O3 72.01(9) . . ?
O4 Y1 N2 74.64(10) . . ?
O4 Y1 N1 108.75(9) . . ?
N2 Y1 N1 64.29(10) . . ?
C19 O5 Y1 130.9(2) . . ?
C26 O8 Y1 135.6(2) . . ?
C21 O6 Y1 132.1(2) . . ?
C14 O3 Y1 135.1(3) . . ?
C24 O7 Y1 134.3(2) . . ?
C16 O4 Y1 136.5(2) . . ?
C11 N2 Y1 120.6(2) . . ?
C10 N2 Y1 121.2(2) . . ?
C10 N2 C11 118.1(3) . . ?
C12 N1 Y1 120.9(2) . . ?
C1 N1 Y1 121.2(2) . . ?
C1 N1 C12 117.9(3) . . ?
O8 C26 C25 127.2(4) . . ?
O8 C26 C27 113.4(3) . . ?
C25 C26 C27 119.4(3) . . ?
N1 C12 C11 116.7(3) . . ?
N1 C12 C4 121.5(4) . . ?
C4 C12 C11 121.8(3) . . ?
C11 C7 C6 120.3(4) . . ?
C8 C7 C11 119.4(4) . . ?
C8 C7 C6 120.3(4) . . ?
N2 C11 C12 117.2(3) . . ?
N2 C11 C7 121.1(4) . . ?
C7 C11 C12 121.7(3) . . ?
C12 C4 C5 119.9(4) . . ?
C3 C4 C12 119.2(4) . . ?
C3 C4 C5 120.9(3) . . ?
N2 C10 H10 118.2 . . ?
N2 C10 C9 123.5(4) . . ?
C9 C10 H10 118.2 . . ?
O3 C14 C15 128.4(4) . . ?
O3 C14 C13 114.4(4) . . ?
C15 C14 C13 117.2(4) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 C26 120.8(3) . . ?
C24 C25 H25 119.6 . . ?
F12 C22 F11 105.1(3) . . ?
F12 C22 C21 111.5(3) . . ?
F11 C22 C21 112.5(3) . . ?
F10 C22 F12 108.7(4) . . ?
F10 C22 F11 107.8(3) . . ?
F10 C22 C21 111.0(3) . . ?
O5 C19 C20 127.3(4) . . ?
O5 C19 C18 115.2(3) . . ?
C20 C19 C18 117.5(3) . . ?
O2 C6 C7 122.6(4) . . ?
O2 C6 C5 119.4(4) . . ?
C7 C6 C5 117.9(3) . . ?
O4 C16 C15 127.8(4) . . ?
O4 C16 C17 113.2(3) . . ?
C15 C16 C17 119.0(3) . . ?
O6 C21 C22 114.9(3) . . ?
O6 C21 C20 127.8(3) . . ?
C20 C21 C22 117.2(3) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 C14 119.7(4) . . ?
C16 C15 H15 120.1 . . ?
F17 C27 F18 106.1(3) . . ?
F17 C27 C26 111.0(3) . . ?
F16 C27 F17 106.7(3) . . ?
F16 C27 F18 108.3(4) . . ?
F16 C27 C26 111.1(3) . . ?
F18 C27 C26 113.2(3) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 C7 119.3(4) . . ?
C9 C8 H8 120.3 . . ?
C19 C20 H20 119.3 . . ?
C21 C20 C19 121.4(3) . . ?
C21 C20 H20 119.3 . . ?
C10 C9 H9 120.7 . . ?
C8 C9 C10 118.6(4) . . ?
C8 C9 H9 120.7 . . ?
O7 C24 C25 127.9(4) . . ?
O7 C24 C23 113.3(4) . . ?
C25 C24 C23 118.8(4) . . ?
H3EC C3E H3ED 108.5 . . ?
H3EA C3E H3EB 108.0 . . ?
C4E C3E H3EC 110.2 . . ?
C4E C3E H3ED 110.2 . . ?
C4E C3E H3EA 109.4 . . ?
C4E C3E H3EB 109.4 . . ?
O10 C3E H3EC 110.2 . . ?
O10 C3E H3ED 110.2 . . ?
O10 C3E C4E 107.7(4) . . ?
O11 C3E H3EA 109.4 . . ?
O11 C3E H3EB 109.4 . . ?
O11 C3E C4E 111.2(4) . . ?
N1 C1 H1 118.2 . . ?
N1 C1 C2 123.6(4) . . ?
C2 C1 H1 118.2 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 120.0(4) . . ?
C2 C3 H3 120.0 . . ?
O1 C5 C4 121.9(4) . . ?
O1 C5 C6 119.9(4) . . ?
C4 C5 C6 118.1(3) . . ?
F7 C18 C19 112.2(3) . . ?
F8 C18 F7 107.3(4) . . ?
F8 C18 C19 111.0(3) . . ?
F9 C18 F7 107.1(3) . . ?
F9 C18 F8 107.8(4) . . ?
F9 C18 C19 111.2(4) . . ?
C1 C2 H2 121.1 . . ?
C3 C2 C1 117.8(4) . . ?
C3 C2 H2 121.1 . . ?
F13 C23 F14 105.2(4) . . ?
F13 C23 C24 111.0(4) . . ?
F15 C23 F13 106.5(4) . . ?
F15 C23 F14 108.5(4) . . ?
F15 C23 C24 111.9(4) . . ?
F14 C23 C24 113.3(4) . . ?
F4 C17 F5 105.0(4) . . ?
F4 C17 C16 113.7(4) . . ?
F6 C17 F4 110.0(4) . . ?
F6 C17 F5 106.5(4) . . ?
F6 C17 C16 111.2(4) . . ?
F5 C17 C16 110.1(4) . . ?
F3 C13 F2 105.7(4) . . ?
F3 C13 F1 109.5(5) . . ?
F3 C13 C14 115.0(4) . . ?
F2 C13 C14 110.6(4) . . ?
F1 C13 F2 104.3(5) . . ?
F1 C13 C14 111.1(4) . . ?
C3E C4E H4EA 109.5 . . ?
C3E C4E H4EB 109.5 . . ?
C3E C4E H4EC 109.5 . . ?
H4EA C4E H4EB 109.5 . . ?
H4EA C4E H4EC 109.5 . . ?
H4EB C4E H4EC 109.5 . . ?
H1EA C1EA H1EB 109.5 . . ?
H1EA C1EA H1EC 109.5 . . ?
H1EB C1EA H1EC 109.5 . . ?
C2EA C1EA H1EA 109.5 . . ?
C2EA C1EA H1EB 109.5 . . ?
C2EA C1EA H1EC 109.5 . . ?
C2EB O10 C3E 113.3(6) . . ?
C1EA C2EA H2EA 108.7 . . ?
C1EA C2EA H2EB 108.7 . . ?
H2EA C2EA H2EB 107.6 . . ?
O11 C2EA C1EA 114.3(9) . . ?
O11 C2EA H2EA 108.7 . . ?
O11 C2EA H2EB 108.7 . . ?
C3E O11 C2EA 111.4(6) . . ?
H1ED C1EB H1EE 109.5 . . ?
H1ED C1EB H1EF 109.5 . . ?
H1EE C1EB H1EF 109.5 . . ?
C2EB C1EB H1ED 109.5 . . ?
C2EB C1EB H1EE 109.5 . . ?
C2EB C1EB H1EF 109.5 . . ?
O10 C2EB C1EB 114.7(9) . . ?
O10 C2EB H2EC 108.6 . . ?
O10 C2EB H2ED 108.6 . . ?
C1EB C2EB H2EC 108.6 . . ?
C1EB C2EB H2ED 108.6 . . ?
H2EC C2EB H2ED 107.6 . . ?
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
Y1 O5 C19 C20 -24.0(6) . . . . ?
Y1 O5 C19 C18 156.8(3) . . . . ?
Y1 O8 C26 C25 -4.0(6) . . . . ?
Y1 O8 C26 C27 177.2(2) . . . . ?
Y1 O6 C21 C22 -170.7(2) . . . . ?
Y1 O6 C21 C20 11.2(6) . . . . ?
Y1 O3 C14 C15 8.3(6) . . . . ?
Y1 O3 C14 C13 -171.6(3) . . . . ?
Y1 O7 C24 C25 2.7(6) . . . . ?
Y1 O7 C24 C23 -177.0(3) . . . . ?
Y1 O4 C16 C15 5.4(6) . . . . ?
Y1 O4 C16 C17 -174.7(3) . . . . ?
Y1 N2 C11 C12 -5.6(4) . . . . ?
Y1 N2 C11 C7 176.1(3) . . . . ?
Y1 N2 C10 C9 -176.5(4) . . . . ?
Y1 N1 C12 C11 2.1(4) . . . . ?
Y1 N1 C12 C4 179.6(2) . . . . ?
Y1 N1 C1 C2 -177.0(3) . . . . ?
O5 C19 C20 C21 0.7(6) . . . . ?
O5 C19 C18 F7 -159.6(3) . . . . ?
O5 C19 C18 F8 -39.6(5) . . . . ?
O5 C19 C18 F9 80.5(4) . . . . ?
F12 C22 C21 O6 36.2(5) . . . . ?
F12 C22 C21 C20 -145.5(4) . . . . ?
O8 C26 C25 C24 -4.5(6) . . . . ?
O8 C26 C27 F17 -61.5(4) . . . . ?
O8 C26 C27 F16 57.2(5) . . . . ?
O8 C26 C27 F18 179.3(4) . . . . ?
F11 C22 C21 O6 154.0(3) . . . . ?
F11 C22 C21 C20 -27.7(5) . . . . ?
O6 C21 C20 C19 6.1(6) . . . . ?
O3 C14 C15 C16 -2.7(6) . . . . ?
O3 C14 C13 F3 168.3(4) . . . . ?
O3 C14 C13 F2 -72.1(5) . . . . ?
O3 C14 C13 F1 43.2(7) . . . . ?
O7 C24 C23 F13 -57.1(5) . . . . ?
O7 C24 C23 F15 61.7(5) . . . . ?
O7 C24 C23 F14 -175.3(4) . . . . ?
O4 C16 C15 C14 -4.0(6) . . . . ?
O4 C16 C17 F4 179.9(4) . . . . ?
O4 C16 C17 F6 55.1(5) . . . . ?
O4 C16 C17 F5 -62.6(5) . . . . ?
O2 C6 C5 O1 0.3(6) . . . . ?
O2 C6 C5 C4 -177.3(3) . . . . ?
N2 C10 C9 C8 0.2(7) . . . . ?
F10 C22 C21 O6 -85.1(4) . . . . ?
F10 C22 C21 C20 93.2(4) . . . . ?
N1 C12 C11 N2 2.3(5) . . . . ?
N1 C12 C11 C7 -179.5(3) . . . . ?
N1 C12 C4 C3 -2.4(5) . . . . ?
N1 C12 C4 C5 176.5(3) . . . . ?
N1 C1 C2 C3 -2.7(6) . . . . ?
C26 C25 C24 O7 5.1(6) . . . . ?
C26 C25 C24 C23 -175.3(4) . . . . ?
C12 N1 C1 C2 1.4(5) . . . . ?
C12 C4 C3 C2 1.0(5) . . . . ?
C12 C4 C5 O1 -173.5(4) . . . . ?
C12 C4 C5 C6 4.0(5) . . . . ?
C7 C6 C5 O1 178.5(4) . . . . ?
C7 C6 C5 C4 1.0(5) . . . . ?
C7 C8 C9 C10 0.2(7) . . . . ?
C11 N2 C10 C9 -0.2(6) . . . . ?
C11 C12 C4 C3 175.0(3) . . . . ?
C11 C12 C4 C5 -6.1(5) . . . . ?
C11 C7 C6 O2 174.2(4) . . . . ?
C11 C7 C6 C5 -4.0(5) . . . . ?
C11 C7 C8 C9 -0.6(6) . . . . ?
C4 C12 C11 N2 -175.2(3) . . . . ?
C4 C12 C11 C7 3.0(5) . . . . ?
C4 C3 C2 C1 1.4(5) . . . . ?
C10 N2 C11 C12 178.0(3) . . . . ?
C10 N2 C11 C7 -0.2(5) . . . . ?
C25 C26 C27 F17 119.7(4) . . . . ?
C25 C26 C27 F16 -121.7(4) . . . . ?
C25 C26 C27 F18 0.5(5) . . . . ?
C25 C24 C23 F13 123.2(4) . . . . ?
C25 C24 C23 F15 -118.0(4) . . . . ?
C25 C24 C23 F14 5.0(6) . . . . ?
C22 C21 C20 C19 -172.0(4) . . . . ?
C6 C7 C11 N2 -179.6(3) . . . . ?
C6 C7 C11 C12 2.2(5) . . . . ?
C6 C7 C8 C9 179.6(4) . . . . ?
C15 C14 C13 F3 -11.6(6) . . . . ?
C15 C14 C13 F2 107.9(5) . . . . ?
C15 C14 C13 F1 -136.7(5) . . . . ?
C15 C16 C17 F4 -0.1(6) . . . . ?
C15 C16 C17 F6 -124.9(4) . . . . ?
C15 C16 C17 F5 117.3(4) . . . . ?
C27 C26 C25 C24 174.2(3) . . . . ?
C8 C7 C11 N2 0.6(6) . . . . ?
C8 C7 C11 C12 -177.6(4) . . . . ?
C8 C7 C6 O2 -6.0(6) . . . . ?
C8 C7 C6 C5 175.8(4) . . . . ?
C20 C19 C18 F7 21.1(5) . . . . ?
C20 C19 C18 F8 141.2(4) . . . . ?
C20 C19 C18 F9 -98.8(4) . . . . ?
C3E O10 C2EB C1EB -72.6(10) . . . . ?
C1 N1 C12 C11 -176.3(3) . . . . ?
C1 N1 C12 C4 1.2(5) . . . . ?
C3 C4 C5 O1 5.4(6) . . . . ?
C3 C4 C5 C6 -177.1(3) . . . . ?
C5 C4 C3 C2 -177.9(3) . . . . ?
C18 C19 C20 C21 179.8(4) . . . . ?
C17 C16 C15 C14 176.1(4) . . . . ?
C13 C14 C15 C16 177.2(4) . . . . ?
C4E C3E O10 C2EB -167.7(7) . . . . ?
C4E C3E O11 C2EA 178.2(7) . . . . ?
C1EA C2EA O11 C3E 74.6(11) . . . . ?
_shelx_res_file
;
TITL mo_jhgla025_0m_a.res in P2(1)/c
mo_jhgla025_0m.res
created by SHELXL-2016/6 at 11:32:42 on 23-Mar-2018
REM Old TITL mo_JHGLA025_0m in P21/c #14
REM SHELXT solution in P2(1)/c
REM R1 0.197, Rweak 0.010, Alpha 0.088, Orientation as input
REM Formula found by SHELXT: C32 N2 O8 F18 Y
CELL 0.71073 9.6263 22.7963 17.0279 90 99.176 90
ZERR 4 0.0003 0.0008 0.0006 0 0.001 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H F N O Y
UNIT 124 76 72 8 36 4
DFIX 1.43 0.01 O11 C2EA O11 C3E O10 C3E O10 C2EB
SADI C4E C3E C2EA C1EA C1EB C2EB
L.S. 4
PLAN 10
SIZE 0.05 0.05 0.27
TEMP -173.15
conf
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.089000 5.862000
FVAR 0.16993
Y1 6 0.228702 0.574040 0.709790 11.00000 0.01870 0.02011 =
0.01783 0.00039 0.00032 -0.00043
F17 3 0.420499 0.379681 0.653995 11.00000 0.03923 0.04165 =
0.03177 -0.00384 0.00820 0.01206
O5 5 0.306314 0.559767 0.588968 11.00000 0.02464 0.02505 =
0.01814 -0.00088 0.00257 0.00205
F12 3 -0.206446 0.634704 0.548116 11.00000 0.03509 0.07697 =
0.03556 0.00680 0.00359 0.02193
O8 5 0.321325 0.480797 0.718281 11.00000 0.02597 0.02317 =
0.03026 0.00200 0.00215 0.00038
F11 3 -0.140615 0.639412 0.435214 11.00000 0.03609 0.06523 =
0.02975 0.01385 -0.00316 0.01227
F7 3 0.324191 0.616673 0.402293 11.00000 0.04048 0.07350 =
0.03139 0.02121 0.01057 0.00642
O6 5 0.031846 0.583011 0.613274 11.00000 0.01996 0.03533 =
0.02003 -0.00195 0.00027 -0.00050
O3 5 0.106171 0.646832 0.767471 11.00000 0.02815 0.02580 =
0.03006 0.00657 0.00023 0.00358
O7 5 0.062312 0.514422 0.752320 11.00000 0.02769 0.02416 =
0.02827 0.00051 -0.00044 -0.00285
O4 5 0.288038 0.664457 0.660916 11.00000 0.02657 0.02288 =
0.03255 -0.00239 0.00542 -0.00199
F13 3 -0.101780 0.468703 0.855469 11.00000 0.06110 0.04488 =
0.04674 0.00533 0.03507 0.00208
F8 3 0.489173 0.599183 0.499302 11.00000 0.02981 0.12610 =
0.02974 0.00869 0.00244 -0.01489
F16 3 0.501852 0.391816 0.776404 11.00000 0.05973 0.06716 =
0.04483 -0.01637 -0.02676 0.03566
F9 3 0.383249 0.528314 0.432440 11.00000 0.07523 0.06341 =
0.05459 -0.00591 0.03567 0.01973
O2 5 0.872787 0.575268 0.970872 11.00000 0.02969 0.04129 =
0.04117 -0.00100 -0.01367 0.00317
F4 3 0.286309 0.813952 0.622999 11.00000 0.10889 0.02604 =
0.11125 0.01504 0.06797 0.00290
F3 3 0.036423 0.785605 0.835211 11.00000 0.10930 0.03928 =
0.09078 -0.01963 0.05964 0.00599
N2 4 0.489356 0.585038 0.756158 11.00000 0.02346 0.02726 =
0.02248 -0.00083 -0.00263 -0.00045
F10 3 -0.199505 0.556715 0.478457 11.00000 0.03978 0.03738 =
0.12202 -0.00019 -0.03607 -0.00738
F15 3 -0.196795 0.456709 0.734475 11.00000 0.03325 0.10160 =
0.07157 -0.02734 0.01057 -0.02661
O1 5 0.685020 0.568189 1.076177 11.00000 0.04735 0.04546 =
0.02649 -0.00141 -0.01239 0.00944
F18 3 0.337676 0.329004 0.740352 11.00000 0.07876 0.02534 =
0.11236 0.02061 0.05291 0.01355
N1 4 0.306397 0.572400 0.858488 11.00000 0.02643 0.01942 =
0.01912 -0.00014 -0.00190 0.00172
F6 3 0.288228 0.743188 0.540890 11.00000 0.14470 0.06217 =
0.04344 0.00957 0.02776 -0.04078
F14 3 -0.093575 0.384178 0.802835 11.00000 0.09908 0.02840 =
0.18211 -0.00870 0.10203 -0.02032
F5 3 0.459658 0.757258 0.632011 11.00000 0.05034 0.07482 =
0.12887 0.02191 0.03642 -0.01564
C26 1 0.276862 0.430732 0.730901 11.00000 0.02936 0.02522 =
0.02123 0.00227 -0.00316 0.00175
C12 1 0.444568 0.574905 0.890131 11.00000 0.02794 0.01634 =
0.02135 -0.00160 -0.00265 0.00115
C7 1 0.689572 0.583136 0.860512 11.00000 0.02237 0.02501 =
0.03231 0.00079 -0.00465 -0.00106
C11 1 0.543659 0.580608 0.834497 11.00000 0.02544 0.01888 =
0.02471 -0.00029 -0.00334 0.00106
F2 3 -0.116201 0.722313 0.800227 11.00000 0.06281 0.09220 =
0.19619 -0.05274 0.07566 -0.00255
C4 1 0.489007 0.574389 0.972523 11.00000 0.03340 0.02055 =
0.02189 0.00005 -0.00186 0.00150
F1 3 0.041519 0.703214 0.893890 11.00000 0.26621 0.10016 =
0.06310 0.02956 0.09521 0.10545
C10 1 0.579009 0.592090 0.704184 11.00000 0.02328 0.04854 =
0.02342 0.00189 -0.00031 -0.00354
AFIX 43
H10 2 0.541291 0.595071 0.649271 11.00000 -1.20000
AFIX 0
C14 1 0.105032 0.701702 0.766730 11.00000 0.03233 0.03030 =
0.02045 -0.00252 0.00225 0.00890
C25 1 0.146126 0.416312 0.749403 11.00000 0.03898 0.02179 =
0.02501 -0.00327 0.00210 -0.00500
AFIX 43
H25 2 0.121573 0.376241 0.754035 11.00000 -1.20000
AFIX 0
C22 1 -0.134097 0.605669 0.499843 11.00000 0.02538 0.03579 =
0.02661 0.00368 -0.00138 -0.00079
C19 1 0.258596 0.577944 0.520690 11.00000 0.02492 0.02958 =
0.02055 -0.00233 0.00127 -0.00040
C6 1 0.746789 0.577864 0.946065 11.00000 0.03060 0.02378 =
0.03574 -0.00040 -0.00854 0.00024
C16 1 0.255477 0.716688 0.669314 11.00000 0.02246 0.02493 =
0.02769 0.00152 0.00181 -0.00290
C21 1 0.017480 0.594010 0.539814 11.00000 0.02607 0.02497 =
0.02297 -0.00064 -0.00349 -0.00109
C15 1 0.171146 0.739336 0.720560 11.00000 0.03339 0.02471 =
0.03244 0.00107 0.00218 0.00527
AFIX 43
H15 2 0.158617 0.780535 0.724080 11.00000 -1.20000
AFIX 0
C27 1 0.384858 0.382144 0.726033 11.00000 0.03614 0.02531 =
0.03468 0.00281 0.00401 0.00360
C8 1 0.778807 0.590778 0.805593 11.00000 0.02426 0.04176 =
0.04081 0.00186 -0.00240 -0.00123
AFIX 43
H8 2 0.877640 0.592934 0.822368 11.00000 -1.20000
AFIX 0
C20 1 0.120422 0.595102 0.491986 11.00000 0.02591 0.03813 =
0.02076 0.00485 0.00019 -0.00012
AFIX 43
H20 2 0.096884 0.607793 0.438373 11.00000 -1.20000
AFIX 0
C9 1 0.723231 0.595254 0.726176 11.00000 0.02537 0.05828 =
0.03273 0.00499 0.00547 -0.00145
AFIX 43
H9 2 0.782848 0.600412 0.687302 11.00000 -1.20000
AFIX 0
C24 1 0.050814 0.459622 0.761223 11.00000 0.02999 0.03193 =
0.01811 -0.00158 0.00508 -0.00791
C3E 1 0.612399 0.744473 0.941187 11.00000 0.04594 0.02770 =
0.04906 0.00158 -0.00277 -0.00282
PART 2
AFIX 23
H3EC 2 0.691998 0.756600 0.914551 10.50000 -1.20000
H3ED 2 0.588172 0.777548 0.974169 10.50000 -1.20000
AFIX 23
PART 0
PART 1
H3EA 2 0.673832 0.771619 0.916993 10.50000 -1.20000
H3EB 2 0.579693 0.765077 0.986052 10.50000 -1.20000
AFIX 0
PART 0
C1 1 0.212118 0.570491 0.908774 11.00000 0.02984 0.02646 =
0.02551 0.00318 0.00652 0.00265
AFIX 43
H1 2 0.115191 0.567854 0.886845 11.00000 -1.20000
AFIX 0
C3 1 0.389525 0.573478 1.022519 11.00000 0.04639 0.02615 =
0.02108 0.00095 -0.00093 0.00374
AFIX 43
H3 2 0.418246 0.573759 1.078545 11.00000 -1.20000
AFIX 0
C5 1 0.641905 0.573782 1.005015 11.00000 0.03970 0.02336 =
0.02447 -0.00269 -0.00829 0.00371
C18 1 0.365042 0.580558 0.462928 11.00000 0.03111 0.05466 =
0.02030 -0.00039 0.00242 0.00398
C2 1 0.248630 0.572163 0.991205 11.00000 0.04471 0.02904 =
0.01874 0.00135 0.00813 0.00203
AFIX 43
H2 2 0.178631 0.572389 1.024723 11.00000 -1.20000
AFIX 0
C23 1 -0.085989 0.441913 0.787600 11.00000 0.05037 0.03365 =
0.05546 -0.01147 0.02579 -0.01285
C17 1 0.320112 0.758715 0.614684 11.00000 0.04904 0.02712 =
0.04867 0.00017 0.01892 -0.00361
C13 1 0.018684 0.729587 0.825024 11.00000 0.06524 0.04013 =
0.04777 0.01010 0.03173 0.01798
C4E 1 0.488752 0.728347 0.880849 11.00000 0.05591 0.03093 =
0.05314 -0.00004 -0.01313 -0.00094
AFIX 33
H4EA 2 0.436752 0.763905 0.861876 11.00000 -1.50000
H4EB 2 0.521088 0.708530 0.835986 11.00000 -1.50000
H4EC 2 0.427042 0.701995 0.904977 11.00000 -1.50000
AFIX 0
PART 1
C1EA 1 0.782086 0.726518 1.106230 10.50000 0.05043 0.07370 =
0.04440 0.01200 0.00606 -0.00652
AFIX 33
H1EA 2 0.869992 0.736388 1.141190 10.50000 -1.50000
H1EB 2 0.719764 0.760769 1.100478 10.50000 -1.50000
H1EC 2 0.735824 0.693963 1.129374 10.50000 -1.50000
AFIX 0
PART 0
PART 2
O10 5 0.650893 0.693450 0.990476 10.50000 0.02720
PART 0
PART 1
C2EA 1 0.813385 0.709016 1.026995 10.50000 0.04165 0.03818 =
0.04133 -0.00527 0.00467 -0.00634
AFIX 23
H2EA 2 0.862463 0.741825 1.004947 10.50000 -1.20000
H2EB 2 0.878498 0.675123 1.033797 10.50000 -1.20000
AFIX 0
O11 5 0.691525 0.693500 0.970531 10.50000 0.03413
PART 0
PART 2
C1EB 1 0.895800 0.718587 1.046340 10.50000 0.03943 0.04791 =
0.05018 -0.00070 -0.00794 -0.00650
AFIX 33
H1ED 2 0.955796 0.726833 1.097239 10.50000 -1.50000
H1EE 2 0.932488 0.684391 1.021414 10.50000 -1.50000
H1EF 2 0.895207 0.752658 1.011191 10.50000 -1.50000
AFIX 0
C2EB 1 0.748474 0.706140 1.060410 10.50000 0.05435 0.04400 =
0.01680 -0.00052 -0.00116 -0.01680
AFIX 23
H2EC 2 0.751064 0.672411 1.097239 10.50000 -1.20000
H2ED 2 0.713853 0.740549 1.087035 10.50000 -1.20000
AFIX 0
HKLF 4
REM mo_jhgla025_0m_a.res in P2(1)/c
REM R1 = 0.0538 for 6684 Fo > 4sig(Fo) and 0.0696 for all 8416 data
REM 567 parameters refined using 7 restraints
END
WGHT 0.0873 5.2135
REM Highest difference peak 0.768, deepest hole -1.022, 1-sigma level 0.105
Q1 1 0.1664 0.6116 0.7036 11.00000 0.05 0.77
Q2 1 0.1224 0.5721 0.7274 11.00000 0.05 0.74
Q3 1 -0.0354 0.7011 0.8640 11.00000 0.05 0.71
Q4 1 0.1419 0.6185 0.7614 11.00000 0.05 0.70
Q5 1 0.2657 0.6105 0.7036 11.00000 0.05 0.68
Q6 1 0.1414 0.5283 0.7599 11.00000 0.05 0.66
Q7 1 0.1972 0.7986 0.5771 11.00000 0.05 0.64
Q8 1 0.1023 0.5067 0.7971 11.00000 0.05 0.64
Q9 1 0.3372 0.5734 0.6913 11.00000 0.05 0.62
Q10 1 0.2898 0.5307 0.7182 11.00000 0.05 0.61
;
_shelx_res_checksum 577
_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_2b
_database_code_depnum_ccdc_archive 'CCDC 1832432'
_audit_update_record
;
2018-03-26 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;
# 2017ncs0758
# [Gd(hfac3)(N,N'-pd)tol
_audit_creation_date 2018-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2018/1
# start Validation Reply Form
_vrf_PLAT201_2017ncs0758
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 14 Report
RESPONSE: Disorder present in a number of the CF3 groups which were
refined with isotropic adps, as was the disordered toluene molecule.
;
_vrf_RINTA01_2017ncs0758
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The crystals were weakly diffracting even with an overnight data
collection on rotating anode source at the NCS.
;
_vrf_PLAT020_2017ncs0758
;
PROBLEM: The Value of Rint is Greater Than 0.12 ......... 0.215 Report
RESPONSE: The crystals were weakly diffracting even with an overnight data
collection on rotating anode source at the NCS.
;
_vrf_PLAT084_2017ncs0758
;
PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.38 Report
RESPONSE: The crystals were weakly diffracting even with an overnight data
collection on rotating anode source at the NCS.
;
# end Validation Reply Form
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C27 H9 F18 Gd N2 O8, C7 H8'
_chemical_formula_sum 'C34 H17 F18 Gd N2 O8'
_chemical_formula_weight 1080.74
_chemical_melting_point ?
_chemical_oxdiff_formula 'C27 H9 N2 O8 F18 Gd'
_chemical_oxdiff_usercomment SHOI-015
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 12.9683(18)
_cell_length_b 16.576(3)
_cell_length_c 18.018(2)
_cell_angle_alpha 90
_cell_angle_beta 103.338(15)
_cell_angle_gamma 90
_cell_volume 3768.9(10)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 2420
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 56.2240
_cell_measurement_theta_min 3.4910
_shelx_estimated_absorpt_T_max 0.702
_shelx_estimated_absorpt_T_min 0.569
_exptl_absorpt_coefficient_mu 12.716
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.40183
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.905
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2100
_exptl_crystal_size_max 0.05
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.03
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.2149
_diffrn_reflns_av_unetI/netI 0.2252
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 24190
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 68.245
_diffrn_reflns_theta_min 3.502
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100(2)
_diffrn_detector 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime 0.000
_diffrn_detector_type 'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -74.00 -48.00 0.50 28.00 -- -90.00 34.00-130.00 52
2 \w -42.00 -4.00 0.50 28.00 -- -90.00 34.00-130.00 76
3 \w -178.00-108.00 0.50 28.00 -- -90.00 34.00-130.00 140
4 \w 39.00 65.00 0.50 7.00 -- 0.00 34.00-130.00 52
5 \w -87.00 88.00 0.50 7.00 -- 0.00 60.00-150.00 350
6 \w -82.00 -56.00 0.50 7.00 -- 0.00 34.00-130.00 52
7 \w -19.00 6.00 0.50 28.00 -- 5.00 34.00-130.00 50
8 \w -165.00-139.00 0.50 28.00 -- -90.00 60.00 120.00 52
9 \w -124.00 -97.00 0.50 28.00 -- -90.00 60.00 150.00 54
10 \w -172.00 -1.00 0.50 28.00 -- -90.00 29.00 90.00 342
11 \w -176.00-135.00 0.50 28.00 -- -90.00 29.00 0.00 82
12 \w -70.00 -44.00 0.50 28.00 -- -90.00 57.00 -30.00 52
13 \w -113.00 -8.00 0.50 28.00 -- -90.00 29.00 0.00 210
14 \w -44.00 -10.00 0.50 28.00 -- -90.00 60.00 150.00 68
15 \w -132.00 -2.00 0.50 28.00 -- -90.00 60.00 120.00 260
16 \w -69.00 -20.00 0.50 28.00 -- -90.00 29.00 -60.00 98
17 \w -161.00-108.00 0.50 28.00 -- -90.00 29.00 -60.00 106
18 \w -92.00 -66.00 0.50 28.00 -- -90.00 60.00 150.00 52
19 \w -178.00-100.00 0.50 28.00 -- -90.00 57.00 -30.00 156
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type 'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.1075678000
_diffrn_orient_matrix_UB_12 0.0403295000
_diffrn_orient_matrix_UB_13 -0.0343481000
_diffrn_orient_matrix_UB_21 -0.0447406000
_diffrn_orient_matrix_UB_22 -0.0339650000
_diffrn_orient_matrix_UB_23 0.0656390000
_diffrn_orient_matrix_UB_31 0.0363981000
_diffrn_orient_matrix_UB_32 0.0766074000
_diffrn_orient_matrix_UB_33 0.0471983000
_diffrn_radiation_collimation 'Varimax focusing mirrors'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_source 'Rotating anode'
_diffrn_source_current 30.0
_diffrn_source_power 1.2
_diffrn_source_target Cu
_diffrn_source_type 'Rigaku 007 HF'
_diffrn_source_voltage 40.0
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2780
_reflns_number_total 6759
_reflns_odcompleteness_completeness 97.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 68.13
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.311
_refine_diff_density_min -0.776
_refine_diff_density_rms 0.145
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.987
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 526
_refine_ls_number_reflns 6759
_refine_ls_number_restraints 219
_refine_ls_R_factor_all 0.2532
_refine_ls_R_factor_gt 0.1180
_refine_ls_restrained_S_all 0.990
_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^)+(0.1980P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2952
_refine_ls_wR_factor_ref 0.3797
_refine_special_details
;
Several CF3 groups showed disorder and were modelled over 2 partially
occupied sites with competitively refined occupancies, suitable distance
restraints and isotropic adps (also C27 was modelled with isotropic adps).
The lattice toluene molecule was also disordered and modelled over
2 0.5 occupied sites with isotropic adps.
;
_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. Restrained distances
F17A-C27 \\sim F17-C27 \\sim F16A-C27 \\sim F16-C27 \\sim F18A-C27 \\sim
F18-C27
with sigma of 0.02
F12A-C22 \\sim F11A-C22 \\sim F12-C22 \\sim F10-C22 \\sim F11-C22 \\sim
F10A-C22 \\sim C23-F13 \\sim C23-
F15 \\sim C23-F14 \\sim F17-C27 \\sim F18-C27 \\sim F16-C27 \\sim F13-C23
\\sim F14-C23 \\sim F15-C23 ~
C23-F14A \\sim C23-F13A \\sim C23-F15A
with sigma of 0.02
F18-F16 \\sim F17-F16 \\sim F18-F17 \\sim F18A-F16A \\sim F18A-F17A \\sim
F16A-F17A \\sim F13-F15 ~
F13-F14 \\sim F15-F14 \\sim F14A-F13A \\sim F14A-F15A \\sim F13A-F15A
with sigma of 0.02
3. Others
Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(1)
Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(2)
Sof(F16)=Sof(F17)=Sof(F18)=FVAR(2)
Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(3)
Sof(F13)=Sof(F14)=Sof(F15)=FVAR(3)
Fixed Sof: C2S(0.5) H2S(0.5) C3S(0.5) H3S(0.5) C4S(0.5) H4S(0.5) C5S(0.5)
H5S(0.5) C6S(0.5) H6S(0.5) C1S(0.5) C7S(0.5) H7SA(0.5) H7SB(0.5) H7SC(0.5)
C3T(0.5) H3T(0.5) C2T(0.5) H2T(0.5) C1T(0.5) C6T(0.5) H6T(0.5) C5T(0.5)
H5T(0.5) C4T(0.5) H4T(0.5) C7T(0.5) H7TA(0.5) H7TB(0.5) H7TC(0.5)
4.a Me refined with riding coordinates:
C7S(H7SA,H7SB,H7SC), C7T(H7TA,H7TB,H7TC)
4.b Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C15(H15), C20(H20),
C25(H25), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S), C3T(H3T), C2T(H2T),
C6T(H6T), C5T(H5T), C4T(H4T)
4.c Fitted hexagon refined as free rotating group:
C2S(C3S,C4S,C5S,C6S,C1S), C3T(C2T,C1T,C6T,C5T,C4T)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.32331(9) 0.22990(8) 0.26318(6) 0.0723(5) Uani 1 1 d . . . . .
F1 F 0.6374(11) 0.3582(11) 0.2019(8) 0.125(5) Uani 1 1 d . . . . .
F2 F 0.6777(11) 0.2330(9) 0.1975(8) 0.114(5) Uani 1 1 d . . . . .
F3 F 0.7604(10) 0.3068(8) 0.2915(7) 0.101(4) Uani 1 1 d . . . . .
F4 F 0.5559(14) 0.2136(9) 0.5345(7) 0.127(5) Uani 1 1 d . . . . .
F5 F 0.6586(13) 0.3063(11) 0.5203(7) 0.139(6) Uani 1 1 d . . . . .
F6 F 0.5003(13) 0.3323(10) 0.5180(7) 0.138(6) Uani 1 1 d . . . . .
F7 F 0.1237(12) 0.0328(10) 0.3711(8) 0.134(6) Uani 1 1 d . . . . .
F8 F 0.2663(13) -0.0370(9) 0.3880(8) 0.117(5) Uani 1 1 d . . . . .
F9 F 0.1291(12) -0.0689(10) 0.3011(8) 0.128(5) Uani 1 1 d . . . . .
F10 F 0.317(2) -0.0454(15) 0.0857(13) 0.116(9) Uiso 0.61(3) 1 d D . P A 1
F11 F 0.1675(15) 0.0101(17) 0.0402(11) 0.100(8) Uiso 0.61(3) 1 d D . P A 1
F12 F 0.311(2) 0.0683(12) 0.0347(11) 0.091(7) Uiso 0.61(3) 1 d D . P A 1
F13 F 0.1274(12) 0.3405(12) 0.4435(10) 0.097(7) Uiso 0.65(2) 1 d D . P B 1
F14 F -0.0338(12) 0.3305(13) 0.3810(10) 0.103(8) Uiso 0.65(2) 1 d D . P B 1
F15 F 0.0534(19) 0.2274(11) 0.4304(15) 0.155(12) Uiso 0.65(2) 1 d D . P B 1
F16 F -0.0253(18) 0.2545(14) 0.0668(13) 0.134(10) Uiso 0.65(3) 1 d D . P C 1
F17 F -0.1295(12) 0.2195(14) 0.1344(9) 0.082(6) Uiso 0.65(3) 1 d D . P C 1
F18 F -0.0201(19) 0.1341(12) 0.1082(16) 0.166(12) Uiso 0.65(3) 1 d D . P C 1
O1 O 0.5239(13) 0.6055(9) 0.1936(8) 0.101(5) Uani 1 1 d . . . . .
O2 O 0.4427(13) 0.5539(10) 0.0484(9) 0.113(5) Uani 1 1 d . . . . .
O3 O 0.4951(12) 0.2549(9) 0.2468(8) 0.083(4) Uani 1 1 d . . . . .
O4 O 0.4358(8) 0.2484(7) 0.3858(6) 0.065(4) Uani 1 1 d . . . . .
O5 O 0.2626(11) 0.1142(10) 0.3113(8) 0.087(4) Uani 1 1 d . . . . .
O6 O 0.3166(10) 0.1286(10) 0.1691(6) 0.078(4) Uani 1 1 d . . . . .
O7 O 0.2036(11) 0.2745(8) 0.3346(6) 0.079(4) Uani 1 1 d . . . . .
O8 O 0.1459(12) 0.2224(9) 0.1827(6) 0.084(4) Uani 1 1 d . . . . .
N1 N 0.3514(11) 0.3832(9) 0.2829(8) 0.064(4) Uani 1 1 d . . . . .
N2 N 0.3168(12) 0.3146(12) 0.1455(9) 0.074(5) Uani 1 1 d . . . . .
C1 C 0.3640(17) 0.4184(16) 0.3517(14) 0.090(7) Uani 1 1 d . . . . .
H1 H 0.343552 0.388401 0.390923 0.109 Uiso 1 1 calc R . . . .
C2 C 0.4041(17) 0.4946(17) 0.3695(12) 0.092(7) Uani 1 1 d . . . . .
H2 H 0.407161 0.517722 0.418222 0.110 Uiso 1 1 calc R . . . .
C3 C 0.4392(18) 0.5354(14) 0.3148(12) 0.088(6) Uani 1 1 d . . . . .
H3 H 0.471343 0.586739 0.326339 0.105 Uiso 1 1 calc R . . . .
C4 C 0.4290(14) 0.5041(12) 0.2436(10) 0.064(5) Uani 1 1 d . . . . .
C5 C 0.4643(16) 0.5449(14) 0.1809(13) 0.076(6) Uani 1 1 d . . . . .
C6 C 0.4317(15) 0.5096(16) 0.1004(12) 0.085(7) Uani 1 1 d . . . . .
C7 C 0.3823(16) 0.4302(15) 0.0908(13) 0.089(7) Uani 1 1 d . . . . .
C8 C 0.3530(16) 0.4021(16) 0.0174(11) 0.081(6) Uani 1 1 d . . . . .
H8 H 0.366154 0.431806 -0.024586 0.097 Uiso 1 1 calc R . . . .
C9 C 0.301(2) 0.3248(18) 0.0080(12) 0.101(8) Uani 1 1 d . . . . .
H9 H 0.276320 0.300988 -0.040792 0.121 Uiso 1 1 calc R . . . .
C10 C 0.2895(15) 0.2864(14) 0.0754(11) 0.080(6) Uani 1 1 d . . . . .
H10 H 0.258384 0.234267 0.069587 0.096 Uiso 1 1 calc R . . . .
C11 C 0.3603(15) 0.3875(16) 0.1527(10) 0.080(7) Uani 1 1 d . . . . .
C12 C 0.3803(15) 0.4284(14) 0.2306(10) 0.075(6) Uani 1 1 d . . . . .
C13 C 0.6645(18) 0.2933(17) 0.2463(14) 0.087(7) Uani 1 1 d . . . . .
C14 C 0.5826(18) 0.2734(13) 0.2902(12) 0.077(6) Uani 1 1 d . . . . .
C15 C 0.6071(15) 0.2821(14) 0.3657(12) 0.096(8) Uani 1 1 d . . . . .
H15 H 0.676576 0.298544 0.390752 0.115 Uiso 1 1 calc R . . . .
C16 C 0.5315(17) 0.2674(11) 0.4089(10) 0.066(5) Uani 1 1 d . . . . .
C17 C 0.564(2) 0.2806(14) 0.4952(16) 0.088(7) Uani 1 1 d . . . . .
C18 C 0.187(2) -0.0064(19) 0.3368(14) 0.105(9) Uani 1 1 d . . . . .
C19 C 0.2221(17) 0.0484(18) 0.2813(13) 0.093(7) Uani 1 1 d . . . . .
C20 C 0.2181(17) 0.0193(15) 0.2066(12) 0.093(7) Uani 1 1 d . . . . .
H20 H 0.181906 -0.029675 0.190417 0.112 Uiso 1 1 calc R . . . .
C21 C 0.2664(16) 0.0613(15) 0.1560(13) 0.081(6) Uani 1 1 d . . . . .
C22 C 0.2655(14) 0.0239(11) 0.0793(11) 0.091(7) Uani 1 1 d D . . . .
C23 C 0.0605(13) 0.2979(11) 0.3932(11) 0.115(9) Uani 1 1 d D . . . .
C24 C 0.101(2) 0.2723(16) 0.3261(12) 0.100(8) Uani 1 1 d . . . . .
C25 C 0.025(2) 0.2498(15) 0.2609(14) 0.114(9) Uani 1 1 d . . . . .
H25 H -0.048314 0.249508 0.261354 0.137 Uiso 1 1 calc R . . . .
C26 C 0.057(2) 0.2284(15) 0.1968(13) 0.099(8) Uani 1 1 d . . . . .
C27 C -0.0316(16) 0.2100(12) 0.1266(12) 0.126(10) Uiso 1 1 d D . . . .
F10A F 0.359(2) -0.010(3) 0.083(2) 0.118(14) Uiso 0.39(3) 1 d D . P A 2
F11A F 0.250(4) 0.0784(19) 0.0247(17) 0.112(14) Uiso 0.39(3) 1 d D . P A 2
F12A F 0.200(2) -0.0383(17) 0.0618(15) 0.077(11) Uiso 0.39(3) 1 d D . P A 2
F13A F 0.055(3) 0.3796(14) 0.3827(19) 0.121(16) Uiso 0.35(2) 1 d D . P B 2
F14A F -0.0376(15) 0.278(2) 0.3941(17) 0.100(13) Uiso 0.35(2) 1 d D . P B 2
F15A F 0.1194(17) 0.2905(18) 0.4621(11) 0.067(10) Uiso 0.35(2) 1 d D . P B 2
F16A F -0.069(5) 0.2816(18) 0.100(3) 0.29(5) Uiso 0.35(3) 1 d D . P C 2
F17A F -0.113(3) 0.171(3) 0.1423(18) 0.105(15) Uiso 0.35(3) 1 d D . P C 2
F18A F -0.006(2) 0.172(2) 0.0696(15) 0.078(12) Uiso 0.35(3) 1 d D . P C 2
C2S C 0.180(4) 0.600(3) 0.159(5) 0.123(18) Uiso 0.5 1 d . . P D 1
H2S H 0.205521 0.652464 0.172732 0.147 Uiso 0.5 1 calc R . P D 1
C3S C 0.158(5) 0.548(7) 0.2136(18) 0.15(3) Uiso 0.5 1 d G . P D 1
H3S H 0.168217 0.565020 0.265084 0.183 Uiso 0.5 1 calc R . P D 1
C4S C 0.120(5) 0.470(6) 0.193(5) 0.16(3) Uiso 0.5 1 d G . P D 1
H4S H 0.105141 0.434841 0.230708 0.191 Uiso 0.5 1 calc R . P D 1
C5S C 0.105(4) 0.445(2) 0.118(6) 0.127(19) Uiso 0.5 1 d G . P D 1
H5S H 0.079368 0.392104 0.103980 0.153 Uiso 0.5 1 calc R . P D 1
C6S C 0.127(4) 0.497(4) 0.063(2) 0.099(15) Uiso 0.5 1 d G . P D 1
H6S H 0.116671 0.479547 0.011626 0.119 Uiso 0.5 1 calc R . P D 1
C1S C 0.165(4) 0.574(3) 0.083(4) 0.102(16) Uiso 0.5 1 d G . P D 1
C7S C 0.176(5) 0.620(4) 0.027(3) 0.17(3) Uiso 0.5 1 d . . P D 1
H7SA H 0.202593 0.672770 0.047064 0.255 Uiso 0.5 1 calc R . P D 1
H7SB H 0.226627 0.594736 0.001541 0.255 Uiso 0.5 1 calc R . P D 1
H7SC H 0.107459 0.626162 -0.008871 0.255 Uiso 0.5 1 calc R . P D 1
C3T C 0.174(5) 0.603(3) 0.123(5) 0.13(2) Uiso 0.5 1 d . . P E 2
H3T H 0.194839 0.655081 0.109609 0.151 Uiso 0.5 1 calc R . P E 2
C2T C 0.170(4) 0.588(3) 0.198(4) 0.127(19) Uiso 0.5 1 d G . P E 2
H2T H 0.188055 0.628883 0.236005 0.153 Uiso 0.5 1 calc R . P E 2
C1T C 0.139(4) 0.512(4) 0.2187(15) 0.085(13) Uiso 0.5 1 d G . P E 2
C6T C 0.112(3) 0.4521(18) 0.164(4) 0.083(12) Uiso 0.5 1 d G . P E 2
H6T H 0.090918 0.400401 0.177616 0.100 Uiso 0.5 1 calc R . P E 2
C5T C 0.116(4) 0.468(5) 0.089(3) 0.101(14) Uiso 0.5 1 d G . P E 2
H5T H 0.097702 0.426598 0.051220 0.121 Uiso 0.5 1 calc R . P E 2
C4T C 0.147(5) 0.543(6) 0.069(2) 0.16(3) Uiso 0.5 1 d G . P E 2
H4T H 0.149662 0.553937 0.017215 0.187 Uiso 0.5 1 calc R . P E 2
C7T C 0.111(6) 0.500(4) 0.294(4) 0.18(3) Uiso 0.5 1 d . . P E 2
H7TA H 0.134608 0.547031 0.326265 0.274 Uiso 0.5 1 calc R . P E 2
H7TB H 0.034128 0.494196 0.285618 0.274 Uiso 0.5 1 calc R . P E 2
H7TC H 0.146183 0.451531 0.317999 0.274 Uiso 0.5 1 calc R . P E 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Gd1 0.0712(8) 0.0871(11) 0.0619(6) -0.0033(6) 0.0223(5) -0.0086(7)
F1 0.106(10) 0.157(16) 0.115(10) 0.038(10) 0.032(8) -0.001(10)
F2 0.105(10) 0.146(13) 0.106(9) -0.018(9) 0.056(8) -0.003(8)
F3 0.076(9) 0.127(12) 0.100(8) -0.002(8) 0.021(7) 0.000(8)
F4 0.196(17) 0.093(13) 0.081(8) -0.015(7) 0.011(9) -0.017(10)
F5 0.125(12) 0.210(18) 0.079(8) -0.001(9) 0.017(8) -0.056(12)
F6 0.161(13) 0.145(15) 0.112(10) -0.046(10) 0.035(9) 0.027(12)
F7 0.133(12) 0.146(14) 0.147(12) -0.033(10) 0.083(10) -0.034(10)
F8 0.141(13) 0.129(13) 0.087(8) 0.004(8) 0.038(9) -0.017(10)
F9 0.141(12) 0.141(14) 0.113(10) -0.008(10) 0.050(9) -0.035(11)
O1 0.132(14) 0.055(11) 0.118(11) 0.018(9) 0.033(10) 0.004(10)
O2 0.130(13) 0.113(14) 0.105(11) 0.020(10) 0.046(10) -0.003(10)
O3 0.066(9) 0.104(13) 0.082(9) -0.016(8) 0.021(7) 0.011(8)
O4 0.018(5) 0.098(11) 0.074(7) -0.011(6) -0.002(5) -0.006(6)
O5 0.078(10) 0.104(14) 0.078(9) 0.008(9) 0.015(7) 0.000(9)
O6 0.068(9) 0.095(12) 0.072(8) -0.004(7) 0.016(7) 0.003(8)
O7 0.081(10) 0.103(11) 0.055(7) -0.014(7) 0.019(7) -0.008(8)
O8 0.097(11) 0.111(13) 0.041(6) -0.005(6) 0.006(6) -0.004(8)
N1 0.066(10) 0.060(12) 0.072(9) 0.004(8) 0.030(7) -0.018(8)
N2 0.073(11) 0.071(13) 0.082(11) -0.004(10) 0.024(9) -0.024(10)
C1 0.080(16) 0.09(2) 0.113(18) -0.008(15) 0.045(13) -0.004(13)
C2 0.080(15) 0.11(2) 0.081(14) -0.006(14) 0.012(12) 0.033(15)
C3 0.105(17) 0.072(17) 0.085(14) -0.004(13) 0.019(12) 0.011(13)
C4 0.059(12) 0.060(15) 0.067(11) -0.005(10) 0.001(9) 0.002(10)
C5 0.076(14) 0.049(15) 0.110(16) 0.020(12) 0.032(12) -0.001(11)
C6 0.055(12) 0.13(2) 0.079(13) 0.026(14) 0.026(10) 0.005(13)
C7 0.061(14) 0.086(19) 0.115(18) 0.024(14) 0.012(12) -0.010(12)
C8 0.075(14) 0.11(2) 0.059(11) -0.009(12) 0.007(10) 0.009(13)
C9 0.13(2) 0.11(2) 0.075(13) 0.002(14) 0.049(14) 0.012(18)
C10 0.057(12) 0.11(2) 0.069(12) -0.007(12) 0.002(9) -0.002(11)
C11 0.052(12) 0.12(2) 0.071(12) 0.022(13) 0.020(10) 0.032(13)
C12 0.072(13) 0.084(18) 0.071(12) 0.009(11) 0.019(10) -0.006(12)
C13 0.065(15) 0.10(2) 0.086(15) -0.005(14) 0.008(12) 0.016(13)
C14 0.075(15) 0.088(17) 0.074(13) 0.008(11) 0.031(11) 0.009(12)
C15 0.037(11) 0.16(3) 0.091(15) 0.007(14) 0.013(10) -0.019(12)
C16 0.092(16) 0.043(12) 0.058(10) -0.006(9) 0.004(10) 0.001(11)
C17 0.081(17) 0.043(17) 0.14(2) 0.002(14) 0.027(15) -0.022(13)
C18 0.11(2) 0.13(3) 0.081(15) -0.027(16) 0.028(15) -0.056(19)
C19 0.070(15) 0.13(2) 0.085(15) 0.006(15) 0.039(12) -0.006(15)
C20 0.089(16) 0.10(2) 0.088(14) 0.011(13) 0.022(12) -0.016(13)
C21 0.063(13) 0.064(17) 0.108(16) -0.017(13) 0.006(11) -0.003(12)
C22 0.088(17) 0.08(2) 0.107(17) -0.013(15) 0.030(14) -0.010(14)
C23 0.13(2) 0.11(2) 0.12(2) -0.013(17) 0.060(19) -0.021(17)
C24 0.085(18) 0.15(2) 0.067(13) 0.003(13) 0.015(12) -0.011(15)
C25 0.11(2) 0.14(3) 0.093(17) 0.003(15) 0.037(16) 0.015(16)
C26 0.095(17) 0.13(2) 0.084(14) 0.001(13) 0.047(13) 0.000(15)
_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
Gd1 O1 2.841(18) 2_645 ?
Gd1 O3 2.351(14) . ?
Gd1 O4 2.370(11) . ?
Gd1 O5 2.316(16) . ?
Gd1 O6 2.373(14) . ?
Gd1 O7 2.352(12) . ?
Gd1 O8 2.423(14) . ?
Gd1 N1 2.580(15) . ?
Gd1 N2 2.529(16) . ?
F1 C13 1.34(3) . ?
F2 C13 1.37(3) . ?
F3 C13 1.34(2) . ?
F4 C17 1.33(2) . ?
F5 C17 1.28(2) . ?
F6 C17 1.32(2) . ?
F7 C18 1.31(3) . ?
F8 C18 1.31(3) . ?
F9 C18 1.35(3) . ?
F10 C22 1.322(14) . ?
F11 C22 1.324(14) . ?
F12 C22 1.325(14) . ?
F13 C23 1.307(14) . ?
F14 C23 1.310(14) . ?
F15 C23 1.360(14) . ?
F16 C27 1.324(15) . ?
F17 C27 1.318(14) . ?
F18 C27 1.319(14) . ?
O1 C5 1.26(2) . ?
O2 C6 1.22(2) . ?
O3 C14 1.26(2) . ?
O4 C16 1.26(2) . ?
O5 C19 1.28(3) . ?
O6 C21 1.29(2) . ?
O7 C24 1.30(3) . ?
O8 C26 1.24(2) . ?
N1 C1 1.35(3) . ?
N1 C12 1.32(2) . ?
N2 C10 1.32(2) . ?
N2 C11 1.33(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.37(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.36(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.36(2) . ?
C4 C5 1.48(2) . ?
C4 C12 1.40(3) . ?
C5 C6 1.53(3) . ?
C6 C7 1.46(3) . ?
C7 C8 1.37(3) . ?
C7 C11 1.40(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.44(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.41(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.53(3) . ?
C13 C14 1.50(3) . ?
C14 C15 1.33(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.41(3) . ?
C16 C17 1.53(3) . ?
C18 C19 1.50(3) . ?
C19 C20 1.42(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.40(3) . ?
C21 C22 1.51(3) . ?
C22 F10A 1.325(15) . ?
C22 F11A 1.318(15) . ?
C22 F12A 1.329(15) . ?
C23 C24 1.49(3) . ?
C23 F13A 1.366(15) . ?
C23 F14A 1.318(15) . ?
C23 F15A 1.304(14) . ?
C24 C25 1.40(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.36(3) . ?
C26 C27 1.53(3) . ?
C27 F16A 1.330(16) . ?
C27 F17A 1.325(15) . ?
C27 F18A 1.312(15) . ?
C2S H2S 0.9500 . ?
C2S C3S 1.3900 . ?
C2S C1S 1.3900 . ?
C3S H3S 0.9500 . ?
C3S C4S 1.3900 . ?
C4S H4S 0.9500 . ?
C4S C5S 1.3900 . ?
C5S H5S 0.9500 . ?
C5S C6S 1.3900 . ?
C6S H6S 0.9500 . ?
C6S C1S 1.3900 . ?
C1S C7S 1.30(7) . ?
C7S H7SA 0.9800 . ?
C7S H7SB 0.9800 . ?
C7S H7SC 0.9800 . ?
C3T H3T 0.9500 . ?
C3T C2T 1.3900 . ?
C3T C4T 1.3900 . ?
C2T H2T 0.9500 . ?
C2T C1T 1.3900 . ?
C1T C6T 1.3900 . ?
C1T C7T 1.49(7) . ?
C6T H6T 0.9500 . ?
C6T C5T 1.3900 . ?
C5T H5T 0.9500 . ?
C5T C4T 1.3900 . ?
C4T H4T 0.9500 . ?
C7T H7TA 0.9800 . ?
C7T H7TB 0.9800 . ?
C7T H7TC 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
O3 Gd1 O1 62.7(5) . 2_645 ?
O3 Gd1 O4 72.4(4) . . ?
O3 Gd1 O6 85.1(5) . . ?
O3 Gd1 O7 141.0(5) . . ?
O3 Gd1 O8 136.9(5) . . ?
O3 Gd1 N1 74.7(4) . . ?
O3 Gd1 N2 69.3(5) . . ?
O4 Gd1 O1 66.3(4) . 2_645 ?
O4 Gd1 O6 132.1(4) . . ?
O4 Gd1 O8 149.3(4) . . ?
O4 Gd1 N1 73.0(4) . . ?
O4 Gd1 N2 127.2(5) . . ?
O5 Gd1 O1 64.7(5) . 2_645 ?
O5 Gd1 O3 127.4(5) . . ?
O5 Gd1 O4 87.0(5) . . ?
O5 Gd1 O6 73.9(5) . . ?
O5 Gd1 O7 74.4(5) . . ?
O5 Gd1 O8 79.8(5) . . ?
O5 Gd1 N1 144.4(5) . . ?
O5 Gd1 N2 145.6(5) . . ?
O6 Gd1 O1 65.8(4) . 2_645 ?
O6 Gd1 O8 70.3(4) . . ?
O6 Gd1 N1 140.9(4) . . ?
O6 Gd1 N2 78.8(5) . . ?
O7 Gd1 O1 125.8(4) . 2_645 ?
O7 Gd1 O4 77.9(4) . . ?
O7 Gd1 O6 133.9(5) . . ?
O7 Gd1 O8 71.9(4) . . ?
O7 Gd1 N1 72.9(4) . . ?
O7 Gd1 N2 112.7(5) . . ?
O8 Gd1 O1 129.2(5) . 2_645 ?
O8 Gd1 N1 102.6(5) . . ?
O8 Gd1 N2 71.5(5) . . ?
N1 Gd1 O1 127.5(4) . 2_645 ?
N2 Gd1 O1 121.3(5) . 2_645 ?
N2 Gd1 N1 62.9(5) . . ?
C5 O1 Gd1 172.5(15) . 2_655 ?
C14 O3 Gd1 135.2(12) . . ?
C16 O4 Gd1 133.7(11) . . ?
C19 O5 Gd1 133.8(13) . . ?
C21 O6 Gd1 132.8(12) . . ?
C24 O7 Gd1 135.3(13) . . ?
C26 O8 Gd1 132.2(14) . . ?
C1 N1 Gd1 122.5(14) . . ?
C12 N1 Gd1 120.9(13) . . ?
C12 N1 C1 114.6(18) . . ?
C10 N2 Gd1 123.8(15) . . ?
C10 N2 C11 115.5(18) . . ?
C11 N2 Gd1 119.5(12) . . ?
N1 C1 H1 117.6 . . ?
N1 C1 C2 125(2) . . ?
C2 C1 H1 117.6 . . ?
C1 C2 H2 121.3 . . ?
C3 C2 C1 117(2) . . ?
C3 C2 H2 121.3 . . ?
C2 C3 H3 119.4 . . ?
C2 C3 C4 121(2) . . ?
C4 C3 H3 119.4 . . ?
C3 C4 C5 124(2) . . ?
C3 C4 C12 116.2(19) . . ?
C12 C4 C5 119.3(17) . . ?
O1 C5 C4 121(2) . . ?
O1 C5 C6 120.1(18) . . ?
C4 C5 C6 118.9(19) . . ?
O2 C6 C5 116(2) . . ?
O2 C6 C7 125(2) . . ?
C7 C6 C5 118.4(18) . . ?
C8 C7 C6 116(2) . . ?
C8 C7 C11 122(2) . . ?
C11 C7 C6 122(2) . . ?
C7 C8 H8 122.1 . . ?
C7 C8 C9 116(2) . . ?
C9 C8 H8 122.1 . . ?
C8 C9 H9 121.9 . . ?
C10 C9 C8 116(2) . . ?
C10 C9 H9 121.9 . . ?
N2 C10 C9 127(2) . . ?
N2 C10 H10 116.3 . . ?
C9 C10 H10 116.3 . . ?
N2 C11 C7 123(2) . . ?
N2 C11 C12 118.2(17) . . ?
C7 C11 C12 119(2) . . ?
N1 C12 C4 125.3(18) . . ?
N1 C12 C11 112.8(19) . . ?
C4 C12 C11 121.8(17) . . ?
F1 C13 F2 105(2) . . ?
F1 C13 C14 111.8(19) . . ?
F2 C13 C14 113(2) . . ?
F3 C13 F1 108(2) . . ?
F3 C13 F2 106.0(17) . . ?
F3 C13 C14 113(2) . . ?
O3 C14 C13 111.9(19) . . ?
O3 C14 C15 129.0(18) . . ?
C15 C14 C13 119(2) . . ?
C14 C15 H15 119.5 . . ?
C14 C15 C16 121.0(19) . . ?
C16 C15 H15 119.5 . . ?
O4 C16 C15 128.4(17) . . ?
O4 C16 C17 113.2(18) . . ?
C15 C16 C17 118.2(19) . . ?
F4 C17 C16 112.5(19) . . ?
F5 C17 F4 106(2) . . ?
F5 C17 F6 107(2) . . ?
F5 C17 C16 115(2) . . ?
F6 C17 F4 104(2) . . ?
F6 C17 C16 111(2) . . ?
F7 C18 F8 109(2) . . ?
F7 C18 F9 105(2) . . ?
F7 C18 C19 110(3) . . ?
F8 C18 F9 107(3) . . ?
F8 C18 C19 113(2) . . ?
F9 C18 C19 112(2) . . ?
O5 C19 C18 113(2) . . ?
O5 C19 C20 128(2) . . ?
C20 C19 C18 119(2) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 C19 122(2) . . ?
C21 C20 H20 119.2 . . ?
O6 C21 C20 126(2) . . ?
O6 C21 C22 114.9(19) . . ?
C20 C21 C22 119(2) . . ?
F10 C22 F11 108(2) . . ?
F10 C22 F12 104(2) . . ?
F10 C22 C21 112.3(19) . . ?
F11 C22 F12 106(2) . . ?
F11 C22 C21 111.2(17) . . ?
F12 C22 C21 114.6(18) . . ?
F10A C22 C21 108(2) . . ?
F10A C22 F12A 103(3) . . ?
F11A C22 C21 112(2) . . ?
F11A C22 F10A 108(3) . . ?
F11A C22 F12A 112(3) . . ?
F12A C22 C21 113.8(19) . . ?
F13 C23 F14 109.8(15) . . ?
F13 C23 F15 103.4(14) . . ?
F13 C23 C24 114.4(17) . . ?
F14 C23 F15 105.7(14) . . ?
F14 C23 C24 118.3(18) . . ?
F15 C23 C24 103(2) . . ?
F13A C23 C24 101(2) . . ?
F14A C23 C24 118(2) . . ?
F14A C23 F13A 103.5(15) . . ?
F15A C23 C24 120.4(19) . . ?
F15A C23 F13A 103.0(15) . . ?
F15A C23 F14A 108.7(16) . . ?
O7 C24 C23 116.1(18) . . ?
O7 C24 C25 128(2) . . ?
C25 C24 C23 116(2) . . ?
C24 C25 H25 120.6 . . ?
C26 C25 C24 119(3) . . ?
C26 C25 H25 120.6 . . ?
O8 C26 C25 133(3) . . ?
O8 C26 C27 111.8(17) . . ?
C25 C26 C27 116(2) . . ?
F16 C27 C26 112.7(19) . . ?
F17 C27 F16 105.2(15) . . ?
F17 C27 F18 107.9(16) . . ?
F17 C27 C26 116.6(18) . . ?
F18 C27 F16 107.1(15) . . ?
F18 C27 C26 107(2) . . ?
F16A C27 C26 105(3) . . ?
F17A C27 C26 114(2) . . ?
F17A C27 F16A 106.0(17) . . ?
F18A C27 C26 117.5(19) . . ?
F18A C27 F16A 106.0(18) . . ?
F18A C27 F17A 107.1(17) . . ?
C3S C2S H2S 120.0 . . ?
C3S C2S C1S 120.0 . . ?
C1S C2S H2S 120.0 . . ?
C2S C3S H3S 120.0 . . ?
C4S C3S C2S 120.0 . . ?
C4S C3S H3S 120.0 . . ?
C3S C4S H4S 120.0 . . ?
C3S C4S C5S 120.0 . . ?
C5S C4S H4S 120.0 . . ?
C4S C5S H5S 120.0 . . ?
C6S C5S C4S 120.0 . . ?
C6S C5S H5S 120.0 . . ?
C5S C6S H6S 120.0 . . ?
C5S C6S C1S 120.0 . . ?
C1S C6S H6S 120.0 . . ?
C6S C1S C2S 120.0 . . ?
C7S C1S C2S 125(7) . . ?
C7S C1S C6S 115(7) . . ?
C1S C7S H7SA 109.5 . . ?
C1S C7S H7SB 109.5 . . ?
C1S C7S H7SC 109.5 . . ?
H7SA C7S H7SB 109.5 . . ?
H7SA C7S H7SC 109.5 . . ?
H7SB C7S H7SC 109.5 . . ?
C2T C3T H3T 120.0 . . ?
C2T C3T C4T 120.0 . . ?
C4T C3T H3T 120.0 . . ?
C3T C2T H2T 120.0 . . ?
C3T C2T C1T 120.0 . . ?
C1T C2T H2T 120.0 . . ?
C2T C1T C7T 120(6) . . ?
C6T C1T C2T 120.0 . . ?
C6T C1T C7T 118(6) . . ?
C1T C6T H6T 120.0 . . ?
C5T C6T C1T 120.0 . . ?
C5T C6T H6T 120.0 . . ?
C6T C5T H5T 120.0 . . ?
C4T C5T C6T 120.0 . . ?
C4T C5T H5T 120.0 . . ?
C3T C4T H4T 120.0 . . ?
C5T C4T C3T 120.0 . . ?
C5T C4T H4T 120.0 . . ?
C1T C7T H7TA 109.5 . . ?
C1T C7T H7TB 109.5 . . ?
C1T C7T H7TC 109.5 . . ?
H7TA C7T H7TB 109.5 . . ?
H7TA C7T H7TC 109.5 . . ?
H7TB C7T H7TC 109.5 . . ?
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
Gd1 O3 C14 C13 -172.0(14) . . . . ?
Gd1 O3 C14 C15 3(4) . . . . ?
Gd1 O4 C16 C15 -2(3) . . . . ?
Gd1 O4 C16 C17 173.5(13) . . . . ?
Gd1 O5 C19 C18 -175.4(16) . . . . ?
Gd1 O5 C19 C20 12(4) . . . . ?
Gd1 O6 C21 C20 -16(3) . . . . ?
Gd1 O6 C21 C22 166.8(11) . . . . ?
Gd1 O7 C24 C23 171.0(13) . . . . ?
Gd1 O7 C24 C25 -10(4) . . . . ?
Gd1 O8 C26 C25 8(4) . . . . ?
Gd1 O8 C26 C27 -173.9(12) . . . . ?
Gd1 N1 C1 C2 163.4(17) . . . . ?
Gd1 N1 C12 C4 -158.8(15) . . . . ?
Gd1 N1 C12 C11 18(2) . . . . ?
Gd1 N2 C10 C9 -168.0(16) . . . . ?
Gd1 N2 C11 C7 164.6(14) . . . . ?
Gd1 N2 C11 C12 -20(2) . . . . ?
F1 C13 C14 O3 63(3) . . . . ?
F1 C13 C14 C15 -113(3) . . . . ?
F2 C13 C14 O3 -55(3) . . . . ?
F2 C13 C14 C15 129(2) . . . . ?
F3 C13 C14 O3 -174.9(19) . . . . ?
F3 C13 C14 C15 9(3) . . . . ?
F7 C18 C19 O5 54(3) . . . . ?
F7 C18 C19 C20 -133(2) . . . . ?
F8 C18 C19 O5 -69(3) . . . . ?
F8 C18 C19 C20 104(2) . . . . ?
F9 C18 C19 O5 170(2) . . . . ?
F9 C18 C19 C20 -17(4) . . . . ?
F13 C23 C24 O7 19(3) . . . . ?
F13 C23 C24 C25 -160(2) . . . . ?
F14 C23 C24 O7 150.6(19) . . . . ?
F14 C23 C24 C25 -29(3) . . . . ?
F15 C23 C24 O7 -93(2) . . . . ?
F15 C23 C24 C25 88(2) . . . . ?
O1 C5 C6 O2 -18(3) . . . . ?
O1 C5 C6 C7 167(2) . . . . ?
O2 C6 C7 C8 5(3) . . . . ?
O2 C6 C7 C11 -171.7(19) . . . . ?
O3 C14 C15 C16 3(4) . . . . ?
O4 C16 C17 F4 64(3) . . . . ?
O4 C16 C17 F5 -174.6(19) . . . . ?
O4 C16 C17 F6 -53(2) . . . . ?
O5 C19 C20 C21 3(4) . . . . ?
O6 C21 C22 F10 115(2) . . . . ?
O6 C21 C22 F11 -124(2) . . . . ?
O6 C21 C22 F12 -4(3) . . . . ?
O6 C21 C22 F10A 77(3) . . . . ?
O6 C21 C22 F11A -42(3) . . . . ?
O6 C21 C22 F12A -170(2) . . . . ?
O7 C24 C25 C26 -1(4) . . . . ?
O8 C26 C27 F16 -54(3) . . . . ?
O8 C26 C27 F17 -176.0(19) . . . . ?
O8 C26 C27 F18 63(2) . . . . ?
O8 C26 C27 F16A -101(3) . . . . ?
O8 C26 C27 F17A 143(3) . . . . ?
O8 C26 C27 F18A 17(3) . . . . ?
N1 C1 C2 C3 -4(3) . . . . ?
N2 C11 C12 N1 1(2) . . . . ?
N2 C11 C12 C4 177.9(18) . . . . ?
C1 N1 C12 C4 6(3) . . . . ?
C1 N1 C12 C11 -177.5(16) . . . . ?
C1 C2 C3 C4 4(3) . . . . ?
C2 C3 C4 C5 179.5(19) . . . . ?
C2 C3 C4 C12 0(3) . . . . ?
C3 C4 C5 O1 13(3) . . . . ?
C3 C4 C5 C6 -169.9(19) . . . . ?
C3 C4 C12 N1 -6(3) . . . . ?
C3 C4 C12 C11 177.9(18) . . . . ?
C4 C5 C6 O2 164.8(18) . . . . ?
C4 C5 C6 C7 -10(3) . . . . ?
C5 C4 C12 N1 175.3(17) . . . . ?
C5 C4 C12 C11 -1(3) . . . . ?
C5 C6 C7 C8 178.9(18) . . . . ?
C5 C6 C7 C11 3(3) . . . . ?
C6 C7 C8 C9 -178.1(19) . . . . ?
C6 C7 C11 N2 -179.0(19) . . . . ?
C6 C7 C11 C12 5(3) . . . . ?
C7 C8 C9 C10 -2(3) . . . . ?
C7 C11 C12 N1 176.8(17) . . . . ?
C7 C11 C12 C4 -6(3) . . . . ?
C8 C7 C11 N2 5(3) . . . . ?
C8 C7 C11 C12 -170.8(19) . . . . ?
C8 C9 C10 N2 3(3) . . . . ?
C10 N2 C11 C7 -4(3) . . . . ?
C10 N2 C11 C12 172.0(16) . . . . ?
C11 N2 C10 C9 0(3) . . . . ?
C11 C7 C8 C9 -2(3) . . . . ?
C12 N1 C1 C2 -1(3) . . . . ?
C12 C4 C5 O1 -168(2) . . . . ?
C12 C4 C5 C6 9(3) . . . . ?
C13 C14 C15 C16 177(2) . . . . ?
C14 C15 C16 O4 -3(4) . . . . ?
C14 C15 C16 C17 -178(2) . . . . ?
C15 C16 C17 F4 -120(2) . . . . ?
C15 C16 C17 F5 2(3) . . . . ?
C15 C16 C17 F6 124(2) . . . . ?
C18 C19 C20 C21 -169(2) . . . . ?
C19 C20 C21 O6 -1(4) . . . . ?
C19 C20 C21 C22 176(2) . . . . ?
C20 C21 C22 F10 -63(3) . . . . ?
C20 C21 C22 F11 58(3) . . . . ?
C20 C21 C22 F12 179(2) . . . . ?
C20 C21 C22 F10A -101(3) . . . . ?
C20 C21 C22 F11A 141(3) . . . . ?
C20 C21 C22 F12A 13(3) . . . . ?
C23 C24 C25 C26 178(2) . . . . ?
C24 C25 C26 O8 2(5) . . . . ?
C24 C25 C26 C27 -176(2) . . . . ?
C25 C26 C27 F16 124(2) . . . . ?
C25 C26 C27 F17 2(3) . . . . ?
C25 C26 C27 F18 -119(2) . . . . ?
C25 C26 C27 F16A 77(3) . . . . ?
C25 C26 C27 F17A -39(3) . . . . ?
C25 C26 C27 F18A -165(2) . . . . ?
F13A C23 C24 O7 85(2) . . . . ?
F13A C23 C24 C25 -94(3) . . . . ?
F14A C23 C24 O7 -163(2) . . . . ?
F14A C23 C24 C25 17(3) . . . . ?
F15A C23 C24 O7 -27(3) . . . . ?
F15A C23 C24 C25 154(2) . . . . ?
C2S C3S C4S C5S 0.0 . . . . ?
C3S C2S C1S C6S 0.0 . . . . ?
C3S C2S C1S C7S 175(6) . . . . ?
C3S C4S C5S C6S 0.0 . . . . ?
C4S C5S C6S C1S 0.0 . . . . ?
C5S C6S C1S C2S 0.0 . . . . ?
C5S C6S C1S C7S -176(5) . . . . ?
C1S C2S C3S C4S 0.0 . . . . ?
C3T C2T C1T C6T 0.0 . . . . ?
C3T C2T C1T C7T -166(5) . . . . ?
C2T C3T C4T C5T 0.0 . . . . ?
C2T C1T C6T C5T 0.0 . . . . ?
C1T C6T C5T C4T 0.0 . . . . ?
C6T C5T C4T C3T 0.0 . . . . ?
C4T C3T C2T C1T 0.0 . . . . ?
C7T C1T C6T C5T 167(5) . . . . ?
_shelx_res_file
;
TITL 2017ncs0758_a.res in P2(1)/c
2017ncs0758.res
created by SHELXL-2018/1 at 12:14:14 on 23-Mar-2018
REM Old TITL 2017ncs0758 in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.289, Rweak 0.175, Alpha 0.182, Orientation as input
REM Formula found by SHELXT: C37 N1 O8 F14 Gd
CELL 1.54178 12.9683 16.5764 18.0184 90 103.338 90
ZERR 4 0.0018 0.003 0.0024 0 0.015 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H F Gd N O
UNIT 136 68 72 4 8 32
SADI F17A C27 F17 C27 F16A C27 F16 C27 F18A C27 F18 C27
SADI F12A C22 F11A C22 F12 C22 F10 C22 F11 C22 F10A C22 C23 F13 C23 F15 C23 =
F14 F17 C27 F18 C27 F16 C27 F13 C23 F14 C23 F15 C23 C23 F14A C23 F13A C23 F15A
SADI F18 F16 F17 F16 F18 F17 F18A F16A F18A F17A F16A F17A F13 F15 F13 F14 =
F15 F14 F14A F13A F14A F15A F13A F15A
L.S. 10
PLAN 50
SIZE 0.03 0.05 0.05
TEMP -173(2)
conf
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.198000
FVAR 0.22057 0.60626 0.65198 0.64765
GD1 4 0.323306 0.229896 0.263179 11.00000 0.07121 0.08705 =
0.06192 -0.00335 0.02231 -0.00856
F1 3 0.637361 0.358245 0.201861 11.00000 0.10596 0.15659 =
0.11473 0.03809 0.03160 -0.00094
F2 3 0.677726 0.232961 0.197525 11.00000 0.10474 0.14589 =
0.10581 -0.01837 0.05639 -0.00349
F3 3 0.760402 0.306797 0.291529 11.00000 0.07606 0.12748 =
0.09963 -0.00235 0.02097 -0.00045
F4 3 0.555940 0.213649 0.534524 11.00000 0.19627 0.09262 =
0.08105 -0.01522 0.01074 -0.01663
F5 3 0.658594 0.306316 0.520328 11.00000 0.12527 0.20953 =
0.07929 -0.00096 0.01662 -0.05580
F6 3 0.500275 0.332323 0.518028 11.00000 0.16063 0.14463 =
0.11154 -0.04639 0.03515 0.02734
F7 3 0.123694 0.032768 0.371140 11.00000 0.13262 0.14589 =
0.14709 -0.03312 0.08280 -0.03439
F8 3 0.266314 -0.036998 0.388038 11.00000 0.14107 0.12909 =
0.08729 0.00440 0.03782 -0.01660
F9 3 0.129142 -0.068912 0.301121 11.00000 0.14145 0.14051 =
0.11285 -0.00764 0.04975 -0.03495
PART 1
F10 3 0.317412 -0.045368 0.085736 21.00000 0.11583
F11 3 0.167474 0.010093 0.040231 21.00000 0.10026
F12 3 0.310985 0.068315 0.034710 21.00000 0.09079
F13 3 0.127419 0.340467 0.443454 41.00000 0.09664
F14 3 -0.033834 0.330537 0.380995 41.00000 0.10284
F15 3 0.053366 0.227446 0.430392 41.00000 0.15518
F16 3 -0.025326 0.254548 0.066840 31.00000 0.13448
F17 3 -0.129467 0.219471 0.134369 31.00000 0.08174
F18 3 -0.020075 0.134136 0.108180 31.00000 0.16565
PART 0
O1 6 0.523892 0.605507 0.193582 11.00000 0.13209 0.05519 =
0.11753 0.01811 0.03294 0.00352
O2 6 0.442718 0.553913 0.048366 11.00000 0.12955 0.11291 =
0.10493 0.01996 0.04643 -0.00322
O3 6 0.495125 0.254940 0.246786 11.00000 0.06556 0.10413 =
0.08166 -0.01631 0.02061 0.01058
O4 6 0.435794 0.248413 0.385785 11.00000 0.01800 0.09821 =
0.07381 -0.01111 -0.00177 -0.00604
O5 6 0.262586 0.114226 0.311283 11.00000 0.07831 0.10419 =
0.07821 0.00771 0.01488 -0.00047
O6 6 0.316596 0.128639 0.169115 11.00000 0.06775 0.09454 =
0.07239 -0.00412 0.01567 0.00326
O7 6 0.203627 0.274453 0.334627 11.00000 0.08075 0.10287 =
0.05505 -0.01425 0.01895 -0.00846
O8 6 0.145940 0.222386 0.182693 11.00000 0.09650 0.11110 =
0.04091 -0.00471 0.00567 -0.00431
N1 5 0.351443 0.383197 0.282924 11.00000 0.06623 0.05994 =
0.07151 0.00446 0.02955 -0.01799
N2 5 0.316775 0.314637 0.145501 11.00000 0.07297 0.07075 =
0.08159 -0.00424 0.02416 -0.02449
C1 1 0.363963 0.418409 0.351728 11.00000 0.07979 0.08920 =
0.11339 -0.00772 0.04486 -0.00377
AFIX 43
H1 2 0.343552 0.388401 0.390923 11.00000 -1.20000
AFIX 0
C2 1 0.404081 0.494556 0.369534 11.00000 0.07997 0.11047 =
0.08116 -0.00606 0.01166 0.03300
AFIX 43
H2 2 0.407161 0.517722 0.418222 11.00000 -1.20000
AFIX 0
C3 1 0.439152 0.535376 0.314761 11.00000 0.10549 0.07193 =
0.08464 -0.00365 0.01863 0.01107
AFIX 43
H3 2 0.471343 0.586739 0.326339 11.00000 -1.20000
AFIX 0
C4 1 0.429028 0.504062 0.243613 11.00000 0.05854 0.05983 =
0.06748 -0.00455 0.00055 0.00199
C5 1 0.464324 0.544901 0.180893 11.00000 0.07599 0.04866 =
0.10955 0.02025 0.03182 -0.00104
C6 1 0.431736 0.509639 0.100403 11.00000 0.05505 0.12593 =
0.07932 0.02614 0.02555 0.00492
C7 1 0.382260 0.430237 0.090803 11.00000 0.06136 0.08587 =
0.11542 0.02420 0.01211 -0.01017
C8 1 0.353038 0.402138 0.017400 11.00000 0.07501 0.10548 =
0.05874 -0.00926 0.00717 0.00902
AFIX 43
H8 2 0.366154 0.431806 -0.024586 11.00000 -1.20000
AFIX 0
C9 1 0.301213 0.324811 0.008012 11.00000 0.12996 0.10988 =
0.07509 0.00185 0.04912 0.01225
AFIX 43
H9 2 0.276320 0.300988 -0.040792 11.00000 -1.20000
AFIX 0
C10 1 0.289513 0.286444 0.075423 11.00000 0.05681 0.10675 =
0.06917 -0.00674 0.00162 -0.00221
AFIX 43
H10 2 0.258384 0.234267 0.069587 11.00000 -1.20000
AFIX 0
C11 1 0.360310 0.387492 0.152704 11.00000 0.05243 0.11914 =
0.07080 0.02159 0.01999 0.03196
C12 1 0.380263 0.428403 0.230558 11.00000 0.07243 0.08367 =
0.07086 0.00949 0.01911 -0.00584
C13 1 0.664510 0.293339 0.246337 11.00000 0.06458 0.10492 =
0.08603 -0.00508 0.00812 0.01563
C14 1 0.582604 0.273391 0.290205 11.00000 0.07482 0.08841 =
0.07393 0.00765 0.03110 0.00902
C15 1 0.607072 0.282118 0.365712 11.00000 0.03718 0.15760 =
0.09119 0.00736 0.01304 -0.01908
AFIX 43
H15 2 0.676576 0.298544 0.390752 11.00000 -1.20000
AFIX 0
C16 1 0.531534 0.267376 0.408918 11.00000 0.09235 0.04281 =
0.05755 -0.00605 0.00417 0.00081
C17 1 0.564224 0.280629 0.495213 11.00000 0.08115 0.04318 =
0.13929 0.00196 0.02741 -0.02196
C18 1 0.187256 -0.006422 0.336785 11.00000 0.10978 0.12722 =
0.08066 -0.02657 0.02849 -0.05577
C19 1 0.222108 0.048386 0.281289 11.00000 0.06959 0.13371 =
0.08505 0.00588 0.03857 -0.00624
C20 1 0.218135 0.019339 0.206573 11.00000 0.08858 0.10399 =
0.08821 0.01123 0.02199 -0.01625
AFIX 43
H20 2 0.181906 -0.029675 0.190417 11.00000 -1.20000
AFIX 0
C21 1 0.266418 0.061263 0.156008 11.00000 0.06340 0.06435 =
0.10803 -0.01698 0.00558 -0.00327
C22 1 0.265520 0.023901 0.079347 11.00000 0.08809 0.08310 =
0.10692 -0.01292 0.03011 -0.00999
C23 1 0.060548 0.297895 0.393216 11.00000 0.12941 0.10543 =
0.12438 -0.01347 0.06036 -0.02109
C24 1 0.101304 0.272344 0.326090 11.00000 0.08547 0.14501 =
0.06694 0.00333 0.01461 -0.01142
C25 1 0.024791 0.249815 0.260896 11.00000 0.11334 0.14174 =
0.09291 0.00348 0.03691 0.01508
AFIX 43
H25 2 -0.048314 0.249508 0.261354 11.00000 -1.20000
AFIX 0
C26 1 0.057186 0.228353 0.196825 11.00000 0.09454 0.13152 =
0.08371 0.00127 0.04681 0.00016
C27 1 -0.031604 0.210044 0.126648 11.00000 0.12573
PART 2
F10A 3 0.359472 -0.009510 0.083319 -21.00000 0.11756
F11A 3 0.249597 0.078420 0.024662 -21.00000 0.11216
F12A 3 0.199718 -0.038281 0.061829 -21.00000 0.07663
F13A 3 0.055421 0.379560 0.382687 -41.00000 0.12147
F14A 3 -0.037578 0.277983 0.394070 -41.00000 0.09976
F15A 3 0.119429 0.290507 0.462099 -41.00000 0.06666
F16A 3 -0.068824 0.281613 0.099635 -31.00000 0.28503
F17A 3 -0.113073 0.170784 0.142302 -31.00000 0.10544
F18A 3 -0.005682 0.172309 0.069593 -31.00000 0.07788
PART 0
PART 1
AFIX 66
C2S 1 0.179913 0.599613 0.158776 10.50000 0.12275
AFIX 43
H2S 2 0.205521 0.652464 0.172732 10.50000 -1.20000
AFIX 65
C3S 1 0.157754 0.547670 0.213634 10.50000 0.15255
AFIX 43
H3S 2 0.168217 0.565020 0.265084 10.50000 -1.20000
AFIX 65
C4S 1 0.120286 0.470341 0.193215 10.50000 0.15881
AFIX 43
H4S 2 0.105141 0.434841 0.230708 10.50000 -1.20000
AFIX 65
C5S 1 0.104976 0.444955 0.117936 10.50000 0.12718
AFIX 43
H5S 2 0.079368 0.392104 0.103980 10.50000 -1.20000
AFIX 65
C6S 1 0.127135 0.496897 0.063076 10.50000 0.09897
AFIX 43
H6S 2 0.116671 0.479547 0.011626 10.50000 -1.20000
AFIX 65
C1S 1 0.164603 0.574227 0.083495 10.50000 0.10184
AFIX 0
C7S 1 0.176018 0.619758 0.027375 10.50000 0.17023
AFIX 33
H7SA 2 0.202593 0.672770 0.047064 10.50000 -1.50000
H7SB 2 0.226627 0.594736 0.001541 10.50000 -1.50000
H7SC 2 0.107459 0.626162 -0.008871 10.50000 -1.50000
AFIX 66
PART 0
PART 2
C3T 1 0.173744 0.603383 0.123414 10.50000 0.12595
AFIX 43
H3T 2 0.194839 0.655081 0.109609 10.50000 -1.20000
AFIX 65
C2T 1 0.169714 0.587821 0.198495 10.50000 0.12713
AFIX 43
H2T 2 0.188055 0.628883 0.236005 10.50000 -1.20000
AFIX 65
C1T 1 0.138849 0.512179 0.218693 10.50000 0.08460
C6T 1 0.112013 0.452099 0.163811 10.50000 0.08341
AFIX 43
H6T 2 0.090918 0.400401 0.177616 10.50000 -1.20000
AFIX 65
C5T 1 0.116043 0.467660 0.088729 10.50000 0.10112
AFIX 43
H5T 2 0.097702 0.426598 0.051220 10.50000 -1.20000
AFIX 65
C4T 1 0.146908 0.543302 0.068530 10.50000 0.15576
AFIX 43
H4T 2 0.149662 0.553937 0.017215 10.50000 -1.20000
AFIX 0
C7T 1 0.111075 0.500214 0.293522 10.50000 0.18289
AFIX 33
H7TA 2 0.134608 0.547031 0.326265 10.50000 -1.50000
H7TB 2 0.034128 0.494196 0.285618 10.50000 -1.50000
H7TC 2 0.146183 0.451531 0.317999 10.50000 -1.50000
AFIX 0
HKLF 4
REM 2017ncs0758_a.res in P2(1)/c
REM R1 = 0.1180 for 2780 Fo > 4sig(Fo) and 0.2532 for all 6759 data
REM 526 parameters refined using 219 restraints
END
WGHT 0.1769 0.0000
REM Highest difference peak 1.311, deepest hole -0.776, 1-sigma level 0.145
Q1 1 0.2997 0.2317 0.2075 11.00000 0.05 1.31
Q2 1 0.3449 0.2300 0.3144 11.00000 0.05 1.20
Q3 1 0.3798 0.2296 0.2522 11.00000 0.05 1.08
Q4 1 0.3453 0.3182 0.3032 11.00000 0.05 0.94
Q5 1 0.2630 0.2207 0.2731 11.00000 0.05 0.90
Q6 1 -0.0245 0.3192 0.0803 11.00000 0.05 0.87
Q7 1 0.1251 0.4079 0.4041 11.00000 0.05 0.84
Q8 1 0.2965 0.3113 0.2152 11.00000 0.05 0.69
Q9 1 0.3259 0.1429 0.2210 11.00000 0.05 0.69
Q10 1 0.0959 0.2132 0.4528 11.00000 0.05 0.65
Q11 1 0.3937 0.3073 0.3829 11.00000 0.05 0.63
Q12 1 -0.0210 0.2188 0.0656 11.00000 0.05 0.60
Q13 1 -0.0304 0.0968 0.1415 11.00000 0.05 0.58
Q14 1 0.5728 0.6611 0.1454 11.00000 0.05 0.57
Q15 1 0.3294 0.1349 0.3039 11.00000 0.05 0.53
Q16 1 0.2015 0.2830 0.0651 11.00000 0.05 0.52
Q17 1 0.5001 0.2620 0.2962 11.00000 0.05 0.51
Q18 1 0.3022 0.0801 0.2727 11.00000 0.05 0.50
Q19 1 0.2664 0.1176 0.1520 11.00000 0.05 0.49
Q20 1 0.0191 0.0878 0.1174 11.00000 0.05 0.48
Q21 1 0.6620 0.2180 0.5294 11.00000 0.05 0.46
Q22 1 0.3533 0.0989 0.1822 11.00000 0.05 0.46
Q23 1 0.2063 0.1472 0.3130 11.00000 0.05 0.45
Q24 1 0.4426 0.1563 0.2070 11.00000 0.05 0.45
Q25 1 0.6398 0.2214 0.5031 11.00000 0.05 0.44
Q26 1 0.1765 0.2036 0.2335 11.00000 0.05 0.44
Q27 1 0.4416 0.3023 0.2118 11.00000 0.05 0.44
Q28 1 0.1047 0.3118 0.4528 11.00000 0.05 0.44
Q29 1 0.3948 0.2240 0.3953 11.00000 0.05 0.43
Q30 1 0.2646 0.3378 0.1547 11.00000 0.05 0.43
Q31 1 0.3567 -0.0677 0.1265 11.00000 0.05 0.43
Q32 1 0.7362 0.2933 0.2334 11.00000 0.05 0.43
Q33 1 0.3228 0.4327 0.0475 11.00000 0.05 0.42
Q34 1 0.1857 0.2424 0.3256 11.00000 0.05 0.42
Q35 1 -0.0208 0.3830 0.3545 11.00000 0.05 0.41
Q36 1 0.4420 0.5404 0.3683 11.00000 0.05 0.40
Q37 1 0.2845 0.1033 0.3405 11.00000 0.05 0.39
Q38 1 0.0023 0.3167 0.2348 11.00000 0.05 0.38
Q39 1 0.1716 0.2942 0.3207 11.00000 0.05 0.38
Q40 1 0.4013 0.4112 0.3049 11.00000 0.05 0.38
Q41 1 0.3286 0.5655 0.3322 11.00000 0.05 0.38
Q42 1 0.2602 0.4786 0.3300 11.00000 0.05 0.38
Q43 1 0.2336 -0.0562 0.1027 11.00000 0.05 0.37
Q44 1 0.2178 0.3380 0.3685 11.00000 0.05 0.37
Q45 1 0.5606 0.6032 0.2530 11.00000 0.05 0.37
Q46 1 0.5135 0.6002 0.1306 11.00000 0.05 0.37
Q47 1 0.5470 0.2043 0.4577 11.00000 0.05 0.37
Q48 1 0.3212 0.0180 0.0424 11.00000 0.05 0.37
Q49 1 0.0533 0.5744 0.3027 11.00000 0.05 0.37
Q50 1 0.2446 0.2766 0.3776 11.00000 0.05 0.37
;
_shelx_res_checksum 92856
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.373
_oxdiff_exptl_absorpt_empirical_full_min 0.295
#######################################################################
#
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 1832431'
_audit_update_record
;
2018-03-26 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;
# 2018ncs0102
# [Gd(hfac)3(n,N'-pd} Et2O
_audit_creation_date 2018-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2018/1
# start Validation Reply Form
_vrf_PLAT971_2018ncs0102
;
PROBLEM: Check Calcd Resid. Dens. 0.89A From Gd1 6.43 eA-3
RESPONSE: The largest residual peaks are all adjacent to the Gd atom. Several
possible twin laws were explored but made no improvement but may be
the cause. Data were corrected
for absorption through a face-indexed crystal description.
;
_vrf_PLAT973_2018ncs0102
;
PROBLEM: Check Calcd Positive Resid. Density on Gd1 3.01 eA-3
RESPONSE: ...
;
_vrf_PLAT213_2018ncs0102
;
PROBLEM: Atom F4 has ADP max/min Ratio ..... 4.7 prolat
RESPONSE: CF3 group with high displacement parameters but not an obvious
alternative position of disorder by rotation.
;
_vrf_PLAT972_2018ncs0102
;
PROBLEM: Check Calcd Resid. Dens. 0.87A From Gd1 -2.75 eA-3
RESPONSE: as above
;
# end Validation Reply Form
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C27 H9 F18 Gd N2 O8, C4 H10 O'
_chemical_formula_sum 'C31 H19 F18 Gd N2 O9'
_chemical_formula_weight 1062.73
_chemical_melting_point ?
_chemical_oxdiff_formula 'C27 H9 O8 F18 Gd1'
_chemical_oxdiff_usercomment SH01_015b
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 9.6200(3)
_cell_length_b 22.9967(6)
_cell_length_c 17.1078(4)
_cell_angle_alpha 90
_cell_angle_beta 98.929(2)
_cell_angle_gamma 90
_cell_volume 3738.87(18)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 18136
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 30.1290
_cell_measurement_theta_min 2.9010
_cell_oxdiff_angle_alpha 89.996(2)
_cell_oxdiff_angle_beta 98.906(3)
_cell_oxdiff_angle_gamma 89.972(2)
_cell_oxdiff_length_a 9.6215(3)
_cell_oxdiff_length_b 22.9900(6)
_cell_oxdiff_length_c 17.1092(5)
_cell_oxdiff_measurement_reflns_used 18136
_cell_oxdiff_volume 3738.87(19)
_shelx_estimated_absorpt_T_max 0.837
_shelx_estimated_absorpt_T_min 0.509
_exptl_absorpt_coefficient_mu 1.918
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.556
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'translucent light green'
_exptl_crystal_density_diffrn 1.888
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2068
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0479
0 1 0 0.0479
1 1 1 0.0506
0 0 -1 0.1129
-3 -1 5 0.1705
1 1 5 0.0504
-3 -2 -5 0.1342
_exptl_crystal_size_max 0.407
_exptl_crystal_size_mid 0.193
_exptl_crystal_size_min 0.096
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0000 -0.9998 -0.0002 0.0137 -0.0274 -0.0036
0.0000 0.9998 0.0002 -0.0137 0.0274 0.0036
1.0005 0.9993 0.9995 -0.0832 -0.0132 0.0465
-0.0006 -0.0005 -0.9998 0.0347 0.0150 0.0181
-2.9966 -0.9939 5.0001 -0.0559 -0.0260 -0.2768
1.0031 1.0015 4.9986 -0.2222 -0.0733 -0.0259
-3.0029 -1.9991 -4.9978 0.3053 0.0970 -0.0996
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0776
_diffrn_reflns_av_unetI/netI 0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 43077
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.484
_diffrn_reflns_theta_min 2.410
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100(2)
_diffrn_detector 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -28.00 94.00 1.00 1.60 -- 5.00 72.00 -30.00 122
2 \w 1.00 28.00 1.00 1.60 -- 5.00 38.00-180.00 27
3 \w -17.00 9.00 1.00 1.60 -- -9.90 -72.00 -60.00 26
4 \w -9.00 63.00 1.00 1.60 -- -9.90 38.00 30.00 72
5 \w -43.00 79.00 1.00 1.60 -- -9.90 72.00 -90.00 122
;
_diffrn_measurement_device 'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method 'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0347161000
_diffrn_orient_matrix_UB_12 -0.0137435000
_diffrn_orient_matrix_UB_13 -0.0347276000
_diffrn_orient_matrix_UB_21 -0.0255140000
_diffrn_orient_matrix_UB_22 0.0273845000
_diffrn_orient_matrix_UB_23 -0.0150406000
_diffrn_orient_matrix_UB_31 0.0609264000
_diffrn_orient_matrix_UB_32 0.0036175000
_diffrn_orient_matrix_UB_33 -0.0181297000
_diffrn_radiation_collimation 0.2
_diffrn_radiation_monochromator 'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'Rotating Anode'
_diffrn_source_current 55.0
_diffrn_source_power 2.475
_diffrn_source_target Mo
_diffrn_source_type 'Rigaku FRE+'
_diffrn_source_voltage 45.0
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7233
_reflns_number_total 8526
_reflns_odcompleteness_completeness 99.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 27.42
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 5.745
_refine_diff_density_min -2.717
_refine_diff_density_rms 0.330
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.130
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 529
_refine_ls_number_reflns 8526
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.1014
_refine_ls_R_factor_gt 0.0915
_refine_ls_restrained_S_all 1.130
_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^)+(0.1510P)^2^+43.2990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2707
_refine_ls_wR_factor_ref 0.2793
_refine_special_details
;
One Me group of the Et2O molecule is modelled over 2 partially occupied sites with
occupancies 0.66/0.33 and all atoms of the Et2O refined with isotropic adps.
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
C5E-C3E = C4E-C3E
1.51 with sigma of 0.02
O9-C2E \\sim O9-C3E
with sigma of 0.02
C4E-C3E \\sim C5E-C3E \\sim C2E-C1E
with sigma of 0.02
3. Others
Fixed Sof: H3EA(0.6666) H3EB(0.6666) H3EC(0.33333) H3ED(0.33333) C4E(0.6666)
H4EA(0.6666) H4EB(0.6666) H4EC(0.6666) C5E(0.33333) H5EA(0.33333)
H5EB(0.33333) H5EC(0.33333)
4.a Secondary CH2 refined with riding coordinates:
C2E(H2EA,H2EB), C3E(H3EA,H3EB), C3E(H3EC,H3ED)
4.b Me refined with riding coordinates:
C1E(H1EA,H1EB,H1EC), C4E(H4EA,H4EB,H4EC), C5E(H5EA,H5EB,H5EC)
4.c Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C15(H15), C20(H20), C25(H25)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.77484(4) 0.42544(2) 0.29286(2) 0.02726(19) Uani 1 1 d . . . . .
F1 F 0.984(2) 0.2961(5) 0.1158(7) 0.154(7) Uani 1 1 d . . . . .
F2 F 0.9747(16) 0.2140(4) 0.1722(8) 0.123(5) Uani 1 1 d . . . . .
F3 F 1.1311(15) 0.2749(6) 0.2119(11) 0.142(6) Uani 1 1 d . . . . .
F4 F 0.724(2) 0.1878(4) 0.3852(11) 0.195(10) Uani 1 1 d . . . . .
F5 F 0.5512(17) 0.2424(7) 0.3754(9) 0.150(6) Uani 1 1 d . . . . .
F6 F 0.7161(14) 0.2581(5) 0.4658(6) 0.107(4) Uani 1 1 d . . . . .
F7 F 1.2104(8) 0.3639(4) 0.4562(4) 0.073(2) Uani 1 1 d . . . . .
F8 F 1.1415(8) 0.3569(4) 0.5668(4) 0.070(2) Uani 1 1 d . . . . .
F9 F 1.2030(10) 0.4390(4) 0.5287(8) 0.102(4) Uani 1 1 d . . . . .
F10 F 0.5158(8) 0.4008(5) 0.5061(4) 0.082(3) Uani 1 1 d . . . . .
F11 F 0.6789(8) 0.3864(4) 0.6030(4) 0.068(2) Uani 1 1 d . . . . .
F12 F 0.6180(11) 0.4737(4) 0.5687(5) 0.083(3) Uani 1 1 d . . . . .
F13 F 1.1015(10) 0.5340(4) 0.1433(5) 0.075(2) Uani 1 1 d . . . . .
F14 F 1.2006(9) 0.5417(5) 0.2627(6) 0.087(3) Uani 1 1 d . . . . .
F15 F 1.1008(13) 0.6163(4) 0.2025(10) 0.136(6) Uani 1 1 d . . . . .
F16 F 0.4925(8) 0.6037(4) 0.2209(4) 0.068(2) Uani 1 1 d . . . . .
F17 F 0.6529(10) 0.6688(3) 0.2456(7) 0.090(3) Uani 1 1 d . . . . .
F18 F 0.5794(8) 0.6233(3) 0.3393(4) 0.0540(17) Uani 1 1 d . . . . .
O1 O 0.3150(11) 0.4308(4) -0.0712(5) 0.058(2) Uani 1 1 d . . . . .
O2 O 0.1296(10) 0.4251(4) 0.0328(6) 0.065(3) Uani 1 1 d . . . . .
O3 O 0.9011(7) 0.3518(3) 0.2355(4) 0.0371(15) Uani 1 1 d . . . . .
O4 O 0.7165(7) 0.3336(3) 0.3427(4) 0.0374(15) Uani 1 1 d . . . . .
O5 O 0.9743(8) 0.4158(3) 0.3916(4) 0.0360(15) Uani 1 1 d . . . . .
O6 O 0.6984(7) 0.4402(3) 0.4152(4) 0.0328(13) Uani 1 1 d . . . . .
O7 O 0.9428(7) 0.4875(3) 0.2503(4) 0.0361(14) Uani 1 1 d . . . . .
O8 O 0.6793(7) 0.5196(3) 0.2820(4) 0.0355(14) Uani 1 1 d . . . . .
N1 N 0.6938(8) 0.4268(3) 0.1416(4) 0.0268(15) Uani 1 1 d . . . . .
N2 N 0.5105(9) 0.4146(4) 0.2467(5) 0.0345(17) Uani 1 1 d . . . . .
C1 C 0.7897(12) 0.4307(5) 0.0928(6) 0.040(2) Uani 1 1 d . . . . .
H1 H 0.886471 0.433969 0.114435 0.048 Uiso 1 1 calc R . . . .
C2 C 0.7504(14) 0.4300(5) 0.0108(6) 0.044(3) Uani 1 1 d . . . . .
H2 H 0.819800 0.431830 -0.023049 0.053 Uiso 1 1 calc R . . . .
C3 C 0.6109(14) 0.4267(4) -0.0204(6) 0.044(3) Uani 1 1 d . . . . .
H3 H 0.582276 0.427085 -0.076060 0.053 Uiso 1 1 calc R . . . .
C4 C 0.5103(13) 0.4227(4) 0.0308(6) 0.040(2) Uani 1 1 d . . . . .
C5 C 0.3597(16) 0.4211(7) -0.0006(8) 0.063(4) Uani 1 1 d . . . . .
C6 C 0.2554(15) 0.4191(6) 0.0588(8) 0.058(3) Uani 1 1 d . . . . .
C7 C 0.3129(12) 0.4146(5) 0.1435(7) 0.044(2) Uani 1 1 d . . . . .
C8 C 0.2235(11) 0.4094(6) 0.1983(8) 0.052(3) Uani 1 1 d . . . . .
H8 H 0.124642 0.407933 0.181718 0.062 Uiso 1 1 calc R . . . .
C9 C 0.2779(13) 0.4065(6) 0.2767(8) 0.053(3) Uani 1 1 d . . . . .
H9 H 0.217713 0.402534 0.315484 0.064 Uiso 1 1 calc R . . . .
C10 C 0.4199(11) 0.4092(5) 0.2984(6) 0.039(2) Uani 1 1 d . . . . .
H10 H 0.456796 0.407158 0.353103 0.047 Uiso 1 1 calc R . . . .
C11 C 0.4567(11) 0.4173(4) 0.1693(6) 0.0333(19) Uani 1 1 d . . . . .
C12 C 0.5564(11) 0.4221(4) 0.1126(6) 0.036(2) Uani 1 1 d . . . . .
C13 C 1.002(2) 0.2702(6) 0.1858(11) 0.084(6) Uani 1 1 d . . . . .
C14 C 0.9079(14) 0.2980(5) 0.2398(7) 0.050(3) Uani 1 1 d . . . . .
C15 C 0.8473(18) 0.2617(6) 0.2899(9) 0.070(4) Uani 1 1 d . . . . .
H15 H 0.868572 0.221371 0.291086 0.084 Uiso 1 1 calc R . . . .
C16 C 0.7558(14) 0.2834(5) 0.3383(7) 0.049(3) Uani 1 1 d . . . . .
C17 C 0.694(2) 0.2412(6) 0.3940(10) 0.078(5) Uani 1 1 d . . . . .
C18 C 1.1381(11) 0.3906(5) 0.5040(6) 0.045(2) Uani 1 1 d . . . . .
C19 C 0.9873(11) 0.4046(4) 0.4644(5) 0.036(2) Uani 1 1 d . . . . .
C20 C 0.8823(11) 0.4041(5) 0.5122(6) 0.040(2) Uani 1 1 d . . . . .
H20 H 0.904012 0.391041 0.565396 0.048 Uiso 1 1 calc R . . . .
C21 C 0.7455(11) 0.4227(4) 0.4832(6) 0.034(2) Uani 1 1 d . . . . .
C22 C 0.6387(13) 0.4208(6) 0.5411(6) 0.048(3) Uani 1 1 d . . . . .
C23 C 1.0883(16) 0.5592(6) 0.2119(9) 0.060(3) Uani 1 1 d . . . . .
C24 C 0.9515(11) 0.5416(4) 0.2388(5) 0.037(2) Uani 1 1 d . . . . .
C25 C 0.8529(12) 0.5833(4) 0.2467(6) 0.039(2) Uani 1 1 d . . . . .
H25 H 0.875246 0.623001 0.239287 0.047 Uiso 1 1 calc R . . . .
C26 C 0.7206(11) 0.5693(4) 0.2655(5) 0.0325(19) Uani 1 1 d . . . . .
C27 C 0.6116(12) 0.6167(4) 0.2675(6) 0.040(2) Uani 1 1 d . . . . .
O9 O 0.341(2) 0.3117(9) 0.0323(11) 0.148(7) Uiso 1 1 d D . . . .
C1E C 0.541(3) 0.2622(14) 0.1314(17) 0.151(11) Uiso 1 1 d D . . . .
H1EA H 0.575194 0.224200 0.152012 0.227 Uiso 1 1 calc R . . . .
H1EB H 0.613211 0.281290 0.106185 0.227 Uiso 1 1 calc R . . . .
H1EC H 0.518617 0.286360 0.175020 0.227 Uiso 1 1 calc R . . . .
C2E C 0.412(2) 0.2540(9) 0.0724(13) 0.100(6) Uiso 1 1 d D . . . .
H2EA H 0.341389 0.233419 0.098549 0.120 Uiso 1 1 calc R . . . .
H2EB H 0.435670 0.228366 0.029942 0.120 Uiso 1 1 calc R . . . .
C3E C 0.212(2) 0.3050(11) -0.0410(14) 0.111(7) Uiso 1 1 d D . . . .
H3EA H 0.127873 0.290168 -0.020863 0.133 Uiso 0.6666 1 calc R . P A 1
H3EB H 0.188900 0.343701 -0.064834 0.133 Uiso 0.6666 1 calc R . P A 1
H3EC H 0.191878 0.344207 -0.063847 0.133 Uiso 0.3333 1 calc R . P B 2
H3ED H 0.247223 0.281216 -0.082094 0.133 Uiso 0.3333 1 calc R . P B 2
C4E C 0.249(8) 0.265(3) -0.103(4) 0.27(4) Uiso 0.6666 1 d D . P C 1
H4EA H 0.168828 0.261860 -0.146014 0.402 Uiso 0.6666 1 calc R . P C 1
H4EB H 0.330971 0.279660 -0.123787 0.402 Uiso 0.6666 1 calc R . P C 1
H4EC H 0.269970 0.226149 -0.079834 0.402 Uiso 0.6666 1 calc R . P C 1
C5E C 0.076(8) 0.279(6) -0.027(9) 0.25(7) Uiso 0.3333 1 d D . P C 2
H5EA H 0.010093 0.278412 -0.077098 0.377 Uiso 0.3333 1 calc R . P C 2
H5EB H 0.091459 0.239607 -0.006858 0.377 Uiso 0.3333 1 calc R . P C 2
H5EC H 0.035784 0.302972 0.011498 0.377 Uiso 0.3333 1 calc R . P C 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Gd1 0.0289(3) 0.0281(3) 0.0258(3) 0.00081(14) 0.00740(18) 0.00011(15)
F1 0.30(2) 0.095(8) 0.100(8) 0.024(6) 0.127(11) 0.085(10)
F2 0.202(13) 0.046(5) 0.146(10) -0.020(5) 0.111(10) 0.016(6)
F3 0.108(10) 0.112(10) 0.231(17) -0.028(10) 0.107(11) 0.021(8)
F4 0.36(2) 0.025(4) 0.261(18) 0.025(7) 0.239(19) 0.016(8)
F5 0.143(12) 0.172(15) 0.142(11) 0.013(10) 0.041(9) -0.102(11)
F6 0.181(13) 0.080(7) 0.067(6) 0.020(5) 0.043(7) -0.037(7)
F7 0.050(4) 0.114(7) 0.053(4) 0.010(4) 0.005(3) 0.028(4)
F8 0.055(4) 0.100(6) 0.052(4) 0.029(4) 0.001(3) 0.010(4)
F9 0.066(6) 0.057(5) 0.161(11) 0.001(6) -0.045(6) -0.016(4)
F10 0.048(4) 0.158(9) 0.044(4) 0.011(5) 0.016(3) -0.015(5)
F11 0.058(5) 0.110(7) 0.040(3) 0.027(4) 0.019(3) 0.017(4)
F12 0.100(7) 0.093(7) 0.067(5) -0.006(5) 0.046(5) 0.030(5)
F13 0.096(6) 0.076(5) 0.067(5) 0.010(4) 0.058(5) -0.004(5)
F14 0.043(5) 0.114(8) 0.106(7) -0.024(6) 0.023(5) -0.031(5)
F15 0.126(9) 0.040(5) 0.279(17) 0.001(7) 0.146(11) -0.018(5)
F16 0.064(5) 0.070(5) 0.061(4) -0.013(4) -0.021(4) 0.029(4)
F17 0.093(7) 0.039(4) 0.148(9) 0.035(5) 0.054(6) 0.011(4)
F18 0.060(4) 0.058(4) 0.043(3) -0.004(3) 0.007(3) 0.019(3)
O1 0.066(6) 0.070(6) 0.034(4) 0.002(3) -0.008(4) 0.003(4)
O2 0.043(5) 0.090(8) 0.057(5) 0.011(4) -0.008(4) 0.005(4)
O3 0.038(4) 0.039(4) 0.036(3) 0.003(3) 0.011(3) 0.010(3)
O4 0.042(4) 0.031(3) 0.041(4) -0.001(3) 0.012(3) -0.006(3)
O5 0.034(4) 0.045(4) 0.030(3) 0.000(3) 0.006(3) -0.002(3)
O6 0.035(4) 0.032(3) 0.031(3) 0.000(3) 0.006(3) 0.000(3)
O7 0.042(4) 0.032(3) 0.037(3) 0.000(3) 0.016(3) -0.004(3)
O8 0.035(4) 0.033(3) 0.040(3) 0.005(3) 0.011(3) 0.001(3)
N1 0.026(4) 0.028(4) 0.029(4) 0.003(3) 0.012(3) 0.004(3)
N2 0.036(4) 0.036(4) 0.031(4) 0.000(3) 0.007(3) 0.003(3)
C1 0.038(6) 0.052(6) 0.031(5) 0.002(4) 0.011(4) 0.000(4)
C2 0.056(7) 0.048(6) 0.031(5) 0.003(4) 0.018(5) 0.004(5)
C3 0.061(7) 0.039(6) 0.031(5) -0.001(4) 0.007(5) 0.010(5)
C4 0.048(6) 0.038(5) 0.033(5) -0.004(4) 0.003(4) 0.002(4)
C5 0.063(9) 0.088(11) 0.036(6) -0.011(6) -0.004(6) 0.005(7)
C6 0.055(8) 0.064(8) 0.051(7) 0.009(5) -0.005(6) -0.001(6)
C7 0.040(6) 0.041(5) 0.048(6) 0.008(4) -0.001(5) -0.003(4)
C8 0.029(6) 0.060(7) 0.065(8) 0.011(6) 0.001(5) -0.002(5)
C9 0.043(7) 0.064(8) 0.054(6) 0.004(6) 0.014(5) 0.001(5)
C10 0.032(5) 0.049(6) 0.039(5) 0.002(4) 0.010(4) 0.001(4)
C11 0.035(5) 0.026(4) 0.038(5) 0.001(3) 0.005(4) 0.002(3)
C12 0.038(6) 0.043(5) 0.026(4) -0.002(3) 0.002(4) -0.001(4)
C13 0.123(16) 0.049(8) 0.096(12) 0.001(7) 0.073(11) 0.028(9)
C14 0.071(8) 0.033(5) 0.051(6) -0.002(4) 0.021(6) 0.013(5)
C15 0.108(12) 0.036(6) 0.077(9) 0.006(6) 0.053(9) 0.015(7)
C16 0.071(8) 0.031(5) 0.050(6) -0.004(4) 0.024(5) -0.008(5)
C17 0.131(15) 0.034(6) 0.082(10) -0.005(6) 0.061(10) -0.017(7)
C18 0.036(6) 0.060(7) 0.037(5) 0.002(5) 0.000(4) -0.001(5)
C19 0.043(6) 0.033(5) 0.031(4) -0.001(4) 0.005(4) -0.006(4)
C20 0.037(5) 0.051(6) 0.031(4) 0.004(4) 0.004(4) -0.001(4)
C21 0.031(5) 0.041(5) 0.031(5) -0.003(3) 0.007(4) 0.001(4)
C22 0.042(6) 0.071(8) 0.031(5) 0.000(5) 0.009(4) 0.003(5)
C23 0.068(9) 0.043(6) 0.077(9) -0.003(6) 0.040(7) -0.015(6)
C24 0.043(6) 0.039(5) 0.031(4) -0.001(4) 0.010(4) -0.008(4)
C25 0.052(6) 0.031(5) 0.037(5) 0.000(4) 0.015(4) -0.007(4)
C26 0.039(5) 0.034(5) 0.023(4) 0.001(3) 0.002(4) -0.002(4)
C27 0.047(6) 0.028(5) 0.044(5) 0.006(4) 0.005(4) 0.003(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O3 2.382(7) . ?
Gd1 O4 2.376(7) . ?
Gd1 O5 2.361(7) . ?
Gd1 O6 2.349(6) . ?
Gd1 O7 2.355(6) . ?
Gd1 O8 2.349(7) . ?
Gd1 N1 2.585(8) . ?
Gd1 N2 2.555(9) . ?
F1 C13 1.32(2) . ?
F2 C13 1.332(19) . ?
F3 C13 1.26(3) . ?
F4 C17 1.278(17) . ?
F5 C17 1.36(2) . ?
F6 C17 1.274(17) . ?
F7 C18 1.306(13) . ?
F8 C18 1.321(13) . ?
F9 C18 1.314(15) . ?
F10 C22 1.323(15) . ?
F11 C22 1.329(13) . ?
F12 C22 1.331(15) . ?
F13 C23 1.332(16) . ?
F14 C23 1.339(19) . ?
F15 C23 1.331(15) . ?
F16 C27 1.324(13) . ?
F17 C27 1.334(12) . ?
F18 C27 1.321(12) . ?
O1 C5 1.237(15) . ?
O2 C6 1.230(17) . ?
O3 C14 1.240(13) . ?
O4 C16 1.222(13) . ?
O5 C19 1.259(11) . ?
O6 C21 1.247(12) . ?
O7 C24 1.264(12) . ?
O8 C26 1.256(11) . ?
N1 C1 1.340(13) . ?
N1 C12 1.341(13) . ?
N2 C10 1.341(13) . ?
N2 C11 1.346(13) . ?
C1 H1 0.9500 . ?
C1 C2 1.395(15) . ?
C2 H2 0.9500 . ?
C2 C3 1.367(18) . ?
C3 H3 0.9500 . ?
C3 C4 1.405(17) . ?
C4 C5 1.466(19) . ?
C4 C12 1.401(14) . ?
C5 C6 1.54(2) . ?
C6 C7 1.472(17) . ?
C7 C8 1.372(17) . ?
C7 C11 1.387(15) . ?
C8 H8 0.9500 . ?
C8 C9 1.365(17) . ?
C9 H9 0.9500 . ?
C9 C10 1.360(16) . ?
C10 H10 0.9500 . ?
C11 C12 1.471(14) . ?
C13 C14 1.527(16) . ?
C14 C15 1.388(18) . ?
C15 H15 0.9500 . ?
C15 C16 1.391(17) . ?
C16 C17 1.545(16) . ?
C18 C19 1.537(15) . ?
C19 C20 1.396(14) . ?
C20 H20 0.9500 . ?
C20 C21 1.400(15) . ?
C21 C22 1.535(15) . ?
C23 C24 1.515(16) . ?
C24 C25 1.371(15) . ?
C25 H25 0.9500 . ?
C25 C26 1.398(15) . ?
C26 C27 1.517(14) . ?
O9 C2E 1.60(2) . ?
O9 C3E 1.62(2) . ?
C1E H1EA 0.9800 . ?
C1E H1EB 0.9800 . ?
C1E H1EC 0.9800 . ?
C1E C2E 1.483(19) . ?
C2E H2EA 0.9900 . ?
C2E H2EB 0.9900 . ?
C3E H3EA 0.9900 . ?
C3E H3EB 0.9900 . ?
C3E H3EC 0.9900 . ?
C3E H3ED 0.9900 . ?
C3E C4E 1.490(16) . ?
C3E C5E 1.492(16) . ?
C4E H4EA 0.9800 . ?
C4E H4EB 0.9800 . ?
C4E H4EC 0.9800 . ?
C5E H5EA 0.9800 . ?
C5E H5EB 0.9800 . ?
C5E H5EC 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
O3 Gd1 N1 72.0(2) . . ?
O3 Gd1 N2 110.5(3) . . ?
O4 Gd1 O3 71.3(2) . . ?
O4 Gd1 N1 108.6(2) . . ?
O4 Gd1 N2 75.3(3) . . ?
O5 Gd1 O3 79.5(2) . . ?
O5 Gd1 O4 82.6(2) . . ?
O5 Gd1 N1 143.4(2) . . ?
O5 Gd1 N2 150.6(2) . . ?
O6 Gd1 O3 136.1(2) . . ?
O6 Gd1 O4 71.6(2) . . ?
O6 Gd1 O5 73.0(2) . . ?
O6 Gd1 O7 120.9(2) . . ?
O6 Gd1 O8 76.4(2) . . ?
O6 Gd1 N1 143.4(2) . . ?
O6 Gd1 N2 81.7(2) . . ?
O7 Gd1 O3 83.4(2) . . ?
O7 Gd1 O4 149.4(2) . . ?
O7 Gd1 O5 76.0(2) . . ?
O7 Gd1 N1 78.3(2) . . ?
O7 Gd1 N2 131.4(3) . . ?
O8 Gd1 O3 147.3(2) . . ?
O8 Gd1 O4 137.4(2) . . ?
O8 Gd1 O5 114.0(2) . . ?
O8 Gd1 O7 72.3(2) . . ?
O8 Gd1 N1 81.7(2) . . ?
O8 Gd1 N2 72.9(2) . . ?
N2 Gd1 N1 63.9(2) . . ?
C14 O3 Gd1 135.2(7) . . ?
C16 O4 Gd1 136.5(7) . . ?
C19 O5 Gd1 132.2(7) . . ?
C21 O6 Gd1 131.7(6) . . ?
C24 O7 Gd1 135.2(6) . . ?
C26 O8 Gd1 136.3(6) . . ?
C1 N1 Gd1 119.6(7) . . ?
C1 N1 C12 120.6(9) . . ?
C12 N1 Gd1 119.7(6) . . ?
C10 N2 Gd1 121.6(7) . . ?
C10 N2 C11 117.5(9) . . ?
C11 N2 Gd1 120.8(6) . . ?
N1 C1 H1 119.3 . . ?
N1 C1 C2 121.3(11) . . ?
C2 C1 H1 119.3 . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.3(10) . . ?
C3 C2 H2 120.4 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.3(10) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C5 120.7(10) . . ?
C12 C4 C3 118.8(11) . . ?
C12 C4 C5 120.5(11) . . ?
O1 C5 C4 121.8(14) . . ?
O1 C5 C6 119.2(13) . . ?
C4 C5 C6 117.9(11) . . ?
O2 C6 C5 117.7(12) . . ?
O2 C6 C7 124.1(14) . . ?
C7 C6 C5 118.0(12) . . ?
C8 C7 C6 119.9(11) . . ?
C8 C7 C11 119.1(10) . . ?
C11 C7 C6 121.0(11) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 C7 119.4(10) . . ?
C9 C8 H8 120.3 . . ?
C8 C9 H9 120.6 . . ?
C10 C9 C8 118.8(11) . . ?
C10 C9 H9 120.6 . . ?
N2 C10 C9 123.6(10) . . ?
N2 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
N2 C11 C7 121.6(10) . . ?
N2 C11 C12 117.5(9) . . ?
C7 C11 C12 120.9(9) . . ?
N1 C12 C4 120.6(10) . . ?
N1 C12 C11 117.9(8) . . ?
C4 C12 C11 121.5(10) . . ?
F1 C13 F2 106.5(16) . . ?
F1 C13 C14 110.7(13) . . ?
F2 C13 C14 113.3(14) . . ?
F3 C13 F1 105.1(17) . . ?
F3 C13 F2 107.4(15) . . ?
F3 C13 C14 113.2(16) . . ?
O3 C14 C13 114.4(11) . . ?
O3 C14 C15 127.9(11) . . ?
C15 C14 C13 117.7(11) . . ?
C14 C15 H15 119.4 . . ?
C14 C15 C16 121.1(11) . . ?
C16 C15 H15 119.4 . . ?
O4 C16 C15 127.3(11) . . ?
O4 C16 C17 113.7(10) . . ?
C15 C16 C17 119.0(11) . . ?
F4 C17 F5 103.5(17) . . ?
F4 C17 C16 114.4(12) . . ?
F5 C17 C16 108.5(15) . . ?
F6 C17 F4 113.4(17) . . ?
F6 C17 F5 103.6(14) . . ?
F6 C17 C16 112.3(12) . . ?
F7 C18 F8 106.6(10) . . ?
F7 C18 F9 109.1(11) . . ?
F7 C18 C19 112.3(9) . . ?
F8 C18 C19 112.6(9) . . ?
F9 C18 F8 106.5(10) . . ?
F9 C18 C19 109.5(10) . . ?
O5 C19 C18 115.0(9) . . ?
O5 C19 C20 127.7(10) . . ?
C20 C19 C18 117.3(9) . . ?
C19 C20 H20 119.5 . . ?
C19 C20 C21 121.0(9) . . ?
C21 C20 H20 119.5 . . ?
O6 C21 C20 128.0(9) . . ?
O6 C21 C22 115.4(9) . . ?
C20 C21 C22 116.6(9) . . ?
F10 C22 F11 106.4(11) . . ?
F10 C22 F12 107.8(11) . . ?
F10 C22 C21 111.0(9) . . ?
F11 C22 F12 107.6(9) . . ?
F11 C22 C21 113.0(9) . . ?
F12 C22 C21 110.7(10) . . ?
F13 C23 F14 105.3(12) . . ?
F13 C23 C24 111.0(11) . . ?
F14 C23 C24 112.0(11) . . ?
F15 C23 F13 107.4(12) . . ?
F15 C23 F14 107.2(13) . . ?
F15 C23 C24 113.5(11) . . ?
O7 C24 C23 113.1(10) . . ?
O7 C24 C25 127.6(9) . . ?
C25 C24 C23 119.3(10) . . ?
C24 C25 H25 119.0 . . ?
C24 C25 C26 121.9(9) . . ?
C26 C25 H25 119.0 . . ?
O8 C26 C25 126.3(9) . . ?
O8 C26 C27 113.9(9) . . ?
C25 C26 C27 119.8(8) . . ?
F16 C27 F17 107.5(9) . . ?
F16 C27 C26 111.1(8) . . ?
F17 C27 C26 113.7(9) . . ?
F18 C27 F16 106.3(9) . . ?
F18 C27 F17 106.3(9) . . ?
F18 C27 C26 111.5(8) . . ?
C2E O9 C3E 118.6(18) . . ?
H1EA C1E H1EB 109.5 . . ?
H1EA C1E H1EC 109.5 . . ?
H1EB C1E H1EC 109.5 . . ?
C2E C1E H1EA 109.5 . . ?
C2E C1E H1EB 109.5 . . ?
C2E C1E H1EC 109.5 . . ?
O9 C2E H2EA 108.2 . . ?
O9 C2E H2EB 108.2 . . ?
C1E C2E O9 117(2) . . ?
C1E C2E H2EA 108.2 . . ?
C1E C2E H2EB 108.2 . . ?
H2EA C2E H2EB 107.3 . . ?
O9 C3E H3EA 109.2 . . ?
O9 C3E H3EB 109.2 . . ?
O9 C3E H3EC 107.4 . . ?
O9 C3E H3ED 107.4 . . ?
H3EA C3E H3EB 107.9 . . ?
H3EC C3E H3ED 106.9 . . ?
C4E C3E O9 112(4) . . ?
C4E C3E H3EA 109.2 . . ?
C4E C3E H3EB 109.2 . . ?
C5E C3E O9 120(6) . . ?
C5E C3E H3EC 107.4 . . ?
C5E C3E H3ED 107.4 . . ?
C3E C4E H4EA 109.5 . . ?
C3E C4E H4EB 109.5 . . ?
C3E C4E H4EC 109.5 . . ?
H4EA C4E H4EB 109.5 . . ?
H4EA C4E H4EC 109.5 . . ?
H4EB C4E H4EC 109.5 . . ?
C3E C5E H5EA 109.5 . . ?
C3E C5E H5EB 109.5 . . ?
C3E C5E H5EC 109.5 . . ?
H5EA C5E H5EB 109.5 . . ?
H5EA C5E H5EC 109.5 . . ?
H5EB C5E H5EC 109.5 . . ?
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
Gd1 O3 C14 C13 176.5(11) . . . . ?
Gd1 O3 C14 C15 -7(2) . . . . ?
Gd1 O4 C16 C15 -9(2) . . . . ?
Gd1 O4 C16 C17 171.5(10) . . . . ?
Gd1 O5 C19 C18 168.6(7) . . . . ?
Gd1 O5 C19 C20 -12.4(16) . . . . ?
Gd1 O6 C21 C20 22.3(15) . . . . ?
Gd1 O6 C21 C22 -156.8(7) . . . . ?
Gd1 O7 C24 C23 178.9(8) . . . . ?
Gd1 O7 C24 C25 -2.3(16) . . . . ?
Gd1 O8 C26 C25 -0.1(15) . . . . ?
Gd1 O8 C26 C27 -179.8(6) . . . . ?
Gd1 N1 C1 C2 178.3(8) . . . . ?
Gd1 N1 C12 C4 -179.9(7) . . . . ?
Gd1 N1 C12 C11 0.9(11) . . . . ?
Gd1 N2 C10 C9 176.4(10) . . . . ?
Gd1 N2 C11 C7 -176.5(7) . . . . ?
Gd1 N2 C11 C12 4.5(11) . . . . ?
F1 C13 C14 O3 -41(2) . . . . ?
F1 C13 C14 C15 142.4(18) . . . . ?
F2 C13 C14 O3 -160.3(15) . . . . ?
F2 C13 C14 C15 23(2) . . . . ?
F3 C13 C14 O3 77.1(18) . . . . ?
F3 C13 C14 C15 -99.8(18) . . . . ?
F7 C18 C19 O5 -33.2(14) . . . . ?
F7 C18 C19 C20 147.7(10) . . . . ?
F8 C18 C19 O5 -153.6(10) . . . . ?
F8 C18 C19 C20 27.3(14) . . . . ?
F9 C18 C19 O5 88.2(12) . . . . ?
F9 C18 C19 C20 -91.0(13) . . . . ?
F13 C23 C24 O7 61.3(15) . . . . ?
F13 C23 C24 C25 -117.7(12) . . . . ?
F14 C23 C24 O7 -56.1(14) . . . . ?
F14 C23 C24 C25 125.0(12) . . . . ?
F15 C23 C24 O7 -177.6(13) . . . . ?
F15 C23 C24 C25 3.4(19) . . . . ?
O1 C5 C6 O2 3(2) . . . . ?
O1 C5 C6 C7 -172.6(12) . . . . ?
O2 C6 C7 C8 8(2) . . . . ?
O2 C6 C7 C11 -169.7(12) . . . . ?
O3 C14 C15 C16 6(3) . . . . ?
O4 C16 C17 F4 174.4(18) . . . . ?
O4 C16 C17 F5 59.4(16) . . . . ?
O4 C16 C17 F6 -55(2) . . . . ?
O5 C19 C20 C21 -6.4(17) . . . . ?
O6 C21 C22 F10 41.3(14) . . . . ?
O6 C21 C22 F11 160.7(10) . . . . ?
O6 C21 C22 F12 -78.4(12) . . . . ?
O7 C24 C25 C26 -3.8(17) . . . . ?
O8 C26 C27 F16 -55.0(11) . . . . ?
O8 C26 C27 F17 -176.5(9) . . . . ?
O8 C26 C27 F18 63.4(11) . . . . ?
N1 C1 C2 C3 1.6(16) . . . . ?
N2 C11 C12 N1 -3.5(13) . . . . ?
N2 C11 C12 C4 177.3(9) . . . . ?
C1 N1 C12 C4 -1.7(13) . . . . ?
C1 N1 C12 C11 179.2(8) . . . . ?
C1 C2 C3 C4 -1.4(15) . . . . ?
C2 C3 C4 C5 177.9(11) . . . . ?
C2 C3 C4 C12 -0.1(14) . . . . ?
C3 C4 C5 O1 -9.8(19) . . . . ?
C3 C4 C5 C6 -177.6(11) . . . . ?
C3 C4 C12 N1 1.7(14) . . . . ?
C3 C4 C12 C11 -179.2(9) . . . . ?
C4 C5 C6 O2 171.1(12) . . . . ?
C4 C5 C6 C7 -4.4(18) . . . . ?
C5 C4 C12 N1 -176.4(10) . . . . ?
C5 C4 C12 C11 2.7(15) . . . . ?
C5 C6 C7 C8 -176.3(12) . . . . ?
C5 C6 C7 C11 5.6(18) . . . . ?
C6 C7 C8 C9 -178.7(13) . . . . ?
C6 C7 C11 N2 178.4(10) . . . . ?
C6 C7 C11 C12 -2.6(15) . . . . ?
C7 C8 C9 C10 1(2) . . . . ?
C7 C11 C12 N1 177.4(9) . . . . ?
C7 C11 C12 C4 -1.7(14) . . . . ?
C8 C7 C11 N2 0.2(16) . . . . ?
C8 C7 C11 C12 179.2(11) . . . . ?
C8 C9 C10 N2 0(2) . . . . ?
C10 N2 C11 C7 0.2(14) . . . . ?
C10 N2 C11 C12 -178.9(9) . . . . ?
C11 N2 C10 C9 -0.3(16) . . . . ?
C11 C7 C8 C9 -0.6(19) . . . . ?
C12 N1 C1 C2 0.0(14) . . . . ?
C12 C4 C5 O1 168.3(12) . . . . ?
C12 C4 C5 C6 0.4(17) . . . . ?
C13 C14 C15 C16 -177.1(16) . . . . ?
C14 C15 C16 O4 1(3) . . . . ?
C14 C15 C16 C17 -178.8(16) . . . . ?
C15 C16 C17 F4 -6(3) . . . . ?
C15 C16 C17 F5 -120.6(16) . . . . ?
C15 C16 C17 F6 125.5(17) . . . . ?
C18 C19 C20 C21 172.7(10) . . . . ?
C19 C20 C21 O6 1.3(17) . . . . ?
C19 C20 C21 C22 -179.6(10) . . . . ?
C20 C21 C22 F10 -137.9(11) . . . . ?
C20 C21 C22 F11 -18.5(14) . . . . ?
C20 C21 C22 F12 102.4(12) . . . . ?
C23 C24 C25 C26 175.0(11) . . . . ?
C24 C25 C26 O8 4.9(16) . . . . ?
C24 C25 C26 C27 -175.4(9) . . . . ?
C25 C26 C27 F16 125.3(10) . . . . ?
C25 C26 C27 F17 3.9(14) . . . . ?
C25 C26 C27 F18 -116.2(10) . . . . ?
C2E O9 C3E C4E -50(4) . . . . ?
C2E O9 C3E C5E 67(7) . . . . ?
C3E O9 C2E C1E 172(2) . . . . ?
_shelx_res_file
;
TITL 2018ncs0102_a.res in P2(1)/c
2018ncs0102.res
created by SHELXL-2018/1 at 11:42:30 on 23-Mar-2018
REM Old TITL 2018ncs0102 in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.140, Rweak 0.060, Alpha 0.065, Orientation as input
REM Formula found by SHELXT: C32 O9 F18 Gd
CELL 0.71073 9.62 22.9967 17.1078 90 98.928 90
ZERR 4 0.0003 0.0006 0.0004 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H F Gd N O
UNIT 124 76 72 4 8 36
DFIX 1.51 C5E C3E C4E C3E
SADI O9 C2E O9 C3E
SADI C4E C3E C5E C3E C2E C1E
L.S. 10
PLAN 20
SIZE 0.096 0.193 0.407
TEMP -173(2)
conf
BOND $H
list 4
fmap 2
acta
OMIT -10 3 3
OMIT -10 4 4
OMIT -10 1 2
OMIT -11 4 2
OMIT -10 7 2
OMIT -9 4 2
OMIT -11 6 3
OMIT -11 10 4
OMIT -11 4 4
OMIT -11 7 4
REM
REM
REM
WGHT 0.151000 43.299000
FVAR 0.22370
GD1 4 0.774843 0.425440 0.292857 11.00000 0.02889 0.02805 =
0.02584 0.00081 0.00740 0.00011
F1 3 0.983912 0.296079 0.115814 11.00000 0.29625 0.09453 =
0.10028 0.02377 0.12671 0.08503
F2 3 0.974703 0.213959 0.172214 11.00000 0.20209 0.04617 =
0.14617 -0.01990 0.11131 0.01578
F3 3 1.131095 0.274943 0.211860 11.00000 0.10772 0.11215 =
0.23137 -0.02841 0.10740 0.02062
F4 3 0.724179 0.187800 0.385220 11.00000 0.36075 0.02473 =
0.26141 0.02540 0.23949 0.01621
F5 3 0.551158 0.242363 0.375423 11.00000 0.14258 0.17243 =
0.14183 0.01316 0.04121 -0.10228
F6 3 0.716116 0.258079 0.465801 11.00000 0.18136 0.08000 =
0.06706 0.01986 0.04330 -0.03669
F7 3 1.210443 0.363910 0.456186 11.00000 0.04975 0.11440 =
0.05265 0.00980 0.00544 0.02751
F8 3 1.141473 0.356928 0.566842 11.00000 0.05487 0.10015 =
0.05166 0.02940 0.00123 0.00972
F9 3 1.203021 0.439016 0.528734 11.00000 0.06618 0.05709 =
0.16134 0.00146 -0.04489 -0.01583
F10 3 0.515819 0.400776 0.506094 11.00000 0.04758 0.15771 =
0.04375 0.01052 0.01564 -0.01538
F11 3 0.678895 0.386448 0.602977 11.00000 0.05759 0.11010 =
0.04042 0.02676 0.01946 0.01683
F12 3 0.618042 0.473748 0.568651 11.00000 0.09982 0.09342 =
0.06727 -0.00610 0.04562 0.03025
F13 3 1.101528 0.534036 0.143315 11.00000 0.09603 0.07591 =
0.06699 0.01011 0.05818 -0.00378
F14 3 1.200634 0.541697 0.262732 11.00000 0.04314 0.11427 =
0.10586 -0.02364 0.02264 -0.03146
F15 3 1.100780 0.616293 0.202485 11.00000 0.12642 0.03958 =
0.27919 0.00147 0.14561 -0.01756
F16 3 0.492496 0.603728 0.220886 11.00000 0.06360 0.07030 =
0.06103 -0.01341 -0.02097 0.02921
F17 3 0.652892 0.668805 0.245627 11.00000 0.09343 0.03873 =
0.14787 0.03473 0.05420 0.01092
F18 3 0.579419 0.623325 0.339278 11.00000 0.05994 0.05832 =
0.04329 -0.00386 0.00685 0.01897
O1 6 0.315036 0.430834 -0.071202 11.00000 0.06567 0.07009 =
0.03440 0.00231 -0.00826 0.00304
O2 6 0.129648 0.425055 0.032811 11.00000 0.04303 0.08960 =
0.05666 0.01060 -0.00750 0.00525
O3 6 0.901147 0.351811 0.235511 11.00000 0.03787 0.03920 =
0.03606 0.00281 0.01115 0.01005
O4 6 0.716523 0.333648 0.342664 11.00000 0.04198 0.03060 =
0.04138 -0.00149 0.01196 -0.00649
O5 6 0.974253 0.415824 0.391568 11.00000 0.03358 0.04459 =
0.03032 -0.00039 0.00646 -0.00233
O6 6 0.698352 0.440206 0.415227 11.00000 0.03541 0.03183 =
0.03142 0.00011 0.00575 0.00034
O7 6 0.942806 0.487503 0.250254 11.00000 0.04205 0.03249 =
0.03666 0.00011 0.01567 -0.00368
O8 6 0.679294 0.519630 0.281989 11.00000 0.03518 0.03318 =
0.03964 0.00501 0.01089 0.00082
N1 5 0.693765 0.426814 0.141570 11.00000 0.02608 0.02809 =
0.02854 0.00253 0.01175 0.00363
N2 5 0.510543 0.414648 0.246698 11.00000 0.03648 0.03618 =
0.03124 0.00010 0.00696 0.00313
C1 1 0.789711 0.430691 0.092757 11.00000 0.03762 0.05216 =
0.03125 0.00211 0.01144 -0.00014
AFIX 43
H1 2 0.886471 0.433969 0.114435 11.00000 -1.20000
AFIX 0
C2 1 0.750383 0.430011 0.010776 11.00000 0.05600 0.04779 =
0.03126 0.00337 0.01828 0.00439
AFIX 43
H2 2 0.819800 0.431830 -0.023049 11.00000 -1.20000
AFIX 0
C3 1 0.610928 0.426699 -0.020362 11.00000 0.06118 0.03946 =
0.03089 -0.00130 0.00710 0.01020
AFIX 43
H3 2 0.582276 0.427085 -0.076060 11.00000 -1.20000
AFIX 0
C4 1 0.510339 0.422720 0.030816 11.00000 0.04766 0.03834 =
0.03312 -0.00368 0.00256 0.00174
C5 1 0.359663 0.421084 -0.000644 11.00000 0.06288 0.08753 =
0.03601 -0.01075 -0.00390 0.00501
C6 1 0.255416 0.419133 0.058763 11.00000 0.05466 0.06417 =
0.05076 0.00912 -0.00510 -0.00089
C7 1 0.312902 0.414650 0.143464 11.00000 0.04047 0.04086 =
0.04849 0.00778 -0.00090 -0.00255
C8 1 0.223519 0.409445 0.198257 11.00000 0.02856 0.05958 =
0.06489 0.01127 0.00052 -0.00150
AFIX 43
H8 2 0.124642 0.407933 0.181718 11.00000 -1.20000
AFIX 0
C9 1 0.277896 0.406459 0.276712 11.00000 0.04317 0.06362 =
0.05407 0.00361 0.01355 0.00093
AFIX 43
H9 2 0.217713 0.402534 0.315484 11.00000 -1.20000
AFIX 0
C10 1 0.419850 0.409207 0.298354 11.00000 0.03154 0.04878 =
0.03876 0.00178 0.00956 0.00088
AFIX 43
H10 2 0.456796 0.407158 0.353103 11.00000 -1.20000
AFIX 0
C11 1 0.456697 0.417270 0.169331 11.00000 0.03528 0.02582 =
0.03844 0.00135 0.00467 0.00167
C12 1 0.556437 0.422132 0.112595 11.00000 0.03829 0.04289 =
0.02641 -0.00183 0.00193 -0.00060
C13 1 1.001550 0.270205 0.185842 11.00000 0.12327 0.04934 =
0.09632 0.00117 0.07309 0.02794
C14 1 0.907935 0.298042 0.239840 11.00000 0.07132 0.03296 =
0.05077 -0.00197 0.02069 0.01319
C15 1 0.847274 0.261729 0.289871 11.00000 0.10813 0.03575 =
0.07749 0.00587 0.05311 0.01478
AFIX 43
H15 2 0.868572 0.221371 0.291086 11.00000 -1.20000
AFIX 0
C16 1 0.755833 0.283413 0.338262 11.00000 0.07054 0.03088 =
0.05012 -0.00421 0.02379 -0.00757
C17 1 0.693515 0.241242 0.393981 11.00000 0.13112 0.03392 =
0.08167 -0.00503 0.06105 -0.01736
C18 1 1.138142 0.390591 0.504013 11.00000 0.03571 0.06015 =
0.03710 0.00247 0.00013 -0.00131
C19 1 0.987310 0.404554 0.464354 11.00000 0.04295 0.03291 =
0.03109 -0.00060 0.00536 -0.00628
C20 1 0.882287 0.404144 0.512239 11.00000 0.03729 0.05073 =
0.03070 0.00351 0.00395 -0.00070
AFIX 43
H20 2 0.904012 0.391041 0.565396 11.00000 -1.20000
AFIX 0
C21 1 0.745469 0.422736 0.483156 11.00000 0.03083 0.04129 =
0.03073 -0.00346 0.00742 0.00077
C22 1 0.638744 0.420809 0.541112 11.00000 0.04188 0.07142 =
0.03069 0.00024 0.00857 0.00294
C23 1 1.088297 0.559184 0.211901 11.00000 0.06769 0.04343 =
0.07683 -0.00254 0.03980 -0.01452
C24 1 0.951495 0.541571 0.238789 11.00000 0.04252 0.03932 =
0.03125 -0.00124 0.00981 -0.00849
C25 1 0.852938 0.583343 0.246730 11.00000 0.05218 0.03139 =
0.03676 0.00047 0.01474 -0.00716
AFIX 43
H25 2 0.875246 0.623001 0.239287 11.00000 -1.20000
AFIX 0
C26 1 0.720555 0.569291 0.265461 11.00000 0.03926 0.03398 =
0.02346 0.00058 0.00220 -0.00224
C27 1 0.611561 0.616691 0.267507 11.00000 0.04693 0.02816 =
0.04385 0.00606 0.00528 0.00344
O9 6 0.340503 0.311663 0.032271 11.00000 0.14827
C1E 1 0.540654 0.262161 0.131408 11.00000 0.15111
AFIX 33
H1EA 2 0.575194 0.224200 0.152012 11.00000 -1.50000
H1EB 2 0.613211 0.281290 0.106185 11.00000 -1.50000
H1EC 2 0.518617 0.286360 0.175020 11.00000 -1.50000
AFIX 0
C2E 1 0.411979 0.254042 0.072420 11.00000 0.09967
AFIX 23
H2EA 2 0.341389 0.233419 0.098549 11.00000 -1.20000
H2EB 2 0.435670 0.228366 0.029942 11.00000 -1.20000
AFIX 0
C3E 1 0.212204 0.304999 -0.041012 11.00000 0.11078
PART 1
AFIX 23
H3EA 2 0.127873 0.290168 -0.020863 10.66660 -1.20000
H3EB 2 0.188900 0.343701 -0.064834 10.66660 -1.20000
AFIX 23
PART 0
PART 2
H3EC 2 0.191878 0.344207 -0.063847 10.33333 -1.20000
H3ED 2 0.247223 0.281216 -0.082094 10.33333 -1.20000
AFIX 0
PART 0
PART 1
C4E 1 0.248607 0.264722 -0.102960 10.66660 0.26816
AFIX 33
H4EA 2 0.168828 0.261860 -0.146014 10.66660 -1.50000
H4EB 2 0.330971 0.279660 -0.123787 10.66660 -1.50000
H4EC 2 0.269970 0.226149 -0.079834 10.66660 -1.50000
AFIX 0
PART 0
PART 2
C5E 1 0.075665 0.279291 -0.027180 10.33333 0.25139
AFIX 33
H5EA 2 0.010093 0.278412 -0.077098 10.33333 -1.50000
H5EB 2 0.091459 0.239607 -0.006858 10.33333 -1.50000
H5EC 2 0.035784 0.302972 0.011498 10.33333 -1.50000
AFIX 0
HKLF 4
REM 2018ncs0102_a.res in P2(1)/c
REM R1 = 0.0915 for 7233 Fo > 4sig(Fo) and 0.1014 for all 8526 data
REM 529 parameters refined using 6 restraints
END
WGHT 0.1514 42.7768
REM Highest difference peak 5.745, deepest hole -2.717, 1-sigma level 0.330
Q1 1 0.8685 0.4258 0.2942 11.00000 0.05 5.75
Q2 1 0.6831 0.4255 0.2900 11.00000 0.05 5.62
Q3 1 0.7640 0.4256 0.2362 11.00000 0.05 4.80
Q4 1 0.7874 0.4258 0.3465 11.00000 0.05 4.46
Q5 1 0.4095 0.3095 0.0666 11.00000 0.05 2.66
Q6 1 0.6035 0.4252 0.2980 11.00000 0.05 1.59
Q7 1 0.9470 0.4244 0.2822 11.00000 0.05 1.46
Q8 1 0.3574 0.3294 -0.0093 11.00000 0.05 1.45
Q9 1 0.7615 0.4287 0.1436 11.00000 0.05 1.37
Q10 1 0.2835 0.3103 0.0357 11.00000 0.05 1.23
Q11 1 0.6248 0.4377 0.4010 11.00000 0.05 1.20
Q12 1 0.1877 0.2895 -0.0155 11.00000 0.05 1.18
Q13 1 0.2834 0.3899 0.0408 11.00000 0.05 1.15
Q14 1 0.6611 0.4262 0.0943 11.00000 0.05 1.14
Q15 1 0.8276 0.2013 0.4221 11.00000 0.05 1.05
Q16 1 0.2448 0.4077 0.2757 11.00000 0.05 0.99
Q17 1 0.2395 0.3090 -0.0620 11.00000 0.05 0.96
Q18 1 1.1754 0.2215 0.1923 11.00000 0.05 0.93
Q19 1 0.4908 0.6202 0.3172 11.00000 0.05 0.90
Q20 1 0.4957 0.2767 0.1267 11.00000 0.05 0.89
;
_shelx_res_checksum 45997
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.747
_oxdiff_exptl_absorpt_empirical_full_min 0.328
#######################################################################
#
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1832434'
_audit_update_record
;
2018-03-26 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;
# 2018ncs0245
# [Y(hfac)3(n,N'-O,O'-pd)VCptet2]
_audit_creation_date 2018-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2018/1
# start Validation Reply Form
_vrf_THETM01_2018ncs0245
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Despite using the high flux system at the National Crystallography Service
the crystals did not diffract to high resolution and data were collected to
1 angstrom resolution.
;
_vrf_REFNR01_2018ncs0245
;
PROBLEM: Ratio of reflections to parameters is < 8 for a
RESPONSE: Despite using the high flux system at the National Crystallography Service
the crystals did not diffract to high resolution and data were collected to
1 angstrom resolution.
;
_vrf_PLAT088_2018ncs0245
;
PROBLEM: Poor Data / Parameter Ratio .................... 7.44 Note
RESPONSE: Despite using the high flux system at the National Crystallography Service
the crystals did not diffract to high resolution and data were collected to
1 angstrom resolution.
;
_vrf_PLAT201_2018ncs0245
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 2 Report
RESPONSE: Several CF3 groups are modelled with the F over 2 partially
occupied sites and isotropic adps retained.
;
# end Validation Reply Form
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C45 H35 F18 N2 O8 V Y'
_chemical_formula_sum 'C45 H35 F18 N2 O8 V Y'
_chemical_formula_weight 1213.60
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -0.2670 2.0244 '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 'I 1 2/a 1'
_space_group_name_Hall '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
_cell_length_a 25.411(6)
_cell_length_b 14.7276(17)
_cell_length_c 26.741(4)
_cell_angle_alpha 90
_cell_angle_beta 106.92(2)
_cell_angle_gamma 90
_cell_volume 9575(3)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 2124
_cell_measurement_temperature 100.01(10)
_cell_measurement_theta_max 52.0940
_cell_measurement_theta_min 3.4410
_shelx_estimated_absorpt_T_max 0.879
_shelx_estimated_absorpt_T_min 0.810
_exptl_absorpt_coefficient_mu 4.396
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.51738
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour black
_exptl_crystal_colour_primary black
_exptl_crystal_density_diffrn 1.684
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description irregular
_exptl_crystal_F_000 4856
_exptl_crystal_size_max 0.05
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_min 0.03
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0699
_diffrn_reflns_av_unetI/netI 0.0844
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max 25
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 12868
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full 50.433
_diffrn_reflns_theta_max 50.433
_diffrn_reflns_theta_min 3.455
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.01(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_source 'Rotating-anode X-ray tube'
_diffrn_source_type 'Rigaku (Cu) X-ray Source'
_diffrn_standards_number ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3121
_reflns_number_total 4967
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution 'SHELXS-97 (Sheldrick 2008)'
_refine_diff_density_max 1.465
_refine_diff_density_min -1.855
_refine_diff_density_rms 0.159
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.024
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 668
_refine_ls_number_reflns 4967
_refine_ls_number_restraints 752
_refine_ls_R_factor_all 0.1426
_refine_ls_R_factor_gt 0.0983
_refine_ls_restrained_S_all 0.961
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2462
_refine_ls_wR_factor_ref 0.2812
_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. Restrained distances
F6-C17 = F5-C17 = F4-C17 = F3-C13 = F1-C13 = F2-C13 = F10-C22 = F12-C22 = F11-
C22 = F8-C18 = F9-C18 = F7-C18 = F18A-C27 = F15A-C23 = F13A-C23 = F14A-C23 =
F14-C23 = F17A-C27 = F18-C27 = F17-C27 = F16-C27 = F16A-C27
1.33 with sigma of 0.02
F13-C23 = F15-C23
1.37 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C22)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
All non-hydrogen atoms
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
Fixed Sof: F13(0.5) F14(0.5) F15(0.5) F16(0.5) F17(0.5) F18(0.5) F13A(0.5)
F14A(0.5) F15A(0.5) F16A(0.5) F17A(0.5) F18A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C15(H15), C20(H20),
C25(H25), C28(H28), C33(H33)
6.b Idealised Me refined as rotating group:
C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,
H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,
H45B,H45C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.54027(4) 0.55642(8) 0.35620(4) 0.0503(5) Uani 1 1 d . U . . .
V1 V 0.33196(9) 0.98803(17) 0.37722(9) 0.0534(7) Uani 1 1 d . U . . .
F1 F 0.4408(5) 0.7557(8) 0.2111(4) 0.119(4) Uani 1 1 d D U . . .
F2 F 0.4205(5) 0.6588(8) 0.1475(4) 0.136(4) Uani 1 1 d D U . . .
F3 F 0.5009(5) 0.7058(8) 0.1781(4) 0.115(3) Uani 1 1 d D U . . .
F4 F 0.3743(3) 0.3807(6) 0.1963(3) 0.084(3) Uani 1 1 d D U . . .
F5 F 0.3956(5) 0.3473(8) 0.2769(4) 0.144(5) Uani 1 1 d D U . . .
F6 F 0.4447(4) 0.3045(7) 0.2297(4) 0.124(4) Uani 1 1 d D U . . .
F7 F 0.6877(3) 0.7040(6) 0.2988(3) 0.072(2) Uani 1 1 d D U . . .
F8 F 0.7546(3) 0.6210(6) 0.3387(4) 0.092(3) Uani 1 1 d D U . . .
F9 F 0.7199(3) 0.7151(6) 0.3810(3) 0.086(3) Uani 1 1 d D U . . .
F10 F 0.6850(5) 0.2882(7) 0.3600(4) 0.118(4) Uani 1 1 d D U . . .
F11 F 0.7286(4) 0.3525(7) 0.4278(6) 0.165(6) Uani 1 1 d D U . . .
F12 F 0.6506(4) 0.2936(6) 0.4208(4) 0.096(3) Uani 1 1 d D U . . .
F13 F 0.5040(9) 0.2777(12) 0.4334(7) 0.080(7) Uiso 0.5 1 d D U P A 2
F14 F 0.4772(9) 0.3592(14) 0.4929(9) 0.110(7) Uiso 0.5 1 d D U P A 2
F15 F 0.5508(7) 0.2939(11) 0.5132(6) 0.068(4) Uiso 0.5 1 d D U P A 2
F16 F 0.6885(8) 0.6380(14) 0.5040(7) 0.097(6) Uiso 0.5 1 d D U P B 1
F17 F 0.6456(7) 0.6097(12) 0.5643(6) 0.072(4) Uiso 0.5 1 d D U P B 1
F18 F 0.6973(7) 0.5128(11) 0.5468(7) 0.077(5) Uiso 0.5 1 d D U P B 1
O1 O 0.4107(3) 0.9660(6) 0.3852(3) 0.053(2) Uani 1 1 d . U . . .
O2 O 0.3289(3) 0.8544(6) 0.3703(3) 0.054(2) Uani 1 1 d . U . . .
O3 O 0.5071(3) 0.6267(6) 0.2752(3) 0.059(2) Uani 1 1 d . U . . .
O4 O 0.4870(4) 0.4523(6) 0.2997(3) 0.060(2) Uani 1 1 d . U . . .
O5 O 0.6185(3) 0.6125(6) 0.3390(3) 0.058(2) Uani 1 1 d . U . . .
O6 O 0.6007(4) 0.4344(6) 0.3650(3) 0.058(2) Uani 1 1 d . U . . .
O7 O 0.5164(3) 0.4560(6) 0.4123(3) 0.055(2) Uani 1 1 d . U . . .
O8 O 0.6012(3) 0.5811(6) 0.4391(3) 0.057(2) Uani 1 1 d . U . . .
N1 N 0.5332(4) 0.7186(7) 0.3778(4) 0.052(3) Uiso 1 1 d . U . . .
N2 N 0.4471(4) 0.6020(8) 0.3595(4) 0.055(3) Uiso 1 1 d . U . . .
C1 C 0.5761(5) 0.7759(9) 0.3897(5) 0.054(3) Uani 1 1 d . U . . .
H1 H 0.611529 0.751406 0.393090 0.064 Uiso 1 1 calc R . . . .
C2 C 0.5723(5) 0.8667(9) 0.3971(5) 0.052(3) Uani 1 1 d . U . . .
H2 H 0.604183 0.903921 0.405501 0.062 Uiso 1 1 calc R . . . .
C3 C 0.5198(5) 0.9047(10) 0.3921(5) 0.056(3) Uani 1 1 d . U . . .
H3 H 0.515860 0.968204 0.396269 0.068 Uiso 1 1 calc R . . . .
C4 C 0.4739(5) 0.8473(9) 0.3810(5) 0.050(3) Uani 1 1 d . U . . .
C5 C 0.4211(5) 0.8784(9) 0.3785(5) 0.049(3) Uani 1 1 d . U . . .
C6 C 0.3776(5) 0.8183(9) 0.3704(4) 0.046(3) Uani 1 1 d . U . . .
C7 C 0.3852(5) 0.7251(9) 0.3627(5) 0.046(3) Uani 1 1 d . U . . .
C8 C 0.3420(5) 0.6602(9) 0.3556(5) 0.051(3) Uani 1 1 d . U . . .
H8 H 0.305782 0.679969 0.353169 0.061 Uiso 1 1 calc R . . . .
C9 C 0.3523(5) 0.5721(10) 0.3523(5) 0.056(3) Uani 1 1 d . U . . .
H9 H 0.323736 0.528787 0.348883 0.067 Uiso 1 1 calc R . . . .
C10 C 0.4074(5) 0.5427(10) 0.3541(5) 0.056(3) Uani 1 1 d . U . . .
H10 H 0.414756 0.479973 0.351393 0.067 Uiso 1 1 calc R . . . .
C11 C 0.4373(5) 0.6919(9) 0.3645(5) 0.048(3) Uani 1 1 d . U . . .
C12 C 0.4820(5) 0.7549(9) 0.3740(5) 0.045(3) Uani 1 1 d . U . . .
C13 C 0.4573(6) 0.6835(11) 0.1914(6) 0.087(4) Uani 1 1 d D U . . .
C14 C 0.4704(5) 0.6077(11) 0.2325(6) 0.064(3) Uani 1 1 d . U . . .
C15 C 0.4405(6) 0.5281(11) 0.2221(6) 0.064(3) Uani 1 1 d . U . . .
H15 H 0.411489 0.523068 0.190437 0.077 Uiso 1 1 calc R . . . .
C16 C 0.4513(5) 0.4561(10) 0.2560(5) 0.058(3) Uani 1 1 d . U . . .
C17 C 0.4155(5) 0.3729(9) 0.2400(5) 0.069(3) Uani 1 1 d D U . . .
C18 C 0.7071(5) 0.6564(9) 0.3419(5) 0.064(3) Uani 1 1 d D U . . .
C19 C 0.6676(5) 0.5827(9) 0.3506(5) 0.052(3) Uani 1 1 d . U . . .
C20 C 0.6858(5) 0.4993(9) 0.3672(5) 0.054(3) Uani 1 1 d . U . . .
H20 H 0.723881 0.486833 0.373366 0.064 Uiso 1 1 calc R . . . .
C21 C 0.6539(5) 0.4328(9) 0.3755(5) 0.053(3) Uani 1 1 d . U . . .
C22 C 0.6785(5) 0.3437(10) 0.3967(5) 0.071(3) Uani 1 1 d D U . . .
C23 C 0.5159(5) 0.3415(10) 0.4706(5) 0.072(4) Uani 1 1 d D U . . .
C24 C 0.5422(6) 0.4266(10) 0.4562(6) 0.058(3) Uani 1 1 d . U . . .
C25 C 0.5883(6) 0.4618(11) 0.4921(5) 0.073(4) Uani 1 1 d . U . . .
H25 H 0.603257 0.432129 0.524713 0.087 Uiso 1 1 calc R . . . .
C26 C 0.6120(5) 0.5378(10) 0.4811(5) 0.057(3) Uani 1 1 d . U . . .
C27 C 0.6620(5) 0.5796(10) 0.5239(5) 0.081(5) Uani 1 1 d D U . . .
C28 C 0.3093(6) 1.0896(11) 0.4325(5) 0.063(3) Uani 1 1 d . U . . .
H28 H 0.294467 1.147294 0.419968 0.076 Uiso 1 1 calc R . . . .
C29 C 0.3653(5) 1.0691(9) 0.4531(5) 0.055(3) Uani 1 1 d . U . . .
C30 C 0.3681(5) 0.9778(9) 0.4690(5) 0.054(3) Uani 1 1 d . U . . .
C31 C 0.3169(6) 0.9384(10) 0.4563(5) 0.058(3) Uani 1 1 d . U . . .
C32 C 0.2785(5) 1.0090(10) 0.4335(5) 0.058(3) Uani 1 1 d . U . . .
C33 C 0.2680(5) 1.0740(11) 0.3205(5) 0.065(3) Uani 1 1 d . U . . .
H33 H 0.241972 1.106753 0.332845 0.077 Uiso 1 1 calc R . . . .
C34 C 0.3185(6) 1.1085(11) 0.3199(5) 0.065(3) Uani 1 1 d . U . . .
C35 C 0.3421(6) 1.0402(11) 0.2960(5) 0.065(3) Uani 1 1 d . U . . .
C36 C 0.3074(6) 0.9649(11) 0.2850(5) 0.064(3) Uani 1 1 d . U . . .
C37 C 0.2598(6) 0.9862(12) 0.3011(6) 0.068(3) Uani 1 1 d . U . . .
C38 C 0.4118(6) 1.1374(9) 0.4591(6) 0.067(4) Uani 1 1 d . U . . .
H38A H 0.437344 1.115055 0.440664 0.100 Uiso 1 1 calc GR . . . .
H38B H 0.431379 1.145108 0.496269 0.100 Uiso 1 1 calc GR . . . .
H38C H 0.396477 1.195833 0.444258 0.100 Uiso 1 1 calc GR . . . .
C39 C 0.4226(6) 0.9274(11) 0.4955(6) 0.077(5) Uani 1 1 d . U . . .
H39A H 0.421080 0.866120 0.480814 0.115 Uiso 1 1 calc GR . . . .
H39B H 0.427711 0.923309 0.533176 0.115 Uiso 1 1 calc GR . . . .
H39C H 0.453399 0.960779 0.489190 0.115 Uiso 1 1 calc GR . . . .
C40 C 0.3051(6) 0.8433(9) 0.4678(5) 0.064(4) Uani 1 1 d . U . . .
H40A H 0.266339 0.829563 0.450271 0.096 Uiso 1 1 calc GR . . . .
H40B H 0.312452 0.835629 0.505601 0.096 Uiso 1 1 calc GR . . . .
H40C H 0.328534 0.802029 0.455047 0.096 Uiso 1 1 calc GR . . . .
C41 C 0.2160(6) 1.0027(11) 0.4206(6) 0.080(5) Uani 1 1 d . U . . .
H41A H 0.198841 1.039985 0.389808 0.120 Uiso 1 1 calc GR . . . .
H41B H 0.204455 1.024685 0.450389 0.120 Uiso 1 1 calc GR . . . .
H41C H 0.204444 0.939344 0.413341 0.120 Uiso 1 1 calc GR . . . .
C42 C 0.3399(7) 1.2036(11) 0.3326(6) 0.076(4) Uani 1 1 d . U . . .
H42A H 0.318218 1.234622 0.352329 0.114 Uiso 1 1 calc GR . . . .
H42B H 0.336793 1.236701 0.300065 0.114 Uiso 1 1 calc GR . . . .
H42C H 0.378538 1.201331 0.353583 0.114 Uiso 1 1 calc GR . . . .
C43 C 0.3975(6) 1.0484(12) 0.2850(6) 0.089(5) Uani 1 1 d . U . . .
H43A H 0.425674 1.066222 0.317114 0.134 Uiso 1 1 calc GR . . . .
H43B H 0.395052 1.094391 0.257992 0.134 Uiso 1 1 calc GR . . . .
H43C H 0.407331 0.989720 0.272950 0.134 Uiso 1 1 calc GR . . . .
C44 C 0.3134(6) 0.8804(11) 0.2574(6) 0.079(4) Uani 1 1 d . U . . .
H44A H 0.352255 0.871129 0.259751 0.119 Uiso 1 1 calc GR . . . .
H44B H 0.291831 0.885153 0.220586 0.119 Uiso 1 1 calc GR . . . .
H44C H 0.300130 0.828861 0.273510 0.119 Uiso 1 1 calc GR . . . .
C45 C 0.2117(6) 0.9254(11) 0.2955(6) 0.074(4) Uani 1 1 d . U . . .
H45A H 0.224674 0.864087 0.307015 0.110 Uiso 1 1 calc GR . . . .
H45B H 0.189585 0.923652 0.258741 0.110 Uiso 1 1 calc GR . . . .
H45C H 0.189277 0.948433 0.316923 0.110 Uiso 1 1 calc GR . . . .
F13A F 0.5249(9) 0.2678(12) 0.4475(8) 0.080(7) Uiso 0.5 1 d D U P A 1
F14A F 0.4595(6) 0.3473(11) 0.4550(7) 0.077(5) Uiso 0.5 1 d D U P A 1
F15A F 0.5217(11) 0.3289(16) 0.5198(7) 0.112(7) Uiso 0.5 1 d D U P A 1
F16A F 0.6626(8) 0.6708(11) 0.5212(7) 0.081(5) Uiso 0.5 1 d D U P B 2
F17A F 0.6654(12) 0.5448(18) 0.5697(8) 0.134(8) Uiso 0.5 1 d D U P B 2
F18A F 0.7076(8) 0.5580(16) 0.5112(8) 0.112(7) Uiso 0.5 1 d D U P B 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Y1 0.0316(7) 0.0685(9) 0.0554(8) 0.0019(6) 0.0199(5) 0.0029(6)
V1 0.0353(13) 0.0743(18) 0.0573(15) 0.0059(12) 0.0239(11) 0.0075(12)
F1 0.117(8) 0.110(7) 0.128(8) 0.038(6) 0.033(6) 0.047(6)
F2 0.125(9) 0.149(10) 0.097(7) 0.027(6) -0.026(6) -0.021(7)
F3 0.120(7) 0.150(10) 0.079(6) 0.017(6) 0.033(5) -0.027(7)
F4 0.050(5) 0.115(7) 0.081(5) -0.005(5) 0.009(4) -0.016(4)
F5 0.180(11) 0.173(11) 0.084(6) -0.025(6) 0.047(6) -0.120(9)
F6 0.106(8) 0.105(7) 0.128(8) -0.036(6) -0.018(6) 0.031(6)
F7 0.041(4) 0.099(6) 0.080(5) 0.024(4) 0.024(4) -0.006(4)
F8 0.032(4) 0.098(7) 0.157(8) 0.034(5) 0.041(5) 0.006(4)
F9 0.071(6) 0.110(7) 0.082(5) -0.021(5) 0.031(4) -0.037(5)
F10 0.162(10) 0.089(7) 0.138(8) 0.018(5) 0.099(7) 0.044(7)
F11 0.087(7) 0.097(8) 0.244(13) 0.043(8) -0.056(8) -0.005(6)
F12 0.092(6) 0.106(7) 0.105(7) 0.047(5) 0.054(5) 0.034(5)
O1 0.034(4) 0.064(5) 0.066(5) -0.002(4) 0.022(4) 0.002(4)
O2 0.027(4) 0.089(6) 0.054(5) -0.001(4) 0.022(4) 0.003(4)
O3 0.039(5) 0.077(6) 0.064(5) 0.016(4) 0.021(4) 0.006(4)
O4 0.049(5) 0.077(6) 0.053(5) -0.003(4) 0.014(4) 0.002(4)
O5 0.041(4) 0.083(6) 0.060(5) 0.011(5) 0.028(4) 0.015(4)
O6 0.045(4) 0.074(6) 0.062(5) 0.000(4) 0.025(4) 0.001(4)
O7 0.038(5) 0.070(6) 0.061(5) -0.001(4) 0.023(4) 0.005(4)
O8 0.039(5) 0.077(6) 0.057(5) 0.001(4) 0.019(4) -0.004(4)
C1 0.041(8) 0.063(7) 0.061(8) -0.006(7) 0.021(7) 0.004(6)
C2 0.028(5) 0.063(7) 0.075(9) -0.011(7) 0.031(6) -0.017(5)
C3 0.034(5) 0.073(8) 0.067(8) -0.015(7) 0.022(6) -0.001(5)
C4 0.033(5) 0.066(6) 0.055(7) -0.004(6) 0.018(6) -0.001(5)
C5 0.034(5) 0.060(6) 0.055(7) -0.001(6) 0.015(6) -0.004(4)
C6 0.029(5) 0.067(6) 0.048(7) 0.000(6) 0.022(5) -0.002(4)
C7 0.028(5) 0.065(6) 0.051(7) 0.005(6) 0.020(5) -0.004(4)
C8 0.034(6) 0.068(6) 0.051(8) -0.004(7) 0.013(6) -0.011(5)
C9 0.039(6) 0.071(7) 0.061(8) -0.009(7) 0.018(6) -0.008(6)
C10 0.045(7) 0.067(9) 0.056(8) -0.010(7) 0.017(6) -0.012(6)
C11 0.027(5) 0.068(8) 0.057(8) 0.002(6) 0.022(6) -0.003(4)
C12 0.025(5) 0.062(6) 0.050(7) 0.006(6) 0.016(5) 0.000(5)
C13 0.074(7) 0.091(7) 0.084(7) 0.009(5) 0.005(5) -0.010(6)
C14 0.031(7) 0.090(8) 0.073(7) 0.012(6) 0.017(5) -0.001(6)
C15 0.043(8) 0.090(8) 0.063(8) 0.008(6) 0.022(6) -0.003(6)
C16 0.044(7) 0.082(7) 0.052(6) -0.009(5) 0.020(5) -0.003(6)
C17 0.067(7) 0.067(6) 0.065(6) 0.002(5) 0.008(4) -0.001(5)
C18 0.048(5) 0.075(7) 0.069(6) 0.001(4) 0.018(5) 0.002(5)
C19 0.037(5) 0.071(7) 0.047(7) -0.001(6) 0.013(6) 0.006(5)
C20 0.033(6) 0.070(7) 0.062(8) -0.002(6) 0.021(6) 0.009(5)
C21 0.043(5) 0.067(6) 0.051(7) -0.007(6) 0.019(6) 0.003(5)
C22 0.055(6) 0.074(6) 0.083(7) 0.006(5) 0.020(5) 0.001(5)
C23 0.074(10) 0.093(11) 0.060(10) 0.007(8) 0.036(8) -0.003(8)
C24 0.048(7) 0.075(9) 0.062(7) 0.006(6) 0.032(5) 0.008(6)
C25 0.062(9) 0.104(11) 0.051(8) 0.021(7) 0.014(6) 0.000(7)
C26 0.034(7) 0.088(9) 0.054(7) 0.003(6) 0.023(5) 0.014(5)
C27 0.051(9) 0.131(15) 0.057(8) 0.047(9) 0.008(6) -0.011(8)
C28 0.053(6) 0.078(7) 0.069(7) 0.005(6) 0.033(6) 0.010(5)
C29 0.052(6) 0.063(7) 0.058(7) -0.010(6) 0.027(5) 0.000(5)
C30 0.048(5) 0.067(7) 0.055(7) -0.008(6) 0.026(5) 0.006(5)
C31 0.048(6) 0.076(7) 0.054(7) -0.002(6) 0.020(6) -0.001(5)
C32 0.039(5) 0.083(8) 0.058(7) -0.002(6) 0.026(6) 0.008(5)
C33 0.039(6) 0.101(8) 0.061(7) 0.014(6) 0.025(6) 0.020(6)
C34 0.051(7) 0.088(7) 0.063(8) 0.016(6) 0.029(6) 0.011(6)
C35 0.042(6) 0.101(8) 0.056(7) 0.010(6) 0.022(6) 0.013(5)
C36 0.047(7) 0.099(8) 0.049(6) 0.012(6) 0.018(6) 0.014(6)
C37 0.044(6) 0.101(9) 0.062(7) 0.011(7) 0.023(6) 0.013(5)
C38 0.062(8) 0.068(9) 0.074(10) -0.020(7) 0.026(8) -0.007(6)
C39 0.054(8) 0.114(13) 0.061(9) -0.001(8) 0.016(7) 0.020(8)
C40 0.056(9) 0.076(8) 0.067(9) -0.010(7) 0.028(7) -0.012(7)
C41 0.044(6) 0.110(14) 0.093(12) 0.025(10) 0.029(8) 0.011(7)
C42 0.075(10) 0.095(9) 0.065(10) 0.016(8) 0.033(8) 0.005(8)
C43 0.060(9) 0.138(16) 0.091(12) 0.021(10) 0.054(9) 0.007(9)
C44 0.073(11) 0.104(10) 0.066(10) 0.006(7) 0.028(8) 0.022(9)
C45 0.045(7) 0.106(11) 0.067(9) 0.006(8) 0.013(7) 0.009(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
Y1 O3 2.326(8) . ?
Y1 O4 2.297(9) . ?
Y1 O5 2.318(9) . ?
Y1 O6 2.331(9) . ?
Y1 O7 2.310(9) . ?
Y1 O8 2.334(9) . ?
Y1 N1 2.476(10) . ?
Y1 N2 2.488(11) . ?
V1 O1 1.975(8) . ?
V1 O2 1.977(9) . ?
V1 C28 2.291(14) . ?
V1 C29 2.294(13) . ?
V1 C30 2.362(13) . ?
V1 C31 2.372(13) . ?
V1 C32 2.322(13) . ?
V1 C33 2.261(13) . ?
V1 C34 2.304(14) . ?
V1 C35 2.388(14) . ?
V1 C36 2.385(13) . ?
V1 C37 2.310(14) . ?
F1 C13 1.308(14) . ?
F2 C13 1.323(14) . ?
F3 C13 1.301(14) . ?
F4 C17 1.328(12) . ?
F5 C17 1.290(13) . ?
F6 C17 1.325(13) . ?
F7 C18 1.316(12) . ?
F8 C18 1.340(12) . ?
F9 C18 1.323(13) . ?
F10 C22 1.324(13) . ?
F11 C22 1.308(13) . ?
F12 C22 1.313(13) . ?
F13 C23 1.338(16) . ?
F14 C23 1.315(16) . ?
F15 C23 1.410(15) . ?
F16 C27 1.299(16) . ?
F17 C27 1.342(15) . ?
F18 C27 1.353(15) . ?
O1 C5 1.340(15) . ?
O2 C6 1.346(14) . ?
O3 C14 1.278(16) . ?
O4 C16 1.256(15) . ?
O5 C19 1.274(15) . ?
O6 C21 1.298(15) . ?
O7 C24 1.242(15) . ?
O8 C26 1.249(15) . ?
N1 C1 1.341(16) . ?
N1 C12 1.384(15) . ?
N2 C10 1.309(16) . ?
N2 C11 1.360(16) . ?
C1 H1 0.9500 . ?
C1 C2 1.359(17) . ?
C2 H2 0.9500 . ?
C2 C3 1.415(17) . ?
C3 H3 0.9500 . ?
C3 C4 1.402(18) . ?
C4 C5 1.401(17) . ?
C4 C12 1.397(17) . ?
C5 C6 1.383(17) . ?
C6 C7 1.409(17) . ?
C7 C8 1.424(17) . ?
C7 C11 1.400(16) . ?
C8 H8 0.9500 . ?
C8 C9 1.331(17) . ?
C9 H9 0.9500 . ?
C9 C10 1.455(18) . ?
C10 H10 0.9500 . ?
C11 C12 1.430(17) . ?
C13 C14 1.53(2) . ?
C14 C15 1.38(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.368(19) . ?
C16 C17 1.511(19) . ?
C18 C19 1.542(19) . ?
C19 C20 1.342(17) . ?
C20 H20 0.9500 . ?
C20 C21 1.331(18) . ?
C21 C22 1.494(19) . ?
C23 C24 1.522(19) . ?
C23 F13A 1.303(16) . ?
C23 F14A 1.372(16) . ?
C23 F15A 1.292(16) . ?
C24 C25 1.38(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.345(19) . ?
C26 C27 1.567(19) . ?
C27 F16A 1.344(15) . ?
C27 F17A 1.309(17) . ?
C27 F18A 1.336(17) . ?
C28 H28 0.9500 . ?
C28 C29 1.399(19) . ?
C28 C32 1.43(2) . ?
C29 C30 1.405(18) . ?
C29 C38 1.525(18) . ?
C30 C31 1.374(18) . ?
C30 C39 1.548(19) . ?
C31 C32 1.435(19) . ?
C31 C40 1.483(18) . ?
C32 C41 1.529(18) . ?
C33 H33 0.9500 . ?
C33 C34 1.386(19) . ?
C33 C37 1.39(2) . ?
C34 C35 1.41(2) . ?
C34 C42 1.50(2) . ?
C35 C36 1.40(2) . ?
C35 C43 1.52(2) . ?
C36 C37 1.434(19) . ?
C36 C44 1.477(19) . ?
C37 C45 1.49(2) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 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
O3 Y1 O6 119.1(3) . . ?
O3 Y1 O8 140.9(3) . . ?
O3 Y1 N1 75.9(3) . . ?
O3 Y1 N2 79.7(3) . . ?
O4 Y1 O3 72.6(3) . . ?
O4 Y1 O5 118.9(3) . . ?
O4 Y1 O6 78.3(3) . . ?
O4 Y1 O7 77.5(3) . . ?
O4 Y1 O8 146.1(3) . . ?
O4 Y1 N1 136.8(3) . . ?
O4 Y1 N2 79.5(3) . . ?
O5 Y1 O3 75.9(3) . . ?
O5 Y1 O6 73.6(3) . . ?
O5 Y1 O8 76.3(3) . . ?
O5 Y1 N1 80.0(3) . . ?
O5 Y1 N2 142.2(3) . . ?
O6 Y1 O8 77.8(3) . . ?
O6 Y1 N1 144.2(3) . . ?
O6 Y1 N2 144.2(3) . . ?
O7 Y1 O3 142.9(3) . . ?
O7 Y1 O5 139.3(3) . . ?
O7 Y1 O6 74.4(3) . . ?
O7 Y1 O8 73.1(3) . . ?
O7 Y1 N1 114.6(3) . . ?
O7 Y1 N2 73.6(3) . . ?
O8 Y1 N1 72.6(3) . . ?
O8 Y1 N2 107.4(3) . . ?
N1 Y1 N2 66.2(4) . . ?
O1 V1 O2 81.8(3) . . ?
O1 V1 C28 118.3(4) . . ?
O1 V1 C29 83.6(4) . . ?
O1 V1 C30 78.6(4) . . ?
O1 V1 C31 105.9(4) . . ?
O1 V1 C32 135.7(4) . . ?
O1 V1 C33 132.3(4) . . ?
O1 V1 C34 98.5(4) . . ?
O1 V1 C35 77.1(4) . . ?
O1 V1 C36 92.3(4) . . ?
O1 V1 C37 127.8(4) . . ?
O2 V1 C28 134.5(5) . . ?
O2 V1 C29 126.6(4) . . ?
O2 V1 C30 91.5(4) . . ?
O2 V1 C31 76.4(4) . . ?
O2 V1 C32 100.3(4) . . ?
O2 V1 C33 119.6(5) . . ?
O2 V1 C34 135.3(5) . . ?
O2 V1 C35 104.3(5) . . ?
O2 V1 C36 76.6(5) . . ?
O2 V1 C37 84.6(5) . . ?
C28 V1 C29 35.5(5) . . ?
C28 V1 C30 57.7(5) . . ?
C28 V1 C31 59.3(5) . . ?
C28 V1 C32 36.0(5) . . ?
C28 V1 C34 84.8(5) . . ?
C28 V1 C35 119.4(5) . . ?
C28 V1 C36 136.2(5) . . ?
C28 V1 C37 107.0(5) . . ?
C29 V1 C30 35.1(4) . . ?
C29 V1 C31 59.0(5) . . ?
C29 V1 C32 59.5(5) . . ?
C29 V1 C34 97.6(5) . . ?
C29 V1 C35 121.8(5) . . ?
C29 V1 C36 155.1(5) . . ?
C29 V1 C37 141.2(5) . . ?
C30 V1 C31 33.7(4) . . ?
C30 V1 C35 148.6(5) . . ?
C30 V1 C36 166.1(5) . . ?
C31 V1 C35 177.0(5) . . ?
C31 V1 C36 144.7(5) . . ?
C32 V1 C30 57.3(4) . . ?
C32 V1 C31 35.6(5) . . ?
C32 V1 C35 141.7(5) . . ?
C32 V1 C36 131.5(5) . . ?
C33 V1 C28 78.5(5) . . ?
C33 V1 C29 108.0(5) . . ?
C33 V1 C30 135.9(5) . . ?
C33 V1 C31 120.0(5) . . ?
C33 V1 C32 85.3(5) . . ?
C33 V1 C34 35.3(5) . . ?
C33 V1 C35 57.1(5) . . ?
C33 V1 C36 57.8(5) . . ?
C33 V1 C37 35.3(5) . . ?
C34 V1 C30 132.7(5) . . ?
C34 V1 C31 143.1(5) . . ?
C34 V1 C32 109.1(5) . . ?
C34 V1 C35 35.0(5) . . ?
C34 V1 C36 58.6(5) . . ?
C34 V1 C37 59.8(6) . . ?
C36 V1 C35 34.0(5) . . ?
C37 V1 C30 152.1(5) . . ?
C37 V1 C31 119.3(5) . . ?
C37 V1 C32 96.2(5) . . ?
C37 V1 C35 58.1(5) . . ?
C37 V1 C36 35.5(5) . . ?
C5 O1 V1 112.1(7) . . ?
C6 O2 V1 112.4(8) . . ?
C14 O3 Y1 135.0(9) . . ?
C16 O4 Y1 135.3(9) . . ?
C19 O5 Y1 131.7(8) . . ?
C21 O6 Y1 130.5(8) . . ?
C24 O7 Y1 132.1(9) . . ?
C26 O8 Y1 133.3(9) . . ?
C1 N1 Y1 123.6(9) . . ?
C1 N1 C12 117.2(11) . . ?
C12 N1 Y1 119.1(8) . . ?
C10 N2 Y1 121.7(9) . . ?
C10 N2 C11 120.2(12) . . ?
C11 N2 Y1 118.0(8) . . ?
N1 C1 H1 117.8 . . ?
N1 C1 C2 124.5(12) . . ?
C2 C1 H1 117.8 . . ?
C1 C2 H2 120.6 . . ?
C1 C2 C3 118.7(11) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 H3 120.5 . . ?
C4 C3 C2 119.0(13) . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 122.7(13) . . ?
C12 C4 C3 118.1(11) . . ?
C12 C4 C5 119.2(12) . . ?
O1 C5 C4 122.1(11) . . ?
O1 C5 C6 117.2(11) . . ?
C6 C5 C4 120.6(13) . . ?
O2 C6 C5 116.1(12) . . ?
O2 C6 C7 123.3(11) . . ?
C5 C6 C7 120.6(11) . . ?
C6 C7 C8 122.7(11) . . ?
C11 C7 C6 120.2(11) . . ?
C11 C7 C8 117.0(12) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 C7 120.4(12) . . ?
C9 C8 H8 119.8 . . ?
C8 C9 H9 120.2 . . ?
C8 C9 C10 119.5(13) . . ?
C10 C9 H9 120.2 . . ?
N2 C10 C9 120.6(13) . . ?
N2 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
N2 C11 C7 122.3(11) . . ?
N2 C11 C12 119.4(11) . . ?
C7 C11 C12 118.2(12) . . ?
N1 C12 C4 122.6(11) . . ?
N1 C12 C11 116.3(11) . . ?
C4 C12 C11 121.1(11) . . ?
F1 C13 F2 110.8(14) . . ?
F1 C13 C14 109.4(13) . . ?
F2 C13 C14 112.7(13) . . ?
F3 C13 F1 107.7(14) . . ?
F3 C13 F2 105.3(13) . . ?
F3 C13 C14 110.8(13) . . ?
O3 C14 C13 115.5(13) . . ?
O3 C14 C15 125.6(13) . . ?
C15 C14 C13 118.8(13) . . ?
C14 C15 H15 118.9 . . ?
C16 C15 C14 122.1(14) . . ?
C16 C15 H15 118.9 . . ?
O4 C16 C15 127.0(14) . . ?
O4 C16 C17 116.0(12) . . ?
C15 C16 C17 116.9(12) . . ?
F4 C17 C16 115.7(11) . . ?
F5 C17 F4 108.4(12) . . ?
F5 C17 F6 107.7(13) . . ?
F5 C17 C16 111.0(11) . . ?
F6 C17 F4 103.2(10) . . ?
F6 C17 C16 110.4(12) . . ?
F7 C18 F8 105.5(10) . . ?
F7 C18 F9 106.7(11) . . ?
F7 C18 C19 114.4(10) . . ?
F8 C18 C19 111.9(11) . . ?
F9 C18 F8 106.6(11) . . ?
F9 C18 C19 111.2(10) . . ?
O5 C19 C18 110.8(11) . . ?
O5 C19 C20 127.9(13) . . ?
C20 C19 C18 121.2(12) . . ?
C19 C20 H20 118.0 . . ?
C21 C20 C19 124.1(13) . . ?
C21 C20 H20 118.0 . . ?
O6 C21 C20 126.7(13) . . ?
O6 C21 C22 113.1(12) . . ?
C20 C21 C22 120.1(12) . . ?
F10 C22 C21 112.9(12) . . ?
F11 C22 F10 103.0(14) . . ?
F11 C22 F12 107.9(13) . . ?
F11 C22 C21 112.1(12) . . ?
F12 C22 F10 102.7(11) . . ?
F12 C22 C21 117.0(12) . . ?
F13 C23 F15 101.7(16) . . ?
F13 C23 C24 114.2(13) . . ?
F14 C23 F13 116.0(17) . . ?
F14 C23 F15 96.3(14) . . ?
F14 C23 C24 113.2(14) . . ?
F15 C23 C24 113.3(12) . . ?
F13A C23 C24 114.5(14) . . ?
F13A C23 F14A 102.6(16) . . ?
F14A C23 C24 111.5(13) . . ?
F15A C23 C24 116.6(15) . . ?
F15A C23 F13A 112.3(18) . . ?
F15A C23 F14A 96.9(16) . . ?
O7 C24 C23 112.2(12) . . ?
O7 C24 C25 129.3(14) . . ?
C25 C24 C23 118.5(13) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 C24 120.2(13) . . ?
C26 C25 H25 119.9 . . ?
O8 C26 C25 128.7(14) . . ?
O8 C26 C27 112.1(12) . . ?
C25 C26 C27 119.2(12) . . ?
F16 C27 F17 115.6(17) . . ?
F16 C27 F18 108.2(15) . . ?
F16 C27 C26 111.6(13) . . ?
F17 C27 F18 101.4(13) . . ?
F17 C27 C26 110.0(12) . . ?
F18 C27 C26 109.5(14) . . ?
F16A C27 C26 111.9(12) . . ?
F17A C27 C26 110.5(16) . . ?
F17A C27 F16A 116.3(18) . . ?
F17A C27 F18A 108.5(18) . . ?
F18A C27 C26 107.4(14) . . ?
F18A C27 F16A 101.5(15) . . ?
V1 C28 H28 120.4 . . ?
C29 C28 V1 72.3(8) . . ?
C29 C28 H28 125.9 . . ?
C29 C28 C32 108.2(13) . . ?
C32 C28 V1 73.2(8) . . ?
C32 C28 H28 125.9 . . ?
C28 C29 V1 72.1(8) . . ?
C28 C29 C30 106.5(12) . . ?
C28 C29 C38 124.5(13) . . ?
C30 C29 V1 75.1(7) . . ?
C30 C29 C38 128.9(13) . . ?
C38 C29 V1 120.8(9) . . ?
C29 C30 V1 69.8(7) . . ?
C29 C30 C39 123.9(13) . . ?
C31 C30 V1 73.5(8) . . ?
C31 C30 C29 111.5(12) . . ?
C31 C30 C39 124.5(13) . . ?
C39 C30 V1 122.1(9) . . ?
C30 C31 V1 72.7(8) . . ?
C30 C31 C32 106.1(13) . . ?
C30 C31 C40 125.7(13) . . ?
C32 C31 V1 70.3(7) . . ?
C32 C31 C40 128.2(13) . . ?
C40 C31 V1 124.8(9) . . ?
C28 C32 V1 70.8(7) . . ?
C28 C32 C31 107.6(12) . . ?
C28 C32 C41 125.9(13) . . ?
C31 C32 V1 74.1(7) . . ?
C31 C32 C41 125.8(13) . . ?
C41 C32 V1 127.7(9) . . ?
V1 C33 H33 119.3 . . ?
C34 C33 V1 74.0(8) . . ?
C34 C33 H33 124.0 . . ?
C34 C33 C37 112.0(13) . . ?
C37 C33 V1 74.3(8) . . ?
C37 C33 H33 124.0 . . ?
C33 C34 V1 70.6(8) . . ?
C33 C34 C35 105.2(14) . . ?
C33 C34 C42 127.8(14) . . ?
C35 C34 V1 75.7(9) . . ?
C35 C34 C42 126.2(14) . . ?
C42 C34 V1 126.4(10) . . ?
C34 C35 V1 69.2(8) . . ?
C34 C35 C43 124.6(15) . . ?
C36 C35 V1 72.9(8) . . ?
C36 C35 C34 109.6(13) . . ?
C36 C35 C43 125.8(15) . . ?
C43 C35 V1 123.5(10) . . ?
C35 C36 V1 73.1(8) . . ?
C35 C36 C37 107.4(14) . . ?
C35 C36 C44 128.7(14) . . ?
C37 C36 V1 69.4(8) . . ?
C37 C36 C44 123.6(15) . . ?
C44 C36 V1 127.1(10) . . ?
C33 C37 V1 70.4(8) . . ?
C33 C37 C36 105.6(14) . . ?
C33 C37 C45 129.0(13) . . ?
C36 C37 V1 75.1(8) . . ?
C36 C37 C45 125.3(15) . . ?
C45 C37 V1 121.0(10) . . ?
C29 C38 H38A 109.5 . . ?
C29 C38 H38B 109.5 . . ?
C29 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C30 C39 H39A 109.5 . . ?
C30 C39 H39B 109.5 . . ?
C30 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C31 C40 H40A 109.5 . . ?
C31 C40 H40B 109.5 . . ?
C31 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C32 C41 H41A 109.5 . . ?
C32 C41 H41B 109.5 . . ?
C32 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C34 C42 H42A 109.5 . . ?
C34 C42 H42B 109.5 . . ?
C34 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C35 C43 H43A 109.5 . . ?
C35 C43 H43B 109.5 . . ?
C35 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C36 C44 H44A 109.5 . . ?
C36 C44 H44B 109.5 . . ?
C36 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C37 C45 H45A 109.5 . . ?
C37 C45 H45B 109.5 . . ?
C37 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
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
Y1 O3 C14 C13 171.4(9) . . . . ?
Y1 O3 C14 C15 -5(2) . . . . ?
Y1 O4 C16 C15 15(2) . . . . ?
Y1 O4 C16 C17 -163.5(9) . . . . ?
Y1 O5 C19 C18 -166.2(7) . . . . ?
Y1 O5 C19 C20 15(2) . . . . ?
Y1 O6 C21 C20 -24.3(19) . . . . ?
Y1 O6 C21 C22 158.8(8) . . . . ?
Y1 O7 C24 C23 -162.9(8) . . . . ?
Y1 O7 C24 C25 19(2) . . . . ?
Y1 O8 C26 C25 -4(2) . . . . ?
Y1 O8 C26 C27 173.3(8) . . . . ?
Y1 N1 C1 C2 173.9(10) . . . . ?
Y1 N1 C12 C4 -174.2(9) . . . . ?
Y1 N1 C12 C11 8.2(14) . . . . ?
Y1 N2 C10 C9 -175.5(9) . . . . ?
Y1 N2 C11 C7 175.0(9) . . . . ?
Y1 N2 C11 C12 -7.4(14) . . . . ?
V1 O1 C5 C4 178.3(9) . . . . ?
V1 O1 C5 C6 -3.7(13) . . . . ?
V1 O2 C6 C5 3.8(13) . . . . ?
V1 O2 C6 C7 -175.9(9) . . . . ?
V1 C28 C29 C30 -67.9(9) . . . . ?
V1 C28 C29 C38 115.5(13) . . . . ?
V1 C28 C32 C31 65.5(9) . . . . ?
V1 C28 C32 C41 -123.2(13) . . . . ?
V1 C29 C30 C31 -61.9(10) . . . . ?
V1 C29 C30 C39 115.8(12) . . . . ?
V1 C30 C31 C32 -62.8(9) . . . . ?
V1 C30 C31 C40 120.8(13) . . . . ?
V1 C31 C32 C28 -63.3(9) . . . . ?
V1 C31 C32 C41 125.4(14) . . . . ?
V1 C33 C34 C35 68.5(9) . . . . ?
V1 C33 C34 C42 -121.6(14) . . . . ?
V1 C33 C37 C36 -67.5(9) . . . . ?
V1 C33 C37 C45 114.5(15) . . . . ?
V1 C34 C35 C36 62.0(10) . . . . ?
V1 C34 C35 C43 -117.0(14) . . . . ?
V1 C35 C36 C37 61.2(10) . . . . ?
V1 C35 C36 C44 -124.4(14) . . . . ?
V1 C36 C37 C33 64.3(9) . . . . ?
V1 C36 C37 C45 -117.7(14) . . . . ?
F1 C13 C14 O3 -58.6(17) . . . . ?
F1 C13 C14 C15 118.1(15) . . . . ?
F2 C13 C14 O3 177.6(13) . . . . ?
F2 C13 C14 C15 -6(2) . . . . ?
F3 C13 C14 O3 59.9(17) . . . . ?
F3 C13 C14 C15 -123.3(14) . . . . ?
F7 C18 C19 O5 -41.8(15) . . . . ?
F7 C18 C19 C20 136.9(12) . . . . ?
F8 C18 C19 O5 -161.7(10) . . . . ?
F8 C18 C19 C20 17.0(17) . . . . ?
F9 C18 C19 O5 79.2(13) . . . . ?
F9 C18 C19 C20 -102.1(14) . . . . ?
F13 C23 C24 O7 48.9(19) . . . . ?
F13 C23 C24 C25 -133.0(17) . . . . ?
F14 C23 C24 O7 -86.8(18) . . . . ?
F14 C23 C24 C25 91.3(19) . . . . ?
F15 C23 C24 O7 164.8(13) . . . . ?
F15 C23 C24 C25 -17.1(19) . . . . ?
O1 C5 C6 O2 0.0(16) . . . . ?
O1 C5 C6 C7 179.6(10) . . . . ?
O2 C6 C7 C8 -2.0(18) . . . . ?
O2 C6 C7 C11 -178.6(10) . . . . ?
O3 C14 C15 C16 -6(2) . . . . ?
O4 C16 C17 F4 173.5(11) . . . . ?
O4 C16 C17 F5 49.5(17) . . . . ?
O4 C16 C17 F6 -69.8(15) . . . . ?
O5 C19 C20 C21 -2(2) . . . . ?
O6 C21 C22 F10 93.0(14) . . . . ?
O6 C21 C22 F11 -151.3(14) . . . . ?
O6 C21 C22 F12 -25.9(17) . . . . ?
O7 C24 C25 C26 -1(2) . . . . ?
O8 C26 C27 F16 -13.3(19) . . . . ?
O8 C26 C27 F17 116.4(14) . . . . ?
O8 C26 C27 F18 -133.0(13) . . . . ?
O8 C26 C27 F16A 36.1(17) . . . . ?
O8 C26 C27 F17A 167.3(17) . . . . ?
O8 C26 C27 F18A -74.5(17) . . . . ?
N1 C1 C2 C3 0(2) . . . . ?
N2 C11 C12 N1 -0.4(17) . . . . ?
N2 C11 C12 C4 -178.1(11) . . . . ?
C1 N1 C12 C4 1.4(18) . . . . ?
C1 N1 C12 C11 -176.3(11) . . . . ?
C1 C2 C3 C4 1.6(19) . . . . ?
C2 C3 C4 C5 176.1(12) . . . . ?
C2 C3 C4 C12 -1.5(18) . . . . ?
C3 C4 C5 O1 2(2) . . . . ?
C3 C4 C5 C6 -176.1(12) . . . . ?
C3 C4 C12 N1 0.1(18) . . . . ?
C3 C4 C12 C11 177.6(12) . . . . ?
C4 C5 C6 O2 178.0(10) . . . . ?
C4 C5 C6 C7 -2.4(18) . . . . ?
C5 C4 C12 N1 -177.7(11) . . . . ?
C5 C4 C12 C11 -0.1(18) . . . . ?
C5 C6 C7 C8 178.4(11) . . . . ?
C5 C6 C7 C11 1.8(18) . . . . ?
C6 C7 C8 C9 -175.0(12) . . . . ?
C6 C7 C11 N2 177.2(11) . . . . ?
C6 C7 C11 C12 -0.4(17) . . . . ?
C7 C8 C9 C10 -2.3(19) . . . . ?
C7 C11 C12 N1 177.3(10) . . . . ?
C7 C11 C12 C4 -0.5(18) . . . . ?
C8 C7 C11 N2 0.4(17) . . . . ?
C8 C7 C11 C12 -177.2(11) . . . . ?
C8 C9 C10 N2 0.7(19) . . . . ?
C10 N2 C11 C7 -2.0(18) . . . . ?
C10 N2 C11 C12 175.6(11) . . . . ?
C11 N2 C10 C9 1.4(18) . . . . ?
C11 C7 C8 C9 1.8(18) . . . . ?
C12 N1 C1 C2 -1.4(19) . . . . ?
C12 C4 C5 O1 179.5(11) . . . . ?
C12 C4 C5 C6 1.5(19) . . . . ?
C13 C14 C15 C16 177.3(13) . . . . ?
C14 C15 C16 O4 2(2) . . . . ?
C14 C15 C16 C17 180.0(13) . . . . ?
C15 C16 C17 F4 -5.0(18) . . . . ?
C15 C16 C17 F5 -128.9(14) . . . . ?
C15 C16 C17 F6 111.8(14) . . . . ?
C18 C19 C20 C21 179.8(12) . . . . ?
C19 C20 C21 O6 7(2) . . . . ?
C19 C20 C21 C22 -176.7(12) . . . . ?
C20 C21 C22 F10 -84.2(15) . . . . ?
C20 C21 C22 F11 31.5(19) . . . . ?
C20 C21 C22 F12 157.0(12) . . . . ?
C23 C24 C25 C26 -178.8(13) . . . . ?
C24 C25 C26 O8 -7(2) . . . . ?
C24 C25 C26 C27 176.1(13) . . . . ?
C25 C26 C27 F16 164.3(17) . . . . ?
C25 C26 C27 F17 -66.0(18) . . . . ?
C25 C26 C27 F18 44.5(18) . . . . ?
C25 C26 C27 F16A -146.4(15) . . . . ?
C25 C26 C27 F17A -15(2) . . . . ?
C25 C26 C27 F18A 103.1(17) . . . . ?
C28 C29 C30 V1 65.8(9) . . . . ?
C28 C29 C30 C31 3.9(15) . . . . ?
C28 C29 C30 C39 -178.4(12) . . . . ?
C29 C28 C32 V1 -64.3(9) . . . . ?
C29 C28 C32 C31 1.2(15) . . . . ?
C29 C28 C32 C41 172.5(13) . . . . ?
C29 C30 C31 V1 59.7(9) . . . . ?
C29 C30 C31 C32 -3.1(15) . . . . ?
C29 C30 C31 C40 -179.5(12) . . . . ?
C30 C31 C32 V1 64.5(9) . . . . ?
C30 C31 C32 C28 1.2(14) . . . . ?
C30 C31 C32 C41 -170.1(13) . . . . ?
C32 C28 C29 V1 64.9(10) . . . . ?
C32 C28 C29 C30 -3.0(15) . . . . ?
C32 C28 C29 C38 -179.6(12) . . . . ?
C33 C34 C35 V1 -64.9(9) . . . . ?
C33 C34 C35 C36 -2.9(16) . . . . ?
C33 C34 C35 C43 178.0(13) . . . . ?
C34 C33 C37 V1 65.0(10) . . . . ?
C34 C33 C37 C36 -2.5(16) . . . . ?
C34 C33 C37 C45 179.5(14) . . . . ?
C34 C35 C36 V1 -59.8(10) . . . . ?
C34 C35 C36 C37 1.5(16) . . . . ?
C34 C35 C36 C44 175.8(13) . . . . ?
C35 C36 C37 V1 -63.7(10) . . . . ?
C35 C36 C37 C33 0.6(16) . . . . ?
C35 C36 C37 C45 178.6(13) . . . . ?
C37 C33 C34 V1 -65.1(11) . . . . ?
C37 C33 C34 C35 3.4(16) . . . . ?
C37 C33 C34 C42 173.3(13) . . . . ?
C38 C29 C30 V1 -117.8(14) . . . . ?
C38 C29 C30 C31 -179.7(12) . . . . ?
C38 C29 C30 C39 -2(2) . . . . ?
C39 C30 C31 V1 -118.0(13) . . . . ?
C39 C30 C31 C32 179.2(12) . . . . ?
C39 C30 C31 C40 3(2) . . . . ?
C40 C31 C32 V1 -119.3(14) . . . . ?
C40 C31 C32 C28 177.4(13) . . . . ?
C40 C31 C32 C41 6(2) . . . . ?
C42 C34 C35 V1 124.9(14) . . . . ?
C42 C34 C35 C36 -173.1(13) . . . . ?
C42 C34 C35 C43 8(2) . . . . ?
C43 C35 C36 V1 119.3(14) . . . . ?
C43 C35 C36 C37 -179.5(13) . . . . ?
C43 C35 C36 C44 -5(2) . . . . ?
C44 C36 C37 V1 121.6(13) . . . . ?
C44 C36 C37 C33 -174.1(13) . . . . ?
C44 C36 C37 C45 4(2) . . . . ?
F13A C23 C24 O7 76.4(18) . . . . ?
F13A C23 C24 C25 -105.5(18) . . . . ?
F14A C23 C24 O7 -39.5(17) . . . . ?
F14A C23 C24 C25 138.5(15) . . . . ?
F15A C23 C24 O7 -149.6(17) . . . . ?
F15A C23 C24 C25 28(2) . . . . ?
_shelx_res_file
;
TITL 2018ncs0245_a.res in I2/a
2018ncs0245.res
created by SHELXL-2018/1 at 16:02:06 on 22-Mar-2018
REM Old TITL 2018ncs0245 in I2/a
REM SHELXT solution in I2/a
REM R1 0.219, Rweak 0.010, Alpha 0.065, Orientation as input
REM Formula found by SHELXT: C52 N3 O5 F15 V Y
CELL 1.54178 25.4111 14.7276 26.7414 90 106.921 90
ZERR 8 0.0055 0.0017 0.0037 0 0.021 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H F N O V Y
UNIT 360 280 144 16 64 8 8
DFIX 1.33 F6 C17 F5 C17 F4 C17 F3 C13 F1 C13 F2 C13 F10 C22 F12 C22 F11 C22 =
F8 C18 F9 C18 F7 C18 F18A C27 F15A C23 F13A C23 F14A C23 F14 C23 F17A C27 =
F18 C27 F17 C27 F16 C27 F16A C27
DFIX 1.37 F13 C23 F15 C23
RIGU
ISOR 0.01 0.02 C13 C17 C18 C22
L.S. 10
PLAN 10
SIZE 0.03 0.04 0.05
TEMP -173.14(10)
BOND $H
conf
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.200000
FVAR 0.13246
Y1 7 0.540271 0.556419 0.356195 11.00000 0.03161 0.06846 =
0.05545 0.00192 0.01988 0.00291
V1 6 0.331956 0.988025 0.377216 11.00000 0.03533 0.07433 =
0.05729 0.00591 0.02393 0.00749
F1 3 0.440750 0.755717 0.211081 11.00000 0.11672 0.10971 =
0.12837 0.03809 0.03289 0.04733
F2 3 0.420508 0.658784 0.147451 11.00000 0.12456 0.14936 =
0.09722 0.02700 -0.02560 -0.02076
F3 3 0.500904 0.705815 0.178133 11.00000 0.11973 0.15037 =
0.07877 0.01698 0.03299 -0.02744
F4 3 0.374342 0.380722 0.196291 11.00000 0.05014 0.11484 =
0.08102 -0.00469 0.00887 -0.01568
F5 3 0.395649 0.347262 0.276931 11.00000 0.18035 0.17339 =
0.08445 -0.02464 0.04659 -0.11992
F6 3 0.444691 0.304545 0.229745 11.00000 0.10618 0.10521 =
0.12773 -0.03582 -0.01798 0.03101
F7 3 0.687705 0.704029 0.298833 11.00000 0.04071 0.09894 =
0.07986 0.02444 0.02361 -0.00563
F8 3 0.754633 0.620983 0.338745 11.00000 0.03151 0.09777 =
0.15673 0.03409 0.04134 0.00567
F9 3 0.719935 0.715120 0.381036 11.00000 0.07135 0.11006 =
0.08169 -0.02064 0.03077 -0.03747
F10 3 0.684993 0.288244 0.359994 11.00000 0.16220 0.08907 =
0.13800 0.01754 0.09927 0.04406
F11 3 0.728577 0.352453 0.427839 11.00000 0.08714 0.09661 =
0.24398 0.04261 -0.05624 -0.00483
F12 3 0.650626 0.293622 0.420810 11.00000 0.09171 0.10609 =
0.10500 0.04716 0.05407 0.03394
PART 2
F13 3 0.503954 0.277653 0.433435 10.50000 0.07970
F14 3 0.477157 0.359185 0.492892 10.50000 0.10951
F15 3 0.550777 0.293890 0.513222 10.50000 0.06806
PART 0
PART 1
F16 3 0.688524 0.638032 0.503977 10.50000 0.09663
F17 3 0.645550 0.609679 0.564286 10.50000 0.07197
F18 3 0.697339 0.512817 0.546774 10.50000 0.07698
PART 0
O1 5 0.410664 0.965999 0.385204 11.00000 0.03369 0.06409 =
0.06550 -0.00152 0.02153 0.00238
O2 5 0.328850 0.854371 0.370264 11.00000 0.02733 0.08863 =
0.05391 -0.00146 0.02186 0.00295
O3 5 0.507093 0.626738 0.275234 11.00000 0.03923 0.07724 =
0.06391 0.01604 0.02100 0.00610
O4 5 0.486981 0.452311 0.299697 11.00000 0.04947 0.07675 =
0.05330 -0.00319 0.01427 0.00212
O5 5 0.618485 0.612481 0.339041 11.00000 0.04071 0.08250 =
0.05986 0.01107 0.02798 0.01512
O6 5 0.600712 0.434355 0.364976 11.00000 0.04452 0.07402 =
0.06236 0.00013 0.02537 0.00121
O7 5 0.516441 0.456025 0.412332 11.00000 0.03822 0.07030 =
0.06084 -0.00144 0.02273 0.00514
O8 5 0.601154 0.581081 0.439139 11.00000 0.03890 0.07729 =
0.05708 0.00063 0.01933 -0.00371
N1 4 0.533216 0.718627 0.377783 11.00000 0.05207
N2 4 0.447053 0.602049 0.359453 11.00000 0.05482
C1 1 0.576072 0.775929 0.389653 11.00000 0.04056 0.06329 =
0.06143 -0.00625 0.02128 0.00368
AFIX 43
H1 2 0.611529 0.751406 0.393090 11.00000 -1.20000
AFIX 0
C2 1 0.572263 0.866718 0.397108 11.00000 0.02780 0.06327 =
0.07470 -0.01052 0.03089 -0.01713
AFIX 43
H2 2 0.604183 0.903921 0.405501 11.00000 -1.20000
AFIX 0
C3 1 0.519843 0.904746 0.392127 11.00000 0.03397 0.07328 =
0.06666 -0.01486 0.02230 -0.00093
AFIX 43
H3 2 0.515860 0.968204 0.396269 11.00000 -1.20000
AFIX 0
C4 1 0.473880 0.847329 0.380986 11.00000 0.03349 0.06556 =
0.05474 -0.00393 0.01790 -0.00087
C5 1 0.421063 0.878375 0.378475 11.00000 0.03397 0.06047 =
0.05496 -0.00135 0.01482 -0.00414
C6 1 0.377568 0.818274 0.370448 11.00000 0.02939 0.06654 =
0.04767 0.00032 0.02190 -0.00166
C7 1 0.385154 0.725094 0.362715 11.00000 0.02776 0.06470 =
0.05090 0.00482 0.01955 -0.00444
C8 1 0.342038 0.660249 0.355602 11.00000 0.03351 0.06799 =
0.05096 -0.00375 0.01335 -0.01150
AFIX 43
H8 2 0.305782 0.679969 0.353169 11.00000 -1.20000
AFIX 0
C9 1 0.352257 0.572142 0.352344 11.00000 0.03892 0.07090 =
0.06074 -0.00867 0.01848 -0.00846
AFIX 43
H9 2 0.323736 0.528787 0.348883 11.00000 -1.20000
AFIX 0
C10 1 0.407425 0.542741 0.354123 11.00000 0.04492 0.06743 =
0.05605 -0.00956 0.01664 -0.01193
AFIX 43
H10 2 0.414756 0.479973 0.351393 11.00000 -1.20000
AFIX 0
C11 1 0.437305 0.691879 0.364523 11.00000 0.02702 0.06759 =
0.05700 0.00230 0.02230 -0.00260
C12 1 0.481961 0.754911 0.374035 11.00000 0.02521 0.06154 =
0.05022 0.00594 0.01564 0.00025
C13 1 0.457271 0.683535 0.191442 11.00000 0.07436 0.09063 =
0.08438 0.00877 0.00475 -0.01014
C14 1 0.470353 0.607689 0.232545 11.00000 0.03074 0.08990 =
0.07349 0.01156 0.01719 -0.00133
C15 1 0.440470 0.528068 0.222124 11.00000 0.04297 0.09031 =
0.06345 0.00821 0.02220 -0.00290
AFIX 43
H15 2 0.411489 0.523068 0.190437 11.00000 -1.20000
AFIX 0
C16 1 0.451250 0.456138 0.255962 11.00000 0.04446 0.08165 =
0.05202 -0.00907 0.02026 -0.00319
C17 1 0.415539 0.372898 0.239997 11.00000 0.06724 0.06721 =
0.06491 0.00164 0.00826 -0.00055
C18 1 0.707131 0.656443 0.341905 11.00000 0.04803 0.07546 =
0.06929 0.00139 0.01836 0.00158
C19 1 0.667647 0.582680 0.350599 11.00000 0.03702 0.07080 =
0.04735 -0.00130 0.01272 0.00611
C20 1 0.685834 0.499250 0.367190 11.00000 0.03312 0.07012 =
0.06196 -0.00169 0.02094 0.00871
AFIX 43
H20 2 0.723881 0.486833 0.373366 11.00000 -1.20000
AFIX 0
C21 1 0.653890 0.432820 0.375530 11.00000 0.04273 0.06748 =
0.05114 -0.00713 0.01939 0.00335
C22 1 0.678493 0.343658 0.396746 11.00000 0.05487 0.07379 =
0.08337 0.00581 0.01990 0.00118
C23 1 0.515865 0.341538 0.470637 11.00000 0.07417 0.09309 =
0.06050 0.00665 0.03634 -0.00335
C24 1 0.542155 0.426632 0.456154 11.00000 0.04782 0.07467 =
0.06245 0.00638 0.03191 0.00809
C25 1 0.588281 0.461776 0.492109 11.00000 0.06170 0.10359 =
0.05120 0.02128 0.01392 -0.00008
AFIX 43
H25 2 0.603257 0.432129 0.524713 11.00000 -1.20000
AFIX 0
C26 1 0.612028 0.537808 0.481084 11.00000 0.03367 0.08783 =
0.05427 0.00306 0.02262 0.01429
C27 1 0.661993 0.579639 0.523883 11.00000 0.05100 0.13139 =
0.05694 0.04661 0.00846 -0.01099
C28 1 0.309340 1.089626 0.432481 11.00000 0.05279 0.07792 =
0.06871 0.00536 0.03311 0.00988
AFIX 43
H28 2 0.294467 1.147294 0.419968 11.00000 -1.20000
AFIX 0
C29 1 0.365250 1.069063 0.453116 11.00000 0.05157 0.06289 =
0.05775 -0.00968 0.02717 -0.00003
C30 1 0.368140 0.977795 0.469016 11.00000 0.04764 0.06713 =
0.05512 -0.00752 0.02620 0.00603
C31 1 0.316937 0.938387 0.456329 11.00000 0.04824 0.07600 =
0.05367 -0.00170 0.01976 -0.00081
C32 1 0.278538 1.008995 0.433485 11.00000 0.03935 0.08300 =
0.05775 -0.00194 0.02591 0.00754
C33 1 0.267956 1.074044 0.320550 11.00000 0.03862 0.10083 =
0.06068 0.01359 0.02486 0.01961
AFIX 43
H33 2 0.241972 1.106753 0.332845 11.00000 -1.20000
AFIX 0
C34 1 0.318529 1.108478 0.319917 11.00000 0.05118 0.08774 =
0.06253 0.01591 0.02892 0.01133
C35 1 0.342145 1.040250 0.296014 11.00000 0.04197 0.10117 =
0.05582 0.01040 0.02203 0.01348
C36 1 0.307441 0.964853 0.285036 11.00000 0.04667 0.09896 =
0.04895 0.01153 0.01843 0.01439
C37 1 0.259762 0.986217 0.301118 11.00000 0.04415 0.10130 =
0.06214 0.01123 0.02337 0.01260
C38 1 0.411767 1.137364 0.459112 11.00000 0.06190 0.06757 =
0.07405 -0.01989 0.02590 -0.00676
AFIX 137
H38A 2 0.437344 1.115055 0.440664 11.00000 -1.50000
H38B 2 0.431379 1.145108 0.496269 11.00000 -1.50000
H38C 2 0.396477 1.195833 0.444258 11.00000 -1.50000
AFIX 0
C39 1 0.422575 0.927377 0.495476 11.00000 0.05433 0.11444 =
0.06132 -0.00112 0.01628 0.01964
AFIX 137
H39A 2 0.421080 0.866120 0.480814 11.00000 -1.50000
H39B 2 0.427711 0.923309 0.533176 11.00000 -1.50000
H39C 2 0.453399 0.960779 0.489190 11.00000 -1.50000
AFIX 0
C40 1 0.305059 0.843348 0.467783 11.00000 0.05552 0.07581 =
0.06729 -0.01005 0.02770 -0.01202
AFIX 137
H40A 2 0.266339 0.829563 0.450271 11.00000 -1.50000
H40B 2 0.312452 0.835629 0.505601 11.00000 -1.50000
H40C 2 0.328534 0.802029 0.455047 11.00000 -1.50000
AFIX 0
C41 1 0.215952 1.002686 0.420599 11.00000 0.04375 0.10964 =
0.09269 0.02516 0.02895 0.01081
AFIX 137
H41A 2 0.198841 1.039985 0.389808 11.00000 -1.50000
H41B 2 0.204455 1.024685 0.450389 11.00000 -1.50000
H41C 2 0.204444 0.939344 0.413341 11.00000 -1.50000
AFIX 0
C42 1 0.339881 1.203570 0.332577 11.00000 0.07535 0.09463 =
0.06483 0.01561 0.03264 0.00467
AFIX 137
H42A 2 0.318218 1.234622 0.352329 11.00000 -1.50000
H42B 2 0.336793 1.236701 0.300065 11.00000 -1.50000
H42C 2 0.378538 1.201331 0.353583 11.00000 -1.50000
AFIX 0
C43 1 0.397479 1.048369 0.285040 11.00000 0.06010 0.13773 =
0.09122 0.02096 0.05435 0.00745
AFIX 137
H43A 2 0.425674 1.066222 0.317114 11.00000 -1.50000
H43B 2 0.395052 1.094391 0.257992 11.00000 -1.50000
H43C 2 0.407331 0.989720 0.272950 11.00000 -1.50000
AFIX 0
C44 1 0.313417 0.880392 0.257395 11.00000 0.07272 0.10420 =
0.06575 0.00599 0.02779 0.02248
AFIX 137
H44A 2 0.352255 0.871129 0.259751 11.00000 -1.50000
H44B 2 0.291831 0.885153 0.220586 11.00000 -1.50000
H44C 2 0.300130 0.828861 0.273510 11.00000 -1.50000
AFIX 0
C45 1 0.211740 0.925427 0.295469 11.00000 0.04479 0.10628 =
0.06715 0.00614 0.01250 0.00865
AFIX 137
H45A 2 0.224674 0.864087 0.307015 11.00000 -1.50000
H45B 2 0.189585 0.923652 0.258741 11.00000 -1.50000
H45C 2 0.189277 0.948433 0.316923 11.00000 -1.50000
AFIX 0
PART 1
F13A 3 0.524860 0.267774 0.447477 10.50000 0.07975
F14A 3 0.459528 0.347308 0.454950 10.50000 0.07700
F15A 3 0.521717 0.328946 0.519783 10.50000 0.11213
PART 0
PART 2
F16A 3 0.662614 0.670769 0.521161 10.50000 0.08056
F17A 3 0.665430 0.544839 0.569750 10.50000 0.13413
F18A 3 0.707550 0.557959 0.511198 10.50000 0.11180
HKLF 4
REM 2018ncs0245_a.res in I2/a
REM R1 = 0.0983 for 3121 Fo > 4sig(Fo) and 0.1426 for all 4967 data
REM 668 parameters refined using 752 restraints
END
WGHT 0.2000 0.0000
REM Highest difference peak 1.465, deepest hole -1.855, 1-sigma level 0.159
Q1 1 0.5393 0.6391 0.3618 11.00000 0.05 1.47
Q2 1 0.5369 0.4760 0.3591 11.00000 0.05 1.12
Q3 1 0.6506 0.6621 0.5523 11.00000 0.05 0.85
Q4 1 0.5004 0.3771 0.5211 11.00000 0.05 0.80
Q5 1 0.5204 0.5592 0.3074 11.00000 0.05 0.79
Q6 1 0.5517 0.5592 0.3993 11.00000 0.05 0.78
Q7 1 0.5458 0.5460 0.3899 11.00000 0.05 0.75
Q8 1 0.3341 1.0644 0.3631 11.00000 0.05 0.73
Q9 1 0.3310 0.9111 0.3806 11.00000 0.05 0.72
Q10 1 0.4664 0.7982 0.2481 11.00000 0.05 0.67
;
_shelx_res_checksum 17862
_olex2_submission_special_instructions 'No special instructions were received'
### END OF CIF 5
#### END OF CIF
#######################################################################
#
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1841191'
_audit_update_record
;
2018-05-03 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;
# [Gd(hfac)3(n,N'-O,O'-pd)VCptet2]
# mo_cb_gdv_cptet_150k_0m
_audit_creation_date 2018-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number 2016/6
# start Validation Reply Form
_vrf_PLAT094_mo_cb_gdv_cptet_150k_0m
;
PROBLEM: Ratio of Maximum / Minimum Residual Density .... 4.20 Report
RESPONSE: Due to one larger residual electron density peak that we have not been able to
account for chemically or through twinning.
;
_vrf_PLAT213_mo_cb_gdv_cptet_150k_0m
;
PROBLEM: Atom F17 has ADP max/min Ratio ..... 4.1 prolat
RESPONSE: This atom belongs to one of the CF3 groups which, as is commonly
the case, shows a high degree of atomic vibration.
;
# end Validation Reply Form
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C45 H35 F18 Gd N2 O8 V'
_chemical_formula_sum 'C45 H35 F18 Gd N2 O8 V'
_chemical_formula_weight 1281.94
_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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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 31.353(2)
_cell_length_b 14.8019(9)
_cell_length_c 25.6961(15)
_cell_angle_alpha 90
_cell_angle_beta 124.668(2)
_cell_angle_gamma 90
_cell_volume 9807.9(11)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 9967
_cell_measurement_temperature 150
_cell_measurement_theta_max 28.259
_cell_measurement_theta_min 2.602
_shelx_estimated_absorpt_T_max 0.968
_shelx_estimated_absorpt_T_min 0.673
_exptl_absorpt_coefficient_mu 1.653
_exptl_absorpt_correction_T_max 0.7457
_exptl_absorpt_correction_T_min 0.6625
_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 0.0531 after correction. The Ratio of minimum to maximum transmission is 0.8884. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour green
_exptl_crystal_colour_primary green
_exptl_crystal_density_diffrn 1.736
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 5056
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.02
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0297
_diffrn_reflns_av_unetI/netI 0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 41
_diffrn_reflns_limit_h_min -41
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 34
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_number 47555
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.271
_diffrn_reflns_theta_min 2.416
_diffrn_ambient_temperature 150
_diffrn_detector 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type 'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 VENTURE'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_collimation 'focusing mirrors'
_diffrn_radiation_monochromator 'multilayer mirror optics'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed tube'
_diffrn_source_type 'INCOATEC I\ms 3.0'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 10891
_reflns_number_total 12106
_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 V8.37A (Bruker-AXS, 2016)'
_computing_data_collection 'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction 'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'XT (Sheldrick, 2015)'
_refine_diff_density_max 2.060
_refine_diff_density_min -0.491
_refine_diff_density_rms 0.083
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.020
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 735
_refine_ls_number_reflns 12106
_refine_ls_number_restraints 1083
_refine_ls_R_factor_all 0.0353
_refine_ls_R_factor_gt 0.0309
_refine_ls_restrained_S_all 1.026
_refine_ls_shift/su_max 0.007
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+27.3989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0795
_refine_ls_wR_factor_ref 0.0829
_refine_special_details
;
Several of the CF3 groups were modelled as disordered over two sites,
two of them with occupancies fixed at 0.75/0.25 after competitive refinement
of the occupancies and one with 0.5/0.5 occupancies. Similarity restraints
were applied to the C-F distances and ISOR restraints to the F adps.
;
_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. Restrained distances
F4A-C17 \\sim F6-C17 \\sim F4-C17 \\sim F6A-C17 \\sim F5A-C17 \\sim F5-C17
with sigma of 0.02
F1A-C13 \\sim F1-C13 \\sim F3-C13 \\sim F3A-C13 \\sim F2-C13 \\sim F2A-C13
with sigma of 0.02
F17A-C27 \\sim F16A-C27 \\sim F18A-C27 \\sim F17-C27 \\sim F16-C27 \\sim
F18-C27
with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8)
\\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq,
Uanis(F12) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq,
Uanis(F1A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A) \\sim Ueq, : with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
All non-hydrogen atoms
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
Fixed Sof: F1(0.5) F2(0.5) F3(0.5) F4(0.75) F5(0.75) F6(0.75) F16(0.75)
F17(0.75) F18(0.75) F1A(0.5) F2A(0.5) F3A(0.5) F4A(0.25) F5A(0.25) F6A(0.25)
F17A(0.25) F16A(0.25) F18A(0.25)
6.a Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C15(H15), C20(H20),
C25(H25), C28(H28), C33(H33)
6.b Idealised Me refined as rotating group:
C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,
H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,
H45B,H45C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.64472(2) 0.44352(2) 0.68492(2) 0.02240(4) Uani 1 1 d . U . . .
V1 V 0.62292(2) 0.01284(3) 0.45513(2) 0.02536(9) Uani 1 1 d . U . . .
F1 F 0.4924(3) 0.3603(8) 0.6785(6) 0.120(4) Uani 0.5 1 d D U P A 1
F2 F 0.4539(3) 0.4847(5) 0.6483(5) 0.090(2) Uani 0.5 1 d D U P A 1
F3 F 0.4379(3) 0.3899(6) 0.5807(4) 0.090(2) Uani 0.5 1 d D U P A 1
F4 F 0.56060(14) 0.7257(2) 0.57462(18) 0.0822(12) Uani 0.75 1 d D U P B 1
F5 F 0.48382(14) 0.6952(3) 0.5286(3) 0.1164(19) Uani 0.75 1 d D U P B 1
F6 F 0.5282(4) 0.6459(3) 0.4944(2) 0.158(3) Uani 0.75 1 d D U P B 1
F7 F 0.82362(11) 0.2966(2) 0.82407(16) 0.1039(11) Uani 1 1 d . U . . .
F8 F 0.85368(11) 0.3441(2) 0.7735(2) 0.1151(13) Uani 1 1 d . U . . .
F9 F 0.79219(14) 0.2459(2) 0.73413(19) 0.1076(11) Uani 1 1 d . U . . .
F10 F 0.76812(12) 0.69761(16) 0.70900(19) 0.0981(11) Uani 1 1 d . U . . .
F11 F 0.80410(8) 0.61756(15) 0.67703(11) 0.0572(5) Uani 1 1 d . U . . .
F12 F 0.72372(11) 0.6460(2) 0.61521(16) 0.1281(16) Uani 1 1 d . U . . .
F13 F 0.70021(9) 0.29609(15) 0.88927(10) 0.0573(5) Uani 1 1 d . U . . .
F14 F 0.65910(14) 0.37708(17) 0.91412(12) 0.0886(10) Uani 1 1 d . U . . .
F15 F 0.61912(10) 0.2827(2) 0.83798(13) 0.0916(10) Uani 1 1 d . U . . .
F16 F 0.6386(2) 0.7068(3) 0.8285(2) 0.106(2) Uani 0.75 1 d D U P C 1
F17 F 0.5653(2) 0.6425(2) 0.7937(3) 0.118(2) Uani 0.75 1 d D U P C 1
F18 F 0.58131(14) 0.7059(2) 0.73225(14) 0.0555(8) Uani 0.75 1 d D U P C 1
O1 O 0.62983(7) 0.14652(12) 0.45916(8) 0.0270(4) Uani 1 1 d . U . . .
O2 O 0.61508(7) 0.03396(12) 0.52561(8) 0.0269(3) Uani 1 1 d . U . . .
O3 O 0.56072(7) 0.41805(14) 0.66092(9) 0.0340(4) Uani 1 1 d . U . . .
O4 O 0.58732(7) 0.54516(13) 0.60441(9) 0.0325(4) Uani 1 1 d . U . . .
O5 O 0.72794(7) 0.37475(13) 0.73437(9) 0.0321(4) Uani 1 1 d . U . . .
O6 O 0.70214(7) 0.54892(12) 0.68712(10) 0.0331(4) Uani 1 1 d . U . . .
O7 O 0.66090(7) 0.38614(12) 0.78058(8) 0.0281(4) Uani 1 1 d . U . . .
O8 O 0.63493(8) 0.56506(12) 0.73854(10) 0.0349(4) Uani 1 1 d . U . . .
N1 N 0.64084(8) 0.39641(14) 0.58757(9) 0.0250(4) Uani 1 1 d . U . . .
N2 N 0.62307(8) 0.27892(14) 0.65539(9) 0.0259(4) Uani 1 1 d . U . . .
C1 C 0.64675(11) 0.45424(17) 0.55269(12) 0.0291(5) Uani 1 1 d . U . . .
H1 H 0.649789 0.516729 0.562665 0.035 Uiso 1 1 calc R . . . .
C2 C 0.64871(11) 0.42736(18) 0.50178(12) 0.0314(5) Uani 1 1 d . U . . .
H2 H 0.653546 0.470826 0.478377 0.038 Uiso 1 1 calc R . . . .
C3 C 0.64356(10) 0.33770(18) 0.48620(11) 0.0282(5) Uani 1 1 d . U . . .
H3 H 0.644689 0.318369 0.451747 0.034 Uiso 1 1 calc R . . . .
C4 C 0.63659(9) 0.27438(16) 0.52164(10) 0.0229(4) Uani 1 1 d . U . . .
C5 C 0.62960(9) 0.18020(16) 0.50709(10) 0.0230(4) Uani 1 1 d . U . . .
C6 C 0.62204(9) 0.12076(16) 0.54240(11) 0.0236(4) Uani 1 1 d . U . . .
C7 C 0.61948(9) 0.15215(16) 0.59292(10) 0.0229(4) Uani 1 1 d . U . . .
C8 C 0.60862(10) 0.09412(18) 0.62756(12) 0.0283(5) Uani 1 1 d . U . . .
H8 H 0.604618 0.031028 0.619327 0.034 Uiso 1 1 calc R . . . .
C9 C 0.60393(11) 0.13000(19) 0.67323(12) 0.0326(6) Uani 1 1 d . U . . .
H9 H 0.595591 0.092251 0.696151 0.039 Uiso 1 1 calc R . . . .
C10 C 0.61153(11) 0.22280(18) 0.68582(12) 0.0308(5) Uani 1 1 d . U . . .
H10 H 0.608245 0.246654 0.717709 0.037 Uiso 1 1 calc R . . . .
C11 C 0.62639(9) 0.24528(16) 0.60839(10) 0.0221(4) Uani 1 1 d . U . . .
C12 C 0.63555(9) 0.30707(16) 0.57266(10) 0.0223(4) Uani 1 1 d . U . . .
C13 C 0.47681(13) 0.4215(3) 0.63712(19) 0.0575(9) Uani 1 1 d D U . . .
C14 C 0.51934(11) 0.4611(2) 0.63140(14) 0.0363(6) Uani 1 1 d . U . . .
C15 C 0.50775(12) 0.5384(2) 0.59533(17) 0.0448(7) Uani 1 1 d . U . . .
H15 H 0.475257 0.567447 0.577738 0.054 Uiso 1 1 calc R . . . .
C16 C 0.54317(11) 0.57418(19) 0.58456(13) 0.0346(6) Uani 1 1 d . U . . .
C17 C 0.52802(13) 0.6592(2) 0.54365(16) 0.0515(8) Uani 1 1 d D U . . .
C18 C 0.81050(16) 0.3195(3) 0.7682(3) 0.0684(12) Uani 1 1 d . U . . .
C19 C 0.76867(11) 0.3941(2) 0.73862(14) 0.0363(6) Uani 1 1 d . U . . .
C20 C 0.77996(11) 0.4731(2) 0.71994(15) 0.0380(6) Uani 1 1 d . U . . .
H20 H 0.812077 0.478466 0.724384 0.046 Uiso 1 1 calc R . . . .
C21 C 0.74537(11) 0.54414(18) 0.69499(13) 0.0309(5) Uani 1 1 d . U . . .
C22 C 0.75985(13) 0.6274(2) 0.67278(18) 0.0475(7) Uani 1 1 d . U . . .
C23 C 0.65708(13) 0.3420(2) 0.86533(15) 0.0395(6) Uani 1 1 d . U . . .
C24 C 0.64961(10) 0.41323(19) 0.81759(12) 0.0287(5) Uani 1 1 d . U . . .
C25 C 0.63071(11) 0.4972(2) 0.81911(14) 0.0348(6) Uani 1 1 d . U . . .
H25 H 0.622048 0.507667 0.848521 0.042 Uiso 1 1 calc R . . . .
C26 C 0.62417(11) 0.56618(18) 0.77859(14) 0.0327(6) Uani 1 1 d . U . . .
C27 C 0.60208(14) 0.6557(2) 0.78350(16) 0.0467(7) Uani 1 1 d D U . . .
C28 C 0.67830(11) -0.0737(2) 0.44589(14) 0.0382(6) Uani 1 1 d . U . . .
H28 H 0.665536 -0.105563 0.407606 0.046 Uiso 1 1 calc R . . . .
C29 C 0.69853(11) 0.0145(2) 0.45906(14) 0.0388(6) Uani 1 1 d . U . . .
C30 C 0.71523(11) 0.0349(2) 0.52196(14) 0.0405(7) Uani 1 1 d . U . . .
C31 C 0.70401(12) -0.0394(2) 0.54631(14) 0.0436(7) Uani 1 1 d . U . . .
C32 C 0.67990(11) -0.1077(2) 0.49848(13) 0.0398(6) Uani 1 1 d . U . . .
C33 C 0.56776(11) -0.0886(2) 0.37778(13) 0.0373(6) Uani 1 1 d . U . . .
H33 H 0.580394 -0.145829 0.375585 0.045 Uiso 1 1 calc R . . . .
C34 C 0.56691(11) -0.0089(2) 0.34612(12) 0.0373(6) Uani 1 1 d . U . . .
C35 C 0.54392(10) 0.05961(18) 0.36059(13) 0.0333(6) Uani 1 1 d . U . . .
C36 C 0.53182(10) 0.02252(19) 0.40137(12) 0.0309(5) Uani 1 1 d . U . . .
C37 C 0.54705(11) -0.06957(18) 0.41274(13) 0.0337(6) Uani 1 1 d . U . . .
C38 C 0.70421(15) 0.0766(3) 0.41688(19) 0.0535(8) Uani 1 1 d . U . . .
H38A H 0.688183 0.048655 0.375144 0.080 Uiso 1 1 calc GR . . . .
H38B H 0.741096 0.087229 0.435648 0.080 Uiso 1 1 calc GR . . . .
H38C H 0.687043 0.134215 0.412409 0.080 Uiso 1 1 calc GR . . . .
C39 C 0.74226(12) 0.1207(3) 0.55540(18) 0.0563(9) Uani 1 1 d . U . . .
H39A H 0.725105 0.171893 0.526504 0.084 Uiso 1 1 calc GR . . . .
H39B H 0.778541 0.117827 0.569350 0.084 Uiso 1 1 calc GR . . . .
H39C H 0.740832 0.128570 0.592254 0.084 Uiso 1 1 calc GR . . . .
C40 C 0.71526(16) -0.0484(3) 0.61070(15) 0.0604(11) Uani 1 1 d . U . . .
H40A H 0.737455 -0.101189 0.631900 0.091 Uiso 1 1 calc GR . . . .
H40B H 0.682679 -0.055952 0.607225 0.091 Uiso 1 1 calc GR . . . .
H40C H 0.733057 0.006062 0.635356 0.091 Uiso 1 1 calc GR . . . .
C41 C 0.66716(15) -0.2015(2) 0.50712(18) 0.0562(9) Uani 1 1 d . U . . .
H41A H 0.654014 -0.199732 0.533768 0.084 Uiso 1 1 calc GR . . . .
H41B H 0.698466 -0.238930 0.527486 0.084 Uiso 1 1 calc GR . . . .
H41C H 0.640641 -0.227217 0.465768 0.084 Uiso 1 1 calc GR . . . .
C42 C 0.57965(14) -0.0035(3) 0.29789(15) 0.0576(10) Uani 1 1 d . U . . .
H42A H 0.593846 0.056390 0.299782 0.086 Uiso 1 1 calc GR . . . .
H42B H 0.548083 -0.013341 0.255519 0.086 Uiso 1 1 calc GR . . . .
H42C H 0.605321 -0.049853 0.306955 0.086 Uiso 1 1 calc GR . . . .
C43 C 0.53303(13) 0.1547(2) 0.33718(15) 0.0463(8) Uani 1 1 d . U . . .
H43A H 0.544104 0.195866 0.372587 0.070 Uiso 1 1 calc GR . . . .
H43B H 0.495761 0.162054 0.305184 0.070 Uiso 1 1 calc GR . . . .
H43C H 0.552082 0.168620 0.318388 0.070 Uiso 1 1 calc GR . . . .
C44 C 0.50540(12) 0.0709(2) 0.42677(17) 0.0443(7) Uani 1 1 d . U . . .
H44A H 0.511686 0.038538 0.463787 0.066 Uiso 1 1 calc GR . . . .
H44B H 0.468030 0.073537 0.394080 0.066 Uiso 1 1 calc GR . . . .
H44C H 0.519204 0.132447 0.439080 0.066 Uiso 1 1 calc GR . . . .
C45 C 0.54005(14) -0.1335(2) 0.45260(17) 0.0481(8) Uani 1 1 d . U . . .
H45A H 0.554490 -0.192630 0.453433 0.072 Uiso 1 1 calc GR . . . .
H45B H 0.503017 -0.139852 0.434628 0.072 Uiso 1 1 calc GR . . . .
H45C H 0.558073 -0.109791 0.495779 0.072 Uiso 1 1 calc GR . . . .
F1A F 0.4765(3) 0.3323(4) 0.6347(5) 0.090(2) Uani 0.5 1 d D U P A 2
F2A F 0.4885(4) 0.4402(8) 0.6941(4) 0.111(3) Uani 0.5 1 d D U P A 2
F3A F 0.4313(2) 0.4479(9) 0.5969(6) 0.136(4) Uani 0.5 1 d D U P A 2
F4A F 0.5551(4) 0.6684(9) 0.5203(6) 0.072(3) Uiso 0.25 1 d D U P B 2
F5A F 0.5277(8) 0.7277(10) 0.5704(8) 0.126(6) Uiso 0.25 1 d D U P B 2
F6A F 0.4833(4) 0.6466(8) 0.4887(4) 0.063(2) Uiso 0.25 1 d D U P B 2
F17A F 0.5635(4) 0.6803(9) 0.7312(5) 0.075(4) Uiso 0.25 1 d D U P C 2
F16A F 0.5937(4) 0.6563(7) 0.8257(4) 0.052(2) Uiso 0.25 1 d D U P C 2
F18A F 0.6369(7) 0.7181(12) 0.8091(9) 0.097(6) Uiso 0.25 1 d D U P C 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Gd1 0.02304(6) 0.02192(7) 0.02427(7) -0.00063(4) 0.01466(5) 0.00211(4)
V1 0.0261(2) 0.0261(2) 0.02242(19) -0.00192(15) 0.01292(16) 0.00440(15)
F1 0.066(4) 0.161(8) 0.166(7) 0.104(7) 0.085(5) 0.041(5)
F2 0.070(4) 0.110(5) 0.134(6) -0.036(4) 0.085(4) -0.010(3)
F3 0.063(4) 0.112(5) 0.118(4) -0.050(4) 0.065(3) -0.048(4)
F4 0.0608(19) 0.0414(16) 0.098(3) 0.0249(16) 0.0171(18) -0.0081(14)
F5 0.0481(18) 0.067(2) 0.202(5) 0.074(3) 0.052(3) 0.0322(17)
F6 0.352(9) 0.055(2) 0.066(3) 0.025(2) 0.118(4) 0.043(4)
F7 0.0633(16) 0.105(2) 0.121(2) 0.068(2) 0.0389(16) 0.0395(16)
F8 0.0669(16) 0.088(2) 0.221(4) 0.062(2) 0.100(2) 0.0374(15)
F9 0.116(2) 0.0608(17) 0.173(3) 0.0029(18) 0.098(2) 0.0357(16)
F10 0.114(2) 0.0363(12) 0.204(3) -0.0319(16) 0.126(2) -0.0226(13)
F11 0.0614(13) 0.0538(12) 0.0787(14) 0.0068(10) 0.0531(12) -0.0043(10)
F12 0.0647(16) 0.131(3) 0.110(2) 0.088(2) 0.0032(15) -0.0316(17)
F13 0.0669(13) 0.0573(12) 0.0613(12) 0.0280(10) 0.0446(11) 0.0257(10)
F14 0.176(3) 0.0652(15) 0.0790(16) 0.0270(12) 0.105(2) 0.0461(17)
F15 0.0742(16) 0.0921(19) 0.0845(17) 0.0337(15) 0.0308(14) -0.0343(14)
F16 0.129(4) 0.0436(19) 0.064(3) -0.030(2) 0.007(2) 0.031(2)
F17 0.147(4) 0.0431(19) 0.274(6) 0.013(3) 0.186(5) 0.024(2)
F18 0.0639(19) 0.0402(16) 0.0624(18) 0.0091(13) 0.0359(15) 0.0269(15)
O1 0.0332(9) 0.0282(9) 0.0245(8) -0.0026(7) 0.0193(7) 0.0001(7)
O2 0.0341(9) 0.0221(8) 0.0263(8) -0.0015(6) 0.0182(7) 0.0000(7)
O3 0.0259(9) 0.0393(10) 0.0392(10) 0.0043(8) 0.0198(8) 0.0035(8)
O4 0.0309(9) 0.0326(10) 0.0342(10) 0.0062(7) 0.0186(8) 0.0072(7)
O5 0.0299(9) 0.0330(10) 0.0389(10) 0.0076(8) 0.0228(8) 0.0070(7)
O6 0.0305(9) 0.0252(9) 0.0445(11) -0.0031(7) 0.0220(9) -0.0008(7)
O7 0.0323(9) 0.0278(9) 0.0274(8) -0.0001(7) 0.0189(7) 0.0049(7)
O8 0.0479(12) 0.0272(9) 0.0390(10) -0.0025(7) 0.0303(10) 0.0030(8)
N1 0.0280(10) 0.0235(10) 0.0241(9) 0.0008(7) 0.0152(8) -0.0001(8)
N2 0.0296(10) 0.0285(10) 0.0242(9) -0.0029(8) 0.0180(8) -0.0024(8)
C1 0.0352(13) 0.0245(12) 0.0293(12) 0.0003(9) 0.0193(11) -0.0031(9)
C2 0.0402(14) 0.0299(13) 0.0292(12) 0.0050(10) 0.0227(11) -0.0030(10)
C3 0.0307(12) 0.0329(13) 0.0252(11) 0.0010(9) 0.0183(10) -0.0011(10)
C4 0.0213(10) 0.0263(11) 0.0206(10) -0.0001(8) 0.0116(9) 0.0000(8)
C5 0.0223(10) 0.0271(11) 0.0199(10) -0.0010(8) 0.0122(9) 0.0000(8)
C6 0.0234(11) 0.0233(11) 0.0223(10) -0.0013(8) 0.0120(9) 0.0004(8)
C7 0.0221(10) 0.0239(11) 0.0217(10) 0.0000(8) 0.0118(9) -0.0007(8)
C8 0.0332(13) 0.0258(12) 0.0280(11) -0.0015(9) 0.0188(10) -0.0053(10)
C9 0.0431(15) 0.0329(13) 0.0308(12) -0.0016(10) 0.0264(12) -0.0099(11)
C10 0.0401(14) 0.0323(13) 0.0286(12) -0.0050(10) 0.0246(11) -0.0059(11)
C11 0.0205(10) 0.0251(11) 0.0210(10) -0.0008(8) 0.0120(8) -0.0001(8)
C12 0.0213(10) 0.0244(11) 0.0202(10) 0.0001(8) 0.0112(8) 0.0002(8)
C13 0.0384(17) 0.070(2) 0.076(2) 0.0131(19) 0.0398(17) 0.0078(16)
C14 0.0273(12) 0.0444(16) 0.0410(15) -0.0016(12) 0.0218(12) 0.0020(11)
C15 0.0274(14) 0.0457(17) 0.0553(19) 0.0088(14) 0.0200(13) 0.0107(12)
C16 0.0306(13) 0.0316(13) 0.0317(13) 0.0004(10) 0.0118(11) 0.0050(10)
C17 0.0445(17) 0.0383(17) 0.0524(18) 0.0118(14) 0.0161(15) 0.0123(13)
C18 0.055(2) 0.054(2) 0.119(3) 0.027(2) 0.063(2) 0.0205(17)
C19 0.0353(14) 0.0385(15) 0.0444(15) 0.0075(12) 0.0282(13) 0.0103(11)
C20 0.0343(14) 0.0422(15) 0.0476(16) 0.0056(13) 0.0293(13) 0.0034(12)
C21 0.0321(13) 0.0294(13) 0.0331(13) -0.0061(10) 0.0196(11) -0.0054(10)
C22 0.0406(16) 0.0348(15) 0.069(2) 0.0043(14) 0.0320(16) -0.0052(12)
C23 0.0497(17) 0.0386(15) 0.0442(15) 0.0065(12) 0.0350(14) 0.0067(12)
C24 0.0287(12) 0.0320(13) 0.0291(12) -0.0007(10) 0.0187(10) -0.0001(10)
C25 0.0428(15) 0.0353(14) 0.0392(14) -0.0014(11) 0.0310(13) 0.0059(11)
C26 0.0341(13) 0.0288(13) 0.0390(14) -0.0065(10) 0.0231(12) 0.0014(10)
C27 0.066(2) 0.0331(15) 0.0556(18) 0.0005(13) 0.0433(17) 0.0108(14)
C28 0.0347(14) 0.0441(16) 0.0326(13) -0.0016(11) 0.0173(12) 0.0139(12)
C29 0.0290(13) 0.0495(17) 0.0407(14) -0.0021(12) 0.0214(12) 0.0081(12)
C30 0.0242(12) 0.0529(17) 0.0350(14) -0.0054(12) 0.0113(11) 0.0074(12)
C31 0.0328(14) 0.0585(19) 0.0285(13) 0.0030(12) 0.0108(11) 0.0180(13)
C32 0.0360(14) 0.0418(16) 0.0328(13) 0.0049(11) 0.0144(12) 0.0166(12)
C33 0.0361(14) 0.0322(14) 0.0304(13) -0.0080(11) 0.0111(11) 0.0043(11)
C34 0.0311(13) 0.0491(17) 0.0245(12) -0.0018(11) 0.0115(10) 0.0048(12)
C35 0.0260(12) 0.0337(14) 0.0275(12) 0.0016(10) 0.0077(10) 0.0025(10)
C36 0.0251(11) 0.0316(13) 0.0291(12) -0.0048(10) 0.0114(10) -0.0007(10)
C37 0.0310(13) 0.0295(13) 0.0310(13) -0.0037(10) 0.0120(11) -0.0028(10)
C38 0.0477(19) 0.066(2) 0.062(2) 0.0029(18) 0.0401(18) 0.0038(16)
C39 0.0297(15) 0.068(2) 0.057(2) -0.0210(18) 0.0161(14) -0.0041(15)
C40 0.055(2) 0.084(3) 0.0271(15) 0.0085(15) 0.0146(15) 0.0263(19)
C41 0.060(2) 0.0442(18) 0.054(2) 0.0149(15) 0.0265(17) 0.0212(16)
C42 0.0468(18) 0.094(3) 0.0272(14) 0.0033(16) 0.0182(14) 0.0149(19)
C43 0.0397(16) 0.0382(16) 0.0417(16) 0.0095(13) 0.0115(13) 0.0050(12)
C44 0.0308(14) 0.0484(18) 0.0528(18) -0.0099(14) 0.0232(14) 0.0011(12)
C45 0.0472(18) 0.0388(16) 0.0529(18) 0.0044(14) 0.0252(15) -0.0066(13)
F1A 0.091(5) 0.066(3) 0.157(7) -0.001(4) 0.098(5) -0.019(3)
F2A 0.121(6) 0.162(8) 0.110(5) -0.022(5) 0.102(5) -0.034(5)
F3A 0.036(3) 0.196(9) 0.170(7) 0.117(7) 0.056(4) 0.037(5)
_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
Gd1 O3 2.3686(19) . ?
Gd1 O4 2.3551(18) . ?
Gd1 O5 2.3847(18) . ?
Gd1 O6 2.3585(19) . ?
Gd1 O7 2.3668(17) . ?
Gd1 O8 2.3895(18) . ?
Gd1 N1 2.532(2) . ?
Gd1 N2 2.527(2) . ?
V1 O1 1.9869(18) . ?
V1 O2 1.9862(18) . ?
V1 C28 2.276(3) . ?
V1 C29 2.315(3) . ?
V1 C30 2.404(3) . ?
V1 C31 2.403(3) . ?
V1 C32 2.313(3) . ?
V1 C33 2.299(3) . ?
V1 C34 2.332(3) . ?
V1 C35 2.381(3) . ?
V1 C36 2.366(3) . ?
V1 C37 2.320(3) . ?
F1 C13 1.266(7) . ?
F2 C13 1.307(6) . ?
F3 C13 1.340(7) . ?
F4 C17 1.312(5) . ?
F5 C17 1.321(5) . ?
F6 C17 1.283(6) . ?
F7 C18 1.293(6) . ?
F8 C18 1.331(4) . ?
F9 C18 1.308(6) . ?
F10 C22 1.319(4) . ?
F11 C22 1.336(4) . ?
F12 C22 1.281(4) . ?
F13 C23 1.313(4) . ?
F14 C23 1.325(4) . ?
F15 C23 1.316(4) . ?
F16 C27 1.308(5) . ?
F17 C27 1.333(5) . ?
F18 C27 1.317(4) . ?
O1 C5 1.333(3) . ?
O2 C6 1.333(3) . ?
O3 C14 1.243(3) . ?
O4 C16 1.248(3) . ?
O5 C19 1.252(3) . ?
O6 C21 1.253(3) . ?
O7 C24 1.255(3) . ?
O8 C26 1.252(3) . ?
N1 C1 1.326(3) . ?
N1 C12 1.360(3) . ?
N2 C10 1.325(3) . ?
N2 C11 1.364(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.402(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.369(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.408(3) . ?
C4 C5 1.428(3) . ?
C4 C12 1.415(3) . ?
C5 C6 1.378(3) . ?
C6 C7 1.423(3) . ?
C7 C8 1.411(3) . ?
C7 C11 1.417(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.370(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.400(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.436(3) . ?
C13 C14 1.538(5) . ?
C13 F1A 1.321(7) . ?
C13 F2A 1.320(7) . ?
C13 F3A 1.256(6) . ?
C14 C15 1.385(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.393(5) . ?
C16 C17 1.532(4) . ?
C17 F4A 1.296(10) . ?
C17 F5A 1.227(12) . ?
C17 F6A 1.320(9) . ?
C18 C19 1.544(4) . ?
C19 C20 1.384(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.379(4) . ?
C21 C22 1.531(4) . ?
C23 C24 1.531(4) . ?
C24 C25 1.386(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.388(4) . ?
C26 C27 1.534(4) . ?
C27 F17A 1.246(11) . ?
C27 F16A 1.253(9) . ?
C27 F18A 1.288(13) . ?
C28 H28 0.9500 . ?
C28 C29 1.406(5) . ?
C28 C32 1.416(4) . ?
C29 C30 1.420(4) . ?
C29 C38 1.506(5) . ?
C30 C31 1.406(5) . ?
C30 C39 1.497(5) . ?
C31 C32 1.430(4) . ?
C31 C40 1.488(5) . ?
C32 C41 1.495(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.425(5) . ?
C33 C37 1.404(4) . ?
C34 C35 1.411(4) . ?
C34 C42 1.505(4) . ?
C35 C36 1.413(4) . ?
C35 C43 1.492(4) . ?
C36 C37 1.419(4) . ?
C36 C44 1.497(4) . ?
C37 C45 1.499(4) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 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
O3 Gd1 O5 142.02(7) . . ?
O3 Gd1 O8 77.39(7) . . ?
O3 Gd1 N1 106.11(7) . . ?
O3 Gd1 N2 72.51(7) . . ?
O4 Gd1 O3 72.07(7) . . ?
O4 Gd1 O5 142.99(7) . . ?
O4 Gd1 O6 77.87(7) . . ?
O4 Gd1 O7 138.31(6) . . ?
O4 Gd1 O8 74.99(7) . . ?
O4 Gd1 N1 74.03(7) . . ?
O4 Gd1 N2 114.30(7) . . ?
O5 Gd1 O8 118.33(7) . . ?
O5 Gd1 N1 80.32(7) . . ?
O5 Gd1 N2 76.94(7) . . ?
O6 Gd1 O3 146.31(7) . . ?
O6 Gd1 O5 71.38(7) . . ?
O6 Gd1 O7 120.19(7) . . ?
O6 Gd1 O8 80.49(7) . . ?
O6 Gd1 N1 79.21(7) . . ?
O6 Gd1 N2 135.71(7) . . ?
O7 Gd1 O3 76.29(7) . . ?
O7 Gd1 O5 76.72(6) . . ?
O7 Gd1 O8 72.14(6) . . ?
O7 Gd1 N1 142.05(6) . . ?
O7 Gd1 N2 80.11(6) . . ?
O8 Gd1 N1 145.80(7) . . ?
O8 Gd1 N2 142.97(7) . . ?
N2 Gd1 N1 65.42(7) . . ?
O1 V1 C28 119.92(10) . . ?
O1 V1 C29 84.74(10) . . ?
O1 V1 C30 77.05(10) . . ?
O1 V1 C31 104.26(10) . . ?
O1 V1 C32 135.36(10) . . ?
O1 V1 C33 134.57(9) . . ?
O1 V1 C34 100.69(10) . . ?
O1 V1 C35 77.47(8) . . ?
O1 V1 C36 91.71(9) . . ?
O1 V1 C37 126.89(9) . . ?
O2 V1 O1 82.07(7) . . ?
O2 V1 C28 132.93(9) . . ?
O2 V1 C29 127.83(9) . . ?
O2 V1 C30 92.89(9) . . ?
O2 V1 C31 76.86(9) . . ?
O2 V1 C32 98.31(9) . . ?
O2 V1 C33 117.95(10) . . ?
O2 V1 C34 135.87(9) . . ?
O2 V1 C35 106.74(9) . . ?
O2 V1 C36 77.78(9) . . ?
O2 V1 C37 83.41(9) . . ?
C28 V1 C29 35.66(11) . . ?
C28 V1 C30 58.07(11) . . ?
C28 V1 C31 58.25(10) . . ?
C28 V1 C32 35.93(11) . . ?
C28 V1 C33 77.62(11) . . ?
C28 V1 C34 83.97(10) . . ?
C28 V1 C35 118.02(10) . . ?
C28 V1 C36 135.43(10) . . ?
C28 V1 C37 107.12(11) . . ?
C29 V1 C30 34.95(10) . . ?
C29 V1 C31 58.11(11) . . ?
C29 V1 C34 96.13(11) . . ?
C29 V1 C35 119.11(11) . . ?
C29 V1 C36 153.01(10) . . ?
C29 V1 C37 140.99(11) . . ?
C31 V1 C30 34.02(12) . . ?
C32 V1 C29 59.75(12) . . ?
C32 V1 C30 58.31(12) . . ?
C32 V1 C31 35.24(11) . . ?
C32 V1 C34 108.64(11) . . ?
C32 V1 C35 141.78(10) . . ?
C32 V1 C36 132.29(11) . . ?
C32 V1 C37 97.19(11) . . ?
C33 V1 C29 107.03(11) . . ?
C33 V1 C30 135.59(11) . . ?
C33 V1 C31 119.40(11) . . ?
C33 V1 C32 84.69(11) . . ?
C33 V1 C34 35.83(11) . . ?
C33 V1 C35 58.24(10) . . ?
C33 V1 C36 58.01(10) . . ?
C33 V1 C37 35.38(11) . . ?
C34 V1 C30 130.92(11) . . ?
C34 V1 C31 141.53(11) . . ?
C34 V1 C35 34.82(10) . . ?
C34 V1 C36 58.19(10) . . ?
C35 V1 C30 145.11(11) . . ?
C35 V1 C31 176.27(11) . . ?
C36 V1 C30 166.39(10) . . ?
C36 V1 C31 147.67(11) . . ?
C36 V1 C35 34.62(10) . . ?
C37 V1 C30 154.55(11) . . ?
C37 V1 C31 121.46(12) . . ?
C37 V1 C34 59.54(11) . . ?
C37 V1 C35 58.69(10) . . ?
C37 V1 C36 35.23(9) . . ?
C5 O1 V1 111.29(15) . . ?
C6 O2 V1 111.37(15) . . ?
C14 O3 Gd1 134.2(2) . . ?
C16 O4 Gd1 134.00(19) . . ?
C19 O5 Gd1 134.55(18) . . ?
C21 O6 Gd1 135.01(17) . . ?
C24 O7 Gd1 133.35(17) . . ?
C26 O8 Gd1 131.82(18) . . ?
C1 N1 Gd1 122.90(17) . . ?
C1 N1 C12 118.6(2) . . ?
C12 N1 Gd1 118.39(15) . . ?
C10 N2 Gd1 122.97(16) . . ?
C10 N2 C11 118.6(2) . . ?
C11 N2 Gd1 118.37(15) . . ?
N1 C1 H1 118.5 . . ?
N1 C1 C2 123.0(2) . . ?
C2 C1 H1 118.5 . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.2(2) . . ?
C3 C2 H2 120.4 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.5(2) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C5 122.5(2) . . ?
C3 C4 C12 117.7(2) . . ?
C12 C4 C5 119.7(2) . . ?
O1 C5 C4 121.8(2) . . ?
O1 C5 C6 117.6(2) . . ?
C6 C5 C4 120.6(2) . . ?
O2 C6 C5 117.4(2) . . ?
O2 C6 C7 121.7(2) . . ?
C5 C6 C7 120.8(2) . . ?
C8 C7 C6 122.4(2) . . ?
C8 C7 C11 117.9(2) . . ?
C11 C7 C6 119.6(2) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.1(2) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 H9 120.3 . . ?
C8 C9 C10 119.4(2) . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 123.1(2) . . ?
N2 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
N2 C11 C7 121.8(2) . . ?
N2 C11 C12 118.5(2) . . ?
C7 C11 C12 119.6(2) . . ?
N1 C12 C4 122.0(2) . . ?
N1 C12 C11 118.4(2) . . ?
C4 C12 C11 119.5(2) . . ?
F1 C13 F2 109.0(7) . . ?
F1 C13 F3 109.8(8) . . ?
F1 C13 C14 114.3(4) . . ?
F2 C13 F3 102.2(5) . . ?
F2 C13 C14 111.3(4) . . ?
F3 C13 C14 109.5(4) . . ?
F1A C13 C14 111.1(4) . . ?
F2A C13 C14 108.5(4) . . ?
F2A C13 F1A 104.5(6) . . ?
F3A C13 C14 116.3(4) . . ?
F3A C13 F1A 107.3(8) . . ?
F3A C13 F2A 108.5(8) . . ?
O3 C14 C13 114.0(3) . . ?
O3 C14 C15 128.1(3) . . ?
C15 C14 C13 117.8(3) . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.8(3) . . ?
C16 C15 H15 119.6 . . ?
O4 C16 C15 127.8(3) . . ?
O4 C16 C17 113.7(3) . . ?
C15 C16 C17 118.5(3) . . ?
F4 C17 F5 101.5(4) . . ?
F4 C17 C16 111.7(3) . . ?
F5 C17 C16 113.4(3) . . ?
F6 C17 F4 106.0(5) . . ?
F6 C17 F5 111.4(5) . . ?
F6 C17 C16 112.2(3) . . ?
F4A C17 C16 112.0(6) . . ?
F4A C17 F6A 95.5(7) . . ?
F5A C17 C16 113.1(9) . . ?
F5A C17 F4A 112.8(11) . . ?
F5A C17 F6A 112.0(11) . . ?
F6A C17 C16 110.1(5) . . ?
F7 C18 F8 107.1(4) . . ?
F7 C18 F9 105.5(4) . . ?
F7 C18 C19 112.2(3) . . ?
F8 C18 C19 112.6(3) . . ?
F9 C18 F8 109.3(4) . . ?
F9 C18 C19 109.9(4) . . ?
O5 C19 C18 114.7(3) . . ?
O5 C19 C20 127.8(3) . . ?
C20 C19 C18 117.5(3) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 C19 121.1(3) . . ?
C21 C20 H20 119.4 . . ?
O6 C21 C20 127.6(3) . . ?
O6 C21 C22 114.7(3) . . ?
C20 C21 C22 117.7(3) . . ?
F10 C22 F11 104.5(3) . . ?
F10 C22 C21 110.6(3) . . ?
F11 C22 C21 113.4(3) . . ?
F12 C22 F10 109.5(4) . . ?
F12 C22 F11 108.2(3) . . ?
F12 C22 C21 110.4(3) . . ?
F13 C23 F14 106.1(3) . . ?
F13 C23 F15 106.4(3) . . ?
F13 C23 C24 112.3(2) . . ?
F14 C23 C24 113.1(3) . . ?
F15 C23 F14 108.0(3) . . ?
F15 C23 C24 110.6(3) . . ?
O7 C24 C23 114.0(2) . . ?
O7 C24 C25 128.1(3) . . ?
C25 C24 C23 117.9(2) . . ?
C24 C25 H25 119.3 . . ?
C24 C25 C26 121.4(2) . . ?
C26 C25 H25 119.3 . . ?
O8 C26 C25 127.8(3) . . ?
O8 C26 C27 115.1(3) . . ?
C25 C26 C27 117.1(3) . . ?
F16 C27 F17 109.2(5) . . ?
F16 C27 F18 104.2(4) . . ?
F16 C27 C26 111.3(3) . . ?
F17 C27 C26 111.7(3) . . ?
F18 C27 F17 106.8(4) . . ?
F18 C27 C26 113.2(3) . . ?
F17A C27 C26 111.8(7) . . ?
F17A C27 F16A 112.2(8) . . ?
F17A C27 F18A 111.3(11) . . ?
F16A C27 C26 113.8(6) . . ?
F16A C27 F18A 95.0(10) . . ?
F18A C27 C26 111.7(10) . . ?
V1 C28 H28 119.4 . . ?
C29 C28 V1 73.67(16) . . ?
C29 C28 H28 125.2 . . ?
C29 C28 C32 109.5(3) . . ?
C32 C28 V1 73.47(16) . . ?
C32 C28 H28 125.2 . . ?
C28 C29 V1 70.67(17) . . ?
C28 C29 C30 107.2(3) . . ?
C28 C29 C38 127.9(3) . . ?
C30 C29 V1 75.95(17) . . ?
C30 C29 C38 124.9(3) . . ?
C38 C29 V1 120.8(2) . . ?
C29 C30 V1 69.10(16) . . ?
C29 C30 C39 123.8(3) . . ?
C31 C30 V1 72.97(17) . . ?
C31 C30 C29 108.5(3) . . ?
C31 C30 C39 127.7(3) . . ?
C39 C30 V1 125.7(2) . . ?
C30 C31 V1 73.01(16) . . ?
C30 C31 C32 108.3(3) . . ?
C30 C31 C40 127.1(3) . . ?
C32 C31 V1 68.94(15) . . ?
C32 C31 C40 124.6(4) . . ?
C40 C31 V1 124.2(2) . . ?
C28 C32 V1 70.60(16) . . ?
C28 C32 C31 106.5(3) . . ?
C28 C32 C41 127.2(3) . . ?
C31 C32 V1 75.81(17) . . ?
C31 C32 C41 125.7(3) . . ?
C41 C32 V1 126.1(2) . . ?
V1 C33 H33 120.0 . . ?
C34 C33 V1 73.34(16) . . ?
C34 C33 H33 125.3 . . ?
C37 C33 V1 73.14(16) . . ?
C37 C33 H33 125.3 . . ?
C37 C33 C34 109.5(3) . . ?
C33 C34 V1 70.83(15) . . ?
C33 C34 C42 126.0(3) . . ?
C35 C34 V1 74.50(16) . . ?
C35 C34 C33 106.9(3) . . ?
C35 C34 C42 126.4(3) . . ?
C42 C34 V1 127.6(2) . . ?
C34 C35 V1 70.67(15) . . ?
C34 C35 C36 108.0(2) . . ?
C34 C35 C43 127.3(3) . . ?
C36 C35 V1 72.11(15) . . ?
C36 C35 C43 124.7(3) . . ?
C43 C35 V1 123.53(19) . . ?
C35 C36 V1 73.27(15) . . ?
C35 C36 C37 109.0(2) . . ?
C35 C36 C44 125.9(3) . . ?
C37 C36 V1 70.63(15) . . ?
C37 C36 C44 125.1(3) . . ?
C44 C36 V1 123.92(19) . . ?
C33 C37 V1 71.48(17) . . ?
C33 C37 C36 106.6(3) . . ?
C33 C37 C45 127.7(3) . . ?
C36 C37 V1 74.14(15) . . ?
C36 C37 C45 125.7(3) . . ?
C45 C37 V1 121.4(2) . . ?
C29 C38 H38A 109.5 . . ?
C29 C38 H38B 109.5 . . ?
C29 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C30 C39 H39A 109.5 . . ?
C30 C39 H39B 109.5 . . ?
C30 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C31 C40 H40A 109.5 . . ?
C31 C40 H40B 109.5 . . ?
C31 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C32 C41 H41A 109.5 . . ?
C32 C41 H41B 109.5 . . ?
C32 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C34 C42 H42A 109.5 . . ?
C34 C42 H42B 109.5 . . ?
C34 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C35 C43 H43A 109.5 . . ?
C35 C43 H43B 109.5 . . ?
C35 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C36 C44 H44A 109.5 . . ?
C36 C44 H44B 109.5 . . ?
C36 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C37 C45 H45A 109.5 . . ?
C37 C45 H45B 109.5 . . ?
C37 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
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
Gd1 O3 C14 C13 -171.7(2) . . . . ?
Gd1 O3 C14 C15 8.0(5) . . . . ?
Gd1 O4 C16 C15 -16.5(5) . . . . ?
Gd1 O4 C16 C17 163.7(2) . . . . ?
Gd1 O5 C19 C18 -171.4(3) . . . . ?
Gd1 O5 C19 C20 8.4(5) . . . . ?
Gd1 O6 C21 C20 -16.5(5) . . . . ?
Gd1 O6 C21 C22 162.4(2) . . . . ?
Gd1 O7 C24 C23 166.04(18) . . . . ?
Gd1 O7 C24 C25 -12.5(4) . . . . ?
Gd1 O8 C26 C25 22.8(5) . . . . ?
Gd1 O8 C26 C27 -158.4(2) . . . . ?
Gd1 N1 C1 C2 174.8(2) . . . . ?
Gd1 N1 C12 C4 -175.64(16) . . . . ?
Gd1 N1 C12 C11 7.1(3) . . . . ?
Gd1 N2 C10 C9 -174.3(2) . . . . ?
Gd1 N2 C11 C7 174.20(16) . . . . ?
Gd1 N2 C11 C12 -7.8(3) . . . . ?
V1 O1 C5 C4 176.92(17) . . . . ?
V1 O1 C5 C6 -3.4(3) . . . . ?
V1 O2 C6 C5 4.2(3) . . . . ?
V1 O2 C6 C7 -178.58(18) . . . . ?
V1 C28 C29 C30 67.8(2) . . . . ?
V1 C28 C29 C38 -114.5(3) . . . . ?
V1 C28 C32 C31 -68.0(2) . . . . ?
V1 C28 C32 C41 121.1(3) . . . . ?
V1 C29 C30 C31 62.7(2) . . . . ?
V1 C29 C30 C39 -119.8(3) . . . . ?
V1 C30 C31 C32 60.2(2) . . . . ?
V1 C30 C31 C40 -120.4(3) . . . . ?
V1 C31 C32 C28 64.41(19) . . . . ?
V1 C31 C32 C41 -124.5(3) . . . . ?
V1 C33 C34 C35 -66.33(19) . . . . ?
V1 C33 C34 C42 123.1(3) . . . . ?
V1 C33 C37 C36 66.40(18) . . . . ?
V1 C33 C37 C45 -115.8(3) . . . . ?
V1 C34 C35 C36 -62.85(19) . . . . ?
V1 C34 C35 C43 117.9(3) . . . . ?
V1 C35 C36 C37 -62.00(18) . . . . ?
V1 C35 C36 C44 120.1(3) . . . . ?
V1 C36 C37 C33 -64.59(19) . . . . ?
V1 C36 C37 C45 117.5(3) . . . . ?
F1 C13 C14 O3 10.7(9) . . . . ?
F1 C13 C14 C15 -169.1(9) . . . . ?
F2 C13 C14 O3 134.7(6) . . . . ?
F2 C13 C14 C15 -45.0(7) . . . . ?
F3 C13 C14 O3 -113.0(5) . . . . ?
F3 C13 C14 C15 67.2(6) . . . . ?
F7 C18 C19 O5 -57.1(5) . . . . ?
F7 C18 C19 C20 123.1(4) . . . . ?
F8 C18 C19 O5 -178.1(4) . . . . ?
F8 C18 C19 C20 2.1(6) . . . . ?
F9 C18 C19 O5 59.9(5) . . . . ?
F9 C18 C19 C20 -119.9(4) . . . . ?
F13 C23 C24 O7 42.4(4) . . . . ?
F13 C23 C24 C25 -138.9(3) . . . . ?
F14 C23 C24 O7 162.4(3) . . . . ?
F14 C23 C24 C25 -18.9(4) . . . . ?
F15 C23 C24 O7 -76.3(3) . . . . ?
F15 C23 C24 C25 102.4(3) . . . . ?
O1 C5 C6 O2 -0.6(3) . . . . ?
O1 C5 C6 C7 -177.8(2) . . . . ?
O2 C6 C7 C8 -1.1(4) . . . . ?
O2 C6 C7 C11 -179.1(2) . . . . ?
O3 C14 C15 C16 4.8(6) . . . . ?
O4 C16 C17 F4 -59.0(5) . . . . ?
O4 C16 C17 F5 -173.0(4) . . . . ?
O4 C16 C17 F6 59.8(6) . . . . ?
O4 C16 C17 F4A 21.1(7) . . . . ?
O4 C16 C17 F5A -107.8(12) . . . . ?
O4 C16 C17 F6A 126.1(6) . . . . ?
O5 C19 C20 C21 2.3(5) . . . . ?
O6 C21 C22 F10 68.1(4) . . . . ?
O6 C21 C22 F11 -174.9(3) . . . . ?
O6 C21 C22 F12 -53.3(4) . . . . ?
O7 C24 C25 C26 -3.3(5) . . . . ?
O8 C26 C27 F16 -94.9(5) . . . . ?
O8 C26 C27 F17 142.7(4) . . . . ?
O8 C26 C27 F18 22.1(5) . . . . ?
O8 C26 C27 F17A 54.5(8) . . . . ?
O8 C26 C27 F16A -177.2(6) . . . . ?
O8 C26 C27 F18A -71.0(10) . . . . ?
N1 C1 C2 C3 1.0(4) . . . . ?
N2 C11 C12 N1 0.4(3) . . . . ?
N2 C11 C12 C4 -176.9(2) . . . . ?
C1 N1 C12 C4 0.5(3) . . . . ?
C1 N1 C12 C11 -176.7(2) . . . . ?
C1 C2 C3 C4 -0.2(4) . . . . ?
C2 C3 C4 C5 178.3(2) . . . . ?
C2 C3 C4 C12 -0.4(4) . . . . ?
C3 C4 C5 O1 0.7(4) . . . . ?
C3 C4 C5 C6 -178.9(2) . . . . ?
C3 C4 C12 N1 0.2(3) . . . . ?
C3 C4 C12 C11 177.4(2) . . . . ?
C4 C5 C6 O2 179.1(2) . . . . ?
C4 C5 C6 C7 1.9(3) . . . . ?
C5 C4 C12 N1 -178.5(2) . . . . ?
C5 C4 C12 C11 -1.3(3) . . . . ?
C5 C6 C7 C8 176.0(2) . . . . ?
C5 C6 C7 C11 -2.0(3) . . . . ?
C6 C7 C8 C9 -176.4(2) . . . . ?
C6 C7 C11 N2 178.4(2) . . . . ?
C6 C7 C11 C12 0.4(3) . . . . ?
C7 C8 C9 C10 -1.9(4) . . . . ?
C7 C11 C12 N1 178.5(2) . . . . ?
C7 C11 C12 C4 1.2(3) . . . . ?
C8 C7 C11 N2 0.4(3) . . . . ?
C8 C7 C11 C12 -177.7(2) . . . . ?
C8 C9 C10 N2 0.2(4) . . . . ?
C10 N2 C11 C7 -2.0(3) . . . . ?
C10 N2 C11 C12 176.0(2) . . . . ?
C11 N2 C10 C9 1.8(4) . . . . ?
C11 C7 C8 C9 1.6(4) . . . . ?
C12 N1 C1 C2 -1.2(4) . . . . ?
C12 C4 C5 O1 179.4(2) . . . . ?
C12 C4 C5 C6 -0.2(3) . . . . ?
C13 C14 C15 C16 -175.5(3) . . . . ?
C14 C15 C16 O4 -0.6(5) . . . . ?
C14 C15 C16 C17 179.3(3) . . . . ?
C15 C16 C17 F4 121.1(4) . . . . ?
C15 C16 C17 F5 7.1(5) . . . . ?
C15 C16 C17 F6 -120.1(6) . . . . ?
C15 C16 C17 F4A -158.8(7) . . . . ?
C15 C16 C17 F5A 72.3(12) . . . . ?
C15 C16 C17 F6A -53.8(7) . . . . ?
C18 C19 C20 C21 -177.9(3) . . . . ?
C19 C20 C21 O6 1.5(5) . . . . ?
C19 C20 C21 C22 -177.3(3) . . . . ?
C20 C21 C22 F10 -112.9(3) . . . . ?
C20 C21 C22 F11 4.1(4) . . . . ?
C20 C21 C22 F12 125.7(4) . . . . ?
C23 C24 C25 C26 178.2(3) . . . . ?
C24 C25 C26 O8 -2.3(5) . . . . ?
C24 C25 C26 C27 178.9(3) . . . . ?
C25 C26 C27 F16 84.1(5) . . . . ?
C25 C26 C27 F17 -38.3(5) . . . . ?
C25 C26 C27 F18 -158.9(3) . . . . ?
C25 C26 C27 F17A -126.6(7) . . . . ?
C25 C26 C27 F16A 1.8(7) . . . . ?
C25 C26 C27 F18A 108.0(10) . . . . ?
C28 C29 C30 V1 -64.25(19) . . . . ?
C28 C29 C30 C31 -1.5(3) . . . . ?
C28 C29 C30 C39 176.0(3) . . . . ?
C29 C28 C32 V1 65.4(2) . . . . ?
C29 C28 C32 C31 -2.6(3) . . . . ?
C29 C28 C32 C41 -173.5(3) . . . . ?
C29 C30 C31 V1 -60.3(2) . . . . ?
C29 C30 C31 C32 -0.1(3) . . . . ?
C29 C30 C31 C40 179.3(3) . . . . ?
C30 C31 C32 V1 -62.8(2) . . . . ?
C30 C31 C32 C28 1.6(3) . . . . ?
C30 C31 C32 C41 172.7(3) . . . . ?
C32 C28 C29 V1 -65.3(2) . . . . ?
C32 C28 C29 C30 2.6(3) . . . . ?
C32 C28 C29 C38 -179.8(3) . . . . ?
C33 C34 C35 V1 63.86(18) . . . . ?
C33 C34 C35 C36 1.0(3) . . . . ?
C33 C34 C35 C43 -178.2(3) . . . . ?
C34 C33 C37 V1 -64.8(2) . . . . ?
C34 C33 C37 C36 1.6(3) . . . . ?
C34 C33 C37 C45 179.4(3) . . . . ?
C34 C35 C36 V1 61.93(19) . . . . ?
C34 C35 C36 C37 -0.1(3) . . . . ?
C34 C35 C36 C44 -178.0(3) . . . . ?
C35 C36 C37 V1 63.67(19) . . . . ?
C35 C36 C37 C33 -0.9(3) . . . . ?
C35 C36 C37 C45 -178.8(3) . . . . ?
C37 C33 C34 V1 64.72(19) . . . . ?
C37 C33 C34 C35 -1.6(3) . . . . ?
C37 C33 C34 C42 -172.2(3) . . . . ?
C38 C29 C30 V1 118.0(3) . . . . ?
C38 C29 C30 C31 -179.3(3) . . . . ?
C38 C29 C30 C39 -1.8(5) . . . . ?
C39 C30 C31 V1 122.4(3) . . . . ?
C39 C30 C31 C32 -177.4(3) . . . . ?
C39 C30 C31 C40 1.9(5) . . . . ?
C40 C31 C32 V1 117.8(3) . . . . ?
C40 C31 C32 C28 -177.7(3) . . . . ?
C40 C31 C32 C41 -6.7(5) . . . . ?
C42 C34 C35 V1 -125.6(3) . . . . ?
C42 C34 C35 C36 171.5(3) . . . . ?
C42 C34 C35 C43 -7.7(5) . . . . ?
C43 C35 C36 V1 -118.8(3) . . . . ?
C43 C35 C36 C37 179.2(3) . . . . ?
C43 C35 C36 C44 1.3(4) . . . . ?
C44 C36 C37 V1 -118.4(3) . . . . ?
C44 C36 C37 C33 177.0(3) . . . . ?
C44 C36 C37 C45 -0.9(4) . . . . ?
F1A C13 C14 O3 -40.0(6) . . . . ?
F1A C13 C14 C15 140.2(6) . . . . ?
F2A C13 C14 O3 74.4(7) . . . . ?
F2A C13 C14 C15 -105.4(7) . . . . ?
F3A C13 C14 O3 -163.1(9) . . . . ?
F3A C13 C14 C15 17.2(10) . . . . ?
_shelx_res_file
;
TITL mo_cb_gdv_cptet_150k_0m_a.res in C2/c
mo_cb_gdv_cptet_150k_0m.res
created by SHELXL-2016/6 at 12:36:05 on 27-Apr-2018
REM Old TITL mo_CB_GdV_cptet_150K_0m in C2/c
REM SHELXT solution in C2/c
REM R1 0.117, Rweak 0.004, Alpha 0.036, Orientation as input
REM Formula found by SHELXT: C49 N2 O6 F17 V Gd
CELL 0.71073 31.3529 14.8019 25.6961 90 124.668 90
ZERR 8 0.0021 0.0009 0.0015 0 0.002 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H F Gd N O V
UNIT 360 280 144 8 16 64 8
SADI F4A C17 F6 C17 F4 C17 F6A C17 F5A C17 F5 C17
SADI F1A C13 F1 C13 F3 C13 F3A C13 F2 C13 F2A C13
SADI F17A C27 F16A C27 F18A C27 F17 C27 F16 C27 F18 C27
RIGU
ISOR 0.01 0.02 $f
L.S. 20 0 0
PLAN 20
SIZE 0.02 0.13 0.26
TEMP -123.15
conf
BOND $H
list 4
fmap 2 53
acta
OMIT -9 5 7
OMIT 2 0 26
OMIT -23 3 33
OMIT -17 5 31
REM
REM
REM
WGHT 0.040300 27.398899
FVAR 0.11282
GD1 4 0.644719 0.443523 0.684925 11.00000 0.02304 0.02192 =
0.02427 -0.00063 0.01466 0.00211
V1 7 0.622919 0.012838 0.455125 11.00000 0.02606 0.02614 =
0.02242 -0.00192 0.01292 0.00440
PART 1
F1 3 0.492397 0.360261 0.678541 10.50000 0.06607 0.16142 =
0.16563 0.10398 0.08515 0.04068
F2 3 0.453869 0.484687 0.648272 10.50000 0.07044 0.11021 =
0.13416 -0.03562 0.08474 -0.00952
F3 3 0.437924 0.389895 0.580702 10.50000 0.06313 0.11152 =
0.11817 -0.05015 0.06545 -0.04811
F4 3 0.560599 0.725748 0.574620 10.75000 0.06075 0.04141 =
0.09751 0.02488 0.01715 -0.00813
F5 3 0.483824 0.695215 0.528618 10.75000 0.04807 0.06651 =
0.20220 0.07445 0.05184 0.03215
F6 3 0.528159 0.645941 0.494396 10.75000 0.35191 0.05550 =
0.06594 0.02491 0.11764 0.04255
PART 0
F7 3 0.823621 0.296615 0.824066 11.00000 0.06334 0.10511 =
0.12057 0.06829 0.03891 0.03950
F8 3 0.853680 0.344060 0.773536 11.00000 0.06691 0.08797 =
0.22063 0.06229 0.09967 0.03735
F9 3 0.792194 0.245921 0.734133 11.00000 0.11568 0.06082 =
0.17263 0.00294 0.09760 0.03568
F10 3 0.768119 0.697610 0.709004 11.00000 0.11406 0.03625 =
0.20374 -0.03191 0.12586 -0.02259
F11 3 0.804102 0.617564 0.677025 11.00000 0.06139 0.05382 =
0.07868 0.00678 0.05310 -0.00431
F12 3 0.723720 0.646023 0.615210 11.00000 0.06472 0.13103 =
0.11034 0.08766 0.00320 -0.03158
F13 3 0.700207 0.296094 0.889270 11.00000 0.06694 0.05732 =
0.06133 0.02803 0.04457 0.02571
F14 3 0.659101 0.377083 0.914118 11.00000 0.17606 0.06525 =
0.07903 0.02703 0.10493 0.04615
F15 3 0.619116 0.282685 0.837981 11.00000 0.07419 0.09209 =
0.08446 0.03375 0.03084 -0.03432
PART 1
F16 3 0.638553 0.706771 0.828515 10.75000 0.12939 0.04360 =
0.06357 -0.02963 0.00670 0.03051
F17 3 0.565340 0.642527 0.793702 10.75000 0.14679 0.04312 =
0.27442 0.01282 0.18556 0.02388
F18 3 0.581305 0.705887 0.732247 10.75000 0.06390 0.04017 =
0.06240 0.00909 0.03587 0.02690
PART 0
O1 6 0.629834 0.146522 0.459164 11.00000 0.03320 0.02821 =
0.02446 -0.00265 0.01925 0.00011
O2 6 0.615077 0.033964 0.525606 11.00000 0.03413 0.02205 =
0.02633 -0.00146 0.01821 0.00000
O3 6 0.560720 0.418046 0.660918 11.00000 0.02587 0.03925 =
0.03916 0.00432 0.01979 0.00351
O4 6 0.587319 0.545159 0.604412 11.00000 0.03094 0.03258 =
0.03421 0.00616 0.01860 0.00718
O5 6 0.727938 0.374749 0.734372 11.00000 0.02992 0.03303 =
0.03891 0.00757 0.02282 0.00703
O6 6 0.702139 0.548919 0.687116 11.00000 0.03052 0.02523 =
0.04453 -0.00314 0.02195 -0.00083
O7 6 0.660896 0.386143 0.780577 11.00000 0.03225 0.02777 =
0.02738 -0.00006 0.01886 0.00493
O8 6 0.634932 0.565064 0.738538 11.00000 0.04790 0.02720 =
0.03902 -0.00247 0.03029 0.00296
N1 5 0.640845 0.396409 0.587574 11.00000 0.02804 0.02351 =
0.02410 0.00083 0.01518 -0.00005
N2 5 0.623068 0.278918 0.655386 11.00000 0.02956 0.02845 =
0.02417 -0.00288 0.01798 -0.00241
C1 1 0.646749 0.454240 0.552692 11.00000 0.03516 0.02445 =
0.02934 0.00028 0.01933 -0.00308
AFIX 43
H1 2 0.649789 0.516729 0.562665 11.00000 -1.20000
AFIX 0
C2 1 0.648707 0.427357 0.501782 11.00000 0.04018 0.02988 =
0.02917 0.00504 0.02272 -0.00298
AFIX 43
H2 2 0.653546 0.470826 0.478377 11.00000 -1.20000
AFIX 0
C3 1 0.643562 0.337704 0.486200 11.00000 0.03068 0.03287 =
0.02517 0.00103 0.01834 -0.00112
AFIX 43
H3 2 0.644689 0.318369 0.451747 11.00000 -1.20000
AFIX 0
C4 1 0.636588 0.274384 0.521635 11.00000 0.02127 0.02633 =
0.02055 -0.00007 0.01163 0.00005
C5 1 0.629597 0.180201 0.507092 11.00000 0.02230 0.02710 =
0.01988 -0.00098 0.01217 0.00002
C6 1 0.622045 0.120763 0.542402 11.00000 0.02344 0.02333 =
0.02234 -0.00134 0.01196 0.00038
C7 1 0.619484 0.152149 0.592925 11.00000 0.02210 0.02390 =
0.02165 0.00000 0.01180 -0.00072
C8 1 0.608622 0.094122 0.627559 11.00000 0.03325 0.02583 =
0.02803 -0.00152 0.01880 -0.00525
AFIX 43
H8 2 0.604618 0.031028 0.619327 11.00000 -1.20000
AFIX 0
C9 1 0.603927 0.130002 0.673232 11.00000 0.04312 0.03289 =
0.03077 -0.00165 0.02635 -0.00987
AFIX 43
H9 2 0.595591 0.092251 0.696151 11.00000 -1.20000
AFIX 0
C10 1 0.611525 0.222802 0.685821 11.00000 0.04009 0.03233 =
0.02860 -0.00500 0.02458 -0.00590
AFIX 43
H10 2 0.608245 0.246654 0.717709 11.00000 -1.20000
AFIX 0
C11 1 0.626387 0.245281 0.608391 11.00000 0.02052 0.02511 =
0.02101 -0.00081 0.01203 -0.00013
C12 1 0.635548 0.307072 0.572663 11.00000 0.02125 0.02445 =
0.02017 0.00011 0.01118 0.00021
C13 1 0.476810 0.421509 0.637115 11.00000 0.03839 0.06984 =
0.07622 0.01306 0.03976 0.00784
C14 1 0.519339 0.461104 0.631398 11.00000 0.02726 0.04436 =
0.04105 -0.00162 0.02176 0.00204
C15 1 0.507748 0.538441 0.595333 11.00000 0.02744 0.04568 =
0.05530 0.00877 0.02000 0.01075
AFIX 43
H15 2 0.475257 0.567447 0.577738 11.00000 -1.20000
AFIX 0
C16 1 0.543174 0.574182 0.584562 11.00000 0.03057 0.03158 =
0.03169 0.00038 0.01183 0.00495
C17 1 0.528020 0.659219 0.543649 11.00000 0.04453 0.03828 =
0.05236 0.01176 0.01609 0.01233
C18 1 0.810503 0.319480 0.768205 11.00000 0.05464 0.05354 =
0.11949 0.02743 0.06281 0.02054
C19 1 0.768675 0.394129 0.738616 11.00000 0.03530 0.03847 =
0.04441 0.00745 0.02816 0.01032
C20 1 0.779961 0.473100 0.719943 11.00000 0.03430 0.04216 =
0.04757 0.00558 0.02933 0.00338
AFIX 43
H20 2 0.812077 0.478466 0.724384 11.00000 -1.20000
AFIX 0
C21 1 0.745371 0.544144 0.694995 11.00000 0.03212 0.02937 =
0.03313 -0.00612 0.01961 -0.00544
C22 1 0.759849 0.627361 0.672780 11.00000 0.04060 0.03483 =
0.06865 0.00429 0.03202 -0.00521
C23 1 0.657081 0.342038 0.865329 11.00000 0.04970 0.03863 =
0.04419 0.00648 0.03498 0.00673
C24 1 0.649606 0.413234 0.817591 11.00000 0.02868 0.03197 =
0.02909 -0.00069 0.01866 -0.00006
C25 1 0.630708 0.497164 0.819109 11.00000 0.04285 0.03532 =
0.03919 -0.00140 0.03097 0.00595
AFIX 43
H25 2 0.622048 0.507667 0.848521 11.00000 -1.20000
AFIX 0
C26 1 0.624165 0.566185 0.778587 11.00000 0.03407 0.02879 =
0.03898 -0.00645 0.02306 0.00138
C27 1 0.602082 0.655748 0.783500 11.00000 0.06605 0.03311 =
0.05563 0.00055 0.04329 0.01077
C28 1 0.678304 -0.073694 0.445890 11.00000 0.03469 0.04409 =
0.03259 -0.00163 0.01730 0.01391
AFIX 43
H28 2 0.665536 -0.105563 0.407606 11.00000 -1.20000
AFIX 0
C29 1 0.698533 0.014531 0.459057 11.00000 0.02902 0.04945 =
0.04070 -0.00208 0.02144 0.00807
C30 1 0.715233 0.034925 0.521964 11.00000 0.02424 0.05290 =
0.03501 -0.00541 0.01125 0.00738
C31 1 0.704012 -0.039448 0.546313 11.00000 0.03284 0.05845 =
0.02847 0.00304 0.01083 0.01797
C32 1 0.679896 -0.107710 0.498475 11.00000 0.03596 0.04181 =
0.03284 0.00486 0.01435 0.01657
C33 1 0.567762 -0.088623 0.377784 11.00000 0.03614 0.03221 =
0.03038 -0.00796 0.01105 0.00433
AFIX 43
H33 2 0.580394 -0.145829 0.375585 11.00000 -1.20000
AFIX 0
C34 1 0.566908 -0.008911 0.346120 11.00000 0.03105 0.04909 =
0.02449 -0.00180 0.01151 0.00477
C35 1 0.543921 0.059611 0.360590 11.00000 0.02603 0.03368 =
0.02749 0.00160 0.00770 0.00252
C36 1 0.531816 0.022524 0.401368 11.00000 0.02509 0.03162 =
0.02909 -0.00475 0.01138 -0.00068
C37 1 0.547054 -0.069570 0.412737 11.00000 0.03098 0.02954 =
0.03103 -0.00374 0.01199 -0.00276
C38 1 0.704209 0.076578 0.416880 11.00000 0.04774 0.06616 =
0.06172 0.00290 0.04005 0.00379
AFIX 137
H38A 2 0.688183 0.048655 0.375144 11.00000 -1.50000
H38B 2 0.741096 0.087229 0.435648 11.00000 -1.50000
H38C 2 0.687043 0.134215 0.412409 11.00000 -1.50000
AFIX 0
C39 1 0.742261 0.120708 0.555404 11.00000 0.02970 0.06771 =
0.05702 -0.02095 0.01613 -0.00407
AFIX 137
H39A 2 0.725105 0.171893 0.526504 11.00000 -1.50000
H39B 2 0.778541 0.117827 0.569350 11.00000 -1.50000
H39C 2 0.740832 0.128570 0.592254 11.00000 -1.50000
AFIX 0
C40 1 0.715261 -0.048396 0.610696 11.00000 0.05526 0.08405 =
0.02709 0.00853 0.01461 0.02632
AFIX 137
H40A 2 0.737455 -0.101189 0.631900 11.00000 -1.50000
H40B 2 0.682679 -0.055952 0.607225 11.00000 -1.50000
H40C 2 0.733057 0.006062 0.635356 11.00000 -1.50000
AFIX 0
C41 1 0.667157 -0.201476 0.507119 11.00000 0.06019 0.04421 =
0.05418 0.01492 0.02652 0.02120
AFIX 137
H41A 2 0.654014 -0.199732 0.533768 11.00000 -1.50000
H41B 2 0.698466 -0.238930 0.527486 11.00000 -1.50000
H41C 2 0.640641 -0.227217 0.465768 11.00000 -1.50000
AFIX 0
C42 1 0.579651 -0.003453 0.297886 11.00000 0.04684 0.09393 =
0.02723 0.00329 0.01819 0.01489
AFIX 137
H42A 2 0.593846 0.056390 0.299782 11.00000 -1.50000
H42B 2 0.548083 -0.013341 0.255519 11.00000 -1.50000
H42C 2 0.605321 -0.049853 0.306955 11.00000 -1.50000
AFIX 0
C43 1 0.533033 0.154693 0.337179 11.00000 0.03967 0.03819 =
0.04165 0.00954 0.01152 0.00499
AFIX 137
H43A 2 0.544104 0.195866 0.372587 11.00000 -1.50000
H43B 2 0.495761 0.162054 0.305184 11.00000 -1.50000
H43C 2 0.552082 0.168620 0.318388 11.00000 -1.50000
AFIX 0
C44 1 0.505404 0.070941 0.426771 11.00000 0.03083 0.04840 =
0.05276 -0.00993 0.02323 0.00112
AFIX 137
H44A 2 0.511686 0.038538 0.463787 11.00000 -1.50000
H44B 2 0.468030 0.073537 0.394080 11.00000 -1.50000
H44C 2 0.519204 0.132447 0.439080 11.00000 -1.50000
AFIX 0
C45 1 0.540052 -0.133497 0.452597 11.00000 0.04724 0.03876 =
0.05285 0.00442 0.02522 -0.00657
AFIX 137
H45A 2 0.554490 -0.192630 0.453433 11.00000 -1.50000
H45B 2 0.503017 -0.139852 0.434628 11.00000 -1.50000
H45C 2 0.558073 -0.109791 0.495779 11.00000 -1.50000
AFIX 0
PART 2
F1A 3 0.476496 0.332330 0.634687 10.50000 0.09090 0.06586 =
0.15735 -0.00099 0.09764 -0.01918
F2A 3 0.488493 0.440157 0.694084 10.50000 0.12070 0.16221 =
0.11002 -0.02193 0.10166 -0.03357
F3A 3 0.431325 0.447854 0.596881 10.50000 0.03622 0.19621 =
0.16959 0.11662 0.05573 0.03714
F4A 3 0.555112 0.668408 0.520310 10.25000 0.07175
F5A 3 0.527734 0.727659 0.570370 10.25000 0.12552
F6A 3 0.483313 0.646622 0.488701 10.25000 0.06286
F17A 3 0.563459 0.680336 0.731238 10.25000 0.07468
F16A 3 0.593689 0.656292 0.825703 10.25000 0.05220
F18A 3 0.636891 0.718079 0.809083 10.25000 0.09730
HKLF 4
REM mo_cb_gdv_cptet_150k_0m_a.res in C2/c
REM R1 = 0.0309 for 10891 Fo > 4sig(Fo) and 0.0353 for all 12106 data
REM 735 parameters refined using 1083 restraints
END
WGHT 0.0403 27.4127
REM Highest difference peak 2.060, deepest hole -0.491, 1-sigma level 0.083
Q1 1 0.5814 0.0763 0.7180 11.00000 0.05 2.06
Q2 1 0.6195 0.4297 0.6790 11.00000 0.05 0.87
Q3 1 0.5604 0.6977 0.5422 11.00000 0.05 0.82
Q4 1 0.8038 0.2820 0.6947 11.00000 0.05 0.81
Q5 1 0.8189 0.3059 0.7132 11.00000 0.05 0.80
Q6 1 0.7365 0.7009 0.6620 11.00000 0.05 0.77
Q7 1 0.4994 0.7052 0.5615 11.00000 0.05 0.68
Q8 1 0.5403 0.6377 0.7367 11.00000 0.05 0.68
Q9 1 0.7595 0.2141 0.7161 11.00000 0.05 0.65
Q10 1 0.7406 0.6137 0.6019 11.00000 0.05 0.59
Q11 1 0.6781 0.4264 0.7006 11.00000 0.05 0.59
Q12 1 0.6774 0.5210 0.4840 11.00000 0.05 0.52
Q13 1 0.6202 0.6632 0.8447 11.00000 0.05 0.50
Q14 1 0.4886 0.6145 0.4760 11.00000 0.05 0.48
Q15 1 0.7779 0.6174 0.6399 11.00000 0.05 0.47
Q16 1 0.6243 0.3503 0.8762 11.00000 0.05 0.42
Q17 1 0.8009 0.6611 0.6999 11.00000 0.05 0.41
Q18 1 0.6174 0.7221 0.7748 11.00000 0.05 0.37
Q19 1 0.6396 0.2244 0.5196 11.00000 0.05 0.36
Q20 1 0.6798 0.3782 0.9191 11.00000 0.05 0.35
;
_shelx_res_checksum 1267
#######################################################################
#
# 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_1b
_database_code_depnum_ccdc_archive 'CCDC 1832430'
_audit_update_record
;
2018-03-26 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;
# mo_jhgla020_r1_0m [
# Y(hfac)3(N,N'-pd)]Tol
_audit_creation_date 2018-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2016/6
# start Validation Reply Form
_vrf_PLAT430_mo_jhgla020_r1_0m
;
PROBLEM: Short Inter D...A Contact O2 ..O4 2.83 Ang.
RESPONSE: Both oxygen positions are well determined, the distance
is likely a consequence of the O2 (dp oxygen) pointing towards the
Y (distance 3.155 angstrom).
;
# end Validation Reply Form
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C27 H9 F18 N2 O8 Y, C7 H8'
_chemical_formula_sum 'C34 H17 F18 N2 O8 Y'
_chemical_formula_weight 1012.41
_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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 12.9792(9)
_cell_length_b 16.4628(13)
_cell_length_c 17.8859(13)
_cell_angle_alpha 90
_cell_angle_beta 103.679(3)
_cell_angle_gamma 90
_cell_volume 3713.3(5)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9995
_cell_measurement_temperature 100
_cell_measurement_theta_max 27.485
_cell_measurement_theta_min 2.474
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.716
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.5704
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1250 before and 0.0517 after correction. The Ratio of minimum to maximum transmission is 0.7650. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.811
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 2000
_exptl_crystal_size_max 0.27
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.01
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0321
_diffrn_reflns_av_unetI/netI 0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 31693
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.480
_diffrn_reflns_theta_min 2.344
_diffrn_ambient_temperature 100
_diffrn_detector 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type 'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 VENTURE'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_collimation 'focusing mirrors'
_diffrn_radiation_monochromator 'multilayer mirror optics'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed tube'
_diffrn_source_type 'INCOATEC I\ms 3.0'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6690
_reflns_number_total 8274
_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 v8.37A (Bruker, 2015)'
_computing_data_collection 'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'XT (Sheldrick, 2015)'
_refine_diff_density_max 0.833
_refine_diff_density_min -0.872
_refine_diff_density_rms 0.093
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.068
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 617
_refine_ls_number_reflns 8274
_refine_ls_number_restraints 30
_refine_ls_R_factor_all 0.0661
_refine_ls_R_factor_gt 0.0510
_refine_ls_restrained_S_all 1.083
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+10.0430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1365
_refine_ls_wR_factor_ref 0.1437
_refine_special_details
;
There is disorder present in a number of the CF3 groups. In most cases
the F are modelled over 2 different positions with occupancy 0.8/0.2
and distance restraints applied. In one case the C atom is also disordered
and one of the F atoms is common to both orientations.
;
_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. Restrained distances
F3-C13 = F2A-C13 = F2-C13 = F3A-C13 = F1A-C13 = F1-C13 = F15A-C23 = F13A-C23 =
F14A-C23 = F14-C23 = F13-C23 = F15-C23 = F16-C27A = F16-C27 = F18-C27 = F17A-
C27A = F17-C27 = F18A-C27A = F9-C18 = F8A-C18 = F8-C18 = F7A-C18 = F7-C18 =
F9A-C18
1.336 with sigma of 0.02
F14A-F15A \\sim F15-F13 \\sim F13A-F15A \\sim F13-F14
with sigma of 0.02
3. Others
Fixed Sof: F1(0.8) F2(0.8) F3(0.8) F7(0.8) F8(0.8) F9(0.8) F13(0.8) F14(0.8)
F15(0.8) F17(0.8) F18(0.8) C27(0.8) F1A(0.2) F2A(0.2) F3A(0.2) F7A(0.2)
F8A(0.2) F9A(0.2) F13A(0.2) F14A(0.2) F15A(0.2) F17A(0.2) F18A(0.2) C27A(0.2)
4.a Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C15(H15), C20(H20),
C25(H25), C3T(H3T), C4T(H4T), C5T(H5T), C6T(H6T), C7T(H7T)
4.b Idealised Me refined as rotating group:
C1T(H1TA,H1TB,H1TC)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.30112(3) 0.76542(2) 0.25659(2) 0.02152(11) Uani 1 1 d . . . . .
F1 F 0.4761(4) 0.6703(3) 0.5145(2) 0.0550(10) Uani 0.8 1 d D . P A 1
F2 F 0.5400(4) 0.7895(2) 0.5291(2) 0.0466(10) Uani 0.8 1 d D . P A 1
F3 F 0.6385(3) 0.6893(3) 0.51436(18) 0.0542(10) Uani 0.8 1 d D . P A 1
F4 F 0.6139(2) 0.64195(16) 0.19527(17) 0.0462(7) Uani 1 1 d . . . . .
F5 F 0.73836(18) 0.69528(16) 0.28244(15) 0.0406(6) Uani 1 1 d . . . . .
F6 F 0.65151(19) 0.76819(15) 0.18917(15) 0.0384(6) Uani 1 1 d . . . . .
F7 F 0.3042(4) 0.9288(2) 0.0331(2) 0.0537(11) Uani 0.8 1 d D . P B 1
F8 F 0.3275(4) 1.0419(3) 0.0912(2) 0.0688(14) Uani 0.8 1 d D . P B 1
F9 F 0.1711(3) 0.9998(3) 0.0422(2) 0.0590(11) Uani 0.8 1 d D . P B 1
F10 F 0.1331(2) 1.07266(16) 0.30314(17) 0.0521(7) Uani 1 1 d . . . . .
F11 F 0.2750(2) 1.03930(15) 0.38648(15) 0.0443(6) Uani 1 1 d . . . . .
F12 F 0.1317(2) 0.97091(16) 0.37863(15) 0.0451(7) Uani 1 1 d . . . . .
F13 F 0.0401(3) 0.7663(2) 0.4324(2) 0.0552(10) Uani 0.8 1 d D . P C 1
F14 F 0.1124(3) 0.6516(2) 0.43760(19) 0.0484(9) Uani 0.8 1 d D . P C 1
F15 F -0.0500(3) 0.6640(5) 0.3738(3) 0.0533(14) Uani 0.8 1 d D . P C 1
F16 F -0.1446(2) 0.7873(2) 0.12680(17) 0.0591(9) Uani 1 1 d D . . . .
F17 F -0.0310(3) 0.8414(3) 0.0754(2) 0.0467(9) Uani 0.8 1 d D . P D 1
F18 F -0.0546(3) 0.7129(2) 0.06681(19) 0.0504(9) Uani 0.8 1 d D . P D 1
O1 O 0.4396(3) 0.44834(19) 0.04281(19) 0.0448(8) Uani 1 1 d . . . . .
O2 O 0.5270(3) 0.40232(17) 0.19070(19) 0.0423(7) Uani 1 1 d . . . . .
O3 O 0.4129(2) 0.75408(15) 0.37997(15) 0.0252(5) Uani 1 1 d . . . . .
O4 O 0.4707(2) 0.74847(15) 0.23865(16) 0.0267(6) Uani 1 1 d . . . . .
O5 O 0.3056(2) 0.86598(15) 0.16569(15) 0.0265(6) Uani 1 1 d . . . . .
O6 O 0.2505(2) 0.88271(15) 0.30782(15) 0.0273(6) Uani 1 1 d . . . . .
O7 O 0.1837(2) 0.72058(16) 0.32827(16) 0.0283(6) Uani 1 1 d . . . . .
O8 O 0.1296(2) 0.77474(17) 0.17825(16) 0.0295(6) Uani 1 1 d . . . . .
N1 N 0.2955(2) 0.68159(18) 0.13912(17) 0.0241(6) Uani 1 1 d . . . . .
N2 N 0.3383(3) 0.61410(19) 0.27933(19) 0.0265(7) Uani 1 1 d . . . . .
C1 C 0.2649(3) 0.7128(2) 0.0678(2) 0.0291(8) Uani 1 1 d . . . . .
H1 H 0.227852 0.761616 0.061582 0.035 Uiso 1 1 calc R . . . .
C2 C 0.2853(3) 0.6761(2) 0.0032(2) 0.0299(8) Uani 1 1 d . . . . .
H2 H 0.262036 0.699652 -0.045119 0.036 Uiso 1 1 calc R . . . .
C3 C 0.3408(3) 0.6041(2) 0.0119(2) 0.0308(8) Uani 1 1 d . . . . .
H3 H 0.357923 0.579170 -0.030184 0.037 Uiso 1 1 calc R . . . .
C4 C 0.3708(3) 0.5695(2) 0.0842(2) 0.0276(8) Uani 1 1 d . . . . .
C5 C 0.4261(3) 0.4896(2) 0.0958(2) 0.0321(9) Uani 1 1 d . . . . .
C6 C 0.4646(3) 0.4586(2) 0.1779(2) 0.0309(8) Uani 1 1 d . . . . .
C7 C 0.4247(3) 0.4990(2) 0.2392(2) 0.0284(8) Uani 1 1 d . . . . .
C8 C 0.4394(3) 0.4646(2) 0.3117(3) 0.0351(9) Uani 1 1 d . . . . .
H8 H 0.475059 0.415531 0.322980 0.042 Uiso 1 1 calc R . . . .
C9 C 0.4001(4) 0.5045(2) 0.3669(3) 0.0363(9) Uani 1 1 d . . . . .
H9 H 0.406289 0.481864 0.415398 0.044 Uiso 1 1 calc R . . . .
C10 C 0.3511(3) 0.5795(2) 0.3484(2) 0.0310(8) Uani 1 1 d . . . . .
H10 H 0.326040 0.606793 0.386061 0.037 Uiso 1 1 calc R . . . .
C11 C 0.3714(3) 0.5734(2) 0.2245(2) 0.0251(7) Uani 1 1 d . . . . .
C12 C 0.3467(3) 0.6096(2) 0.1466(2) 0.0232(7) Uani 1 1 d . . . . .
C13 C 0.5441(3) 0.7226(2) 0.4912(2) 0.0333(9) Uani 1 1 d D . . . .
C14 C 0.5087(3) 0.7350(2) 0.4044(2) 0.0278(8) Uani 1 1 d . . . . .
C15 C 0.5836(3) 0.7211(2) 0.3614(2) 0.0294(8) Uani 1 1 d . . . . .
H15 H 0.652186 0.706332 0.386441 0.035 Uiso 1 1 calc R . . . .
C16 C 0.5577(3) 0.7289(2) 0.2817(2) 0.0241(7) Uani 1 1 d . . . . .
C17 C 0.6419(3) 0.7086(2) 0.2372(2) 0.0302(8) Uani 1 1 d . . . . .
C18 C 0.2675(3) 0.9769(2) 0.0796(2) 0.0314(9) Uani 1 1 d D . . . .
C19 C 0.2656(3) 0.9358(2) 0.1565(2) 0.0262(8) Uani 1 1 d . . . . .
C20 C 0.2232(3) 0.9809(2) 0.2076(2) 0.0301(8) Uani 1 1 d . . . . .
H20 H 0.194696 1.031912 0.192905 0.036 Uiso 1 1 calc R . . . .
C21 C 0.2226(3) 0.9516(2) 0.2801(2) 0.0274(8) Uani 1 1 d . . . . .
C22 C 0.1888(4) 1.0096(2) 0.3373(3) 0.0365(10) Uani 1 1 d . . . . .
C23 C 0.0457(4) 0.6962(3) 0.3895(3) 0.0497(12) Uani 1 1 d D . . . .
C24 C 0.0846(3) 0.7207(2) 0.3189(2) 0.0299(8) Uani 1 1 d . . . . .
C25 C 0.0087(3) 0.7414(3) 0.2539(3) 0.0346(9) Uani 1 1 d . . . . .
H25 H -0.062633 0.739470 0.254621 0.041 Uiso 1 1 calc R . . . .
C26 C 0.0376(3) 0.7653(3) 0.1870(2) 0.0301(8) Uani 1 1 d . . . . .
C27 C -0.0503(4) 0.7760(3) 0.1140(3) 0.0298(11) Uani 0.8 1 d D . P D 1
F1A F 0.5282(17) 0.6506(10) 0.5117(12) 0.069(6) Uiso 0.2 1 d D . P A 2
F2A F 0.6490(12) 0.7411(12) 0.5166(11) 0.065(5) Uiso 0.2 1 d D . P A 2
F3A F 0.5018(17) 0.7717(12) 0.5323(13) 0.063(7) Uiso 0.2 1 d D . P A 2
F7A F 0.2405(18) 0.9262(12) 0.0229(11) 0.077(7) Uiso 0.2 1 d D . P B 2
F8A F 0.2162(14) 1.0459(9) 0.0659(10) 0.061(4) Uiso 0.2 1 d D . P B 2
F9A F 0.3666(11) 0.9961(12) 0.0747(11) 0.064(5) Uiso 0.2 1 d D . P B 2
F13A F 0.0915(13) 0.7069(12) 0.4535(8) 0.062(4) Uiso 0.2 1 d D . P C 2
F14A F 0.0719(15) 0.6043(9) 0.3897(11) 0.075(5) Uiso 0.2 1 d D . P C 2
F15A F -0.0584(12) 0.6867(18) 0.375(2) 0.068(11) Uiso 0.2 1 d D . P C 2
F17A F -0.026(2) 0.8016(18) 0.0556(14) 0.101(10) Uiso 0.2 1 d D . P D 2
F18A F -0.0363(18) 0.9023(12) 0.1252(13) 0.095(6) Uiso 0.2 1 d D . P D 2
C27A C -0.0485(16) 0.8217(14) 0.1205(15) 0.048(6) Uiso 0.2 1 d D . P D 2
C1T C 0.1037(6) 0.4894(4) 0.2903(4) 0.0756(18) Uani 1 1 d . . . . .
H1TA H 0.110515 0.546097 0.303074 0.113 Uiso 1 1 calc GR . . . .
H1TB H 0.153107 0.458794 0.328362 0.113 Uiso 1 1 calc GR . . . .
H1TC H 0.032807 0.471774 0.289148 0.113 Uiso 1 1 calc GR . . . .
C2T C 0.1268(4) 0.4760(3) 0.2117(3) 0.0505(12) Uani 1 1 d . . . . .
C3T C 0.1009(4) 0.5328(3) 0.1533(4) 0.0570(15) Uani 1 1 d . . . . .
H3T H 0.073227 0.582849 0.162682 0.068 Uiso 1 1 calc R . . . .
C4T C 0.1161(4) 0.5155(4) 0.0813(4) 0.0595(16) Uani 1 1 d . . . . .
H4T H 0.097457 0.553551 0.041986 0.071 Uiso 1 1 calc R . . . .
C5T C 0.1582(5) 0.4428(4) 0.0674(4) 0.0651(16) Uani 1 1 d . . . . .
H5T H 0.167677 0.431060 0.018574 0.078 Uiso 1 1 calc R . . . .
C6T C 0.1861(5) 0.3878(4) 0.1247(4) 0.0679(17) Uani 1 1 d . . . . .
H6T H 0.216288 0.338684 0.115450 0.082 Uiso 1 1 calc R . . . .
C7T C 0.1703(4) 0.4038(3) 0.1965(4) 0.0597(15) Uani 1 1 d . . . . .
H7T H 0.189355 0.365133 0.235257 0.072 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
Y1 0.02211(18) 0.02214(17) 0.02079(18) 0.00142(13) 0.00602(13) 0.00294(13)
F1 0.056(3) 0.077(3) 0.0279(18) 0.0250(18) 0.0020(18) -0.017(2)
F2 0.072(3) 0.039(2) 0.0236(18) -0.0011(14) 0.0002(19) 0.007(2)
F3 0.048(2) 0.084(3) 0.0256(17) 0.0105(18) 0.0000(15) 0.037(2)
F4 0.0383(14) 0.0440(15) 0.0603(18) -0.0203(13) 0.0196(13) 0.0019(11)
F5 0.0221(11) 0.0574(16) 0.0423(15) 0.0017(12) 0.0074(11) 0.0086(11)
F6 0.0319(13) 0.0485(15) 0.0390(14) 0.0050(11) 0.0166(11) -0.0008(11)
F7 0.094(3) 0.045(2) 0.0328(18) 0.0129(15) 0.035(2) 0.022(2)
F8 0.118(4) 0.055(2) 0.0331(19) 0.0012(17) 0.018(2) -0.054(3)
F9 0.048(2) 0.096(3) 0.0302(18) 0.027(2) 0.0048(16) 0.021(2)
F10 0.0712(19) 0.0398(14) 0.0525(17) 0.0136(12) 0.0290(15) 0.0307(14)
F11 0.0661(18) 0.0348(13) 0.0342(14) -0.0052(11) 0.0164(13) -0.0023(12)
F12 0.0533(16) 0.0435(14) 0.0496(16) 0.0101(12) 0.0346(14) 0.0138(12)
F13 0.063(2) 0.074(3) 0.039(2) -0.0117(18) 0.0318(18) 0.003(2)
F14 0.0429(19) 0.071(3) 0.0338(18) 0.0232(17) 0.0150(16) 0.0060(17)
F15 0.033(2) 0.089(5) 0.039(3) 0.011(3) 0.0102(17) -0.025(2)
F16 0.0247(13) 0.112(3) 0.0387(16) 0.0057(16) 0.0037(12) 0.0122(15)
F17 0.0397(19) 0.058(3) 0.037(2) 0.0240(19) -0.0011(16) 0.0070(17)
F18 0.049(2) 0.067(2) 0.0282(17) -0.0168(16) -0.0050(15) 0.0067(17)
O1 0.0506(19) 0.0410(17) 0.0455(19) -0.0090(14) 0.0171(16) 0.0137(14)
O2 0.0467(18) 0.0278(15) 0.052(2) -0.0008(13) 0.0107(16) 0.0122(13)
O3 0.0236(13) 0.0234(12) 0.0280(14) 0.0023(10) 0.0047(11) 0.0004(10)
O4 0.0249(13) 0.0259(13) 0.0289(14) 0.0002(10) 0.0055(12) 0.0005(10)
O5 0.0325(14) 0.0259(13) 0.0220(13) 0.0038(10) 0.0086(11) 0.0006(11)
O6 0.0321(14) 0.0248(13) 0.0266(14) 0.0022(11) 0.0105(12) 0.0025(11)
O7 0.0239(13) 0.0320(14) 0.0285(14) -0.0003(11) 0.0049(11) 0.0021(10)
O8 0.0223(13) 0.0379(15) 0.0271(14) 0.0009(11) 0.0036(11) 0.0043(11)
N1 0.0246(15) 0.0262(15) 0.0218(15) 0.0002(12) 0.0063(13) 0.0003(12)
N2 0.0258(16) 0.0260(15) 0.0276(16) 0.0003(13) 0.0062(13) -0.0018(12)
C1 0.0277(19) 0.0266(18) 0.032(2) 0.0000(15) 0.0048(17) 0.0036(15)
C2 0.031(2) 0.037(2) 0.0235(19) -0.0001(16) 0.0094(16) 0.0021(16)
C3 0.032(2) 0.035(2) 0.028(2) -0.0058(16) 0.0111(17) -0.0003(16)
C4 0.0221(18) 0.0291(19) 0.032(2) 0.0004(15) 0.0074(16) -0.0017(14)
C5 0.029(2) 0.032(2) 0.038(2) -0.0064(17) 0.0139(18) 0.0002(16)
C6 0.034(2) 0.0212(17) 0.040(2) -0.0024(16) 0.0127(18) -0.0012(15)
C7 0.0248(18) 0.0234(17) 0.038(2) 0.0012(16) 0.0085(17) -0.0013(14)
C8 0.033(2) 0.0237(19) 0.048(3) 0.0067(17) 0.009(2) 0.0010(16)
C9 0.045(2) 0.028(2) 0.037(2) 0.0088(17) 0.011(2) 0.0015(17)
C10 0.036(2) 0.0285(19) 0.031(2) 0.0039(16) 0.0120(18) -0.0011(16)
C11 0.0246(18) 0.0238(17) 0.0284(19) -0.0022(14) 0.0094(16) -0.0028(14)
C12 0.0204(17) 0.0242(17) 0.0248(18) -0.0028(14) 0.0046(15) -0.0001(13)
C13 0.032(2) 0.039(2) 0.029(2) 0.0090(17) 0.0071(17) 0.0079(17)
C14 0.0278(19) 0.0253(17) 0.028(2) 0.0035(15) 0.0027(16) 0.0017(15)
C15 0.0234(18) 0.033(2) 0.031(2) 0.0049(16) 0.0047(16) 0.0036(15)
C16 0.0249(18) 0.0236(17) 0.0248(18) 0.0019(14) 0.0078(15) 0.0013(14)
C17 0.0258(19) 0.034(2) 0.031(2) -0.0012(16) 0.0081(17) 0.0022(16)
C18 0.038(2) 0.0284(19) 0.027(2) 0.0027(16) 0.0071(18) -0.0012(16)
C19 0.0261(18) 0.0257(18) 0.0259(19) 0.0025(14) 0.0045(16) -0.0031(14)
C20 0.035(2) 0.0255(18) 0.031(2) 0.0058(15) 0.0105(18) 0.0070(15)
C21 0.0272(19) 0.0257(18) 0.030(2) 0.0006(15) 0.0073(16) 0.0025(15)
C22 0.042(2) 0.030(2) 0.042(2) 0.0087(18) 0.020(2) 0.0114(18)
C23 0.030(2) 0.079(4) 0.041(3) 0.012(3) 0.009(2) 0.001(2)
C24 0.0268(19) 0.032(2) 0.032(2) -0.0008(16) 0.0100(17) 0.0017(15)
C25 0.0218(19) 0.049(2) 0.034(2) -0.0018(19) 0.0082(17) 0.0041(17)
C26 0.0252(19) 0.040(2) 0.0232(19) -0.0030(16) 0.0009(16) 0.0064(16)
C27 0.022(2) 0.041(3) 0.026(3) 0.000(2) 0.006(2) 0.005(2)
C1T 0.073(4) 0.068(4) 0.094(5) 0.000(4) 0.035(4) -0.006(3)
C2T 0.034(2) 0.062(3) 0.058(3) -0.002(3) 0.015(2) -0.009(2)
C3T 0.038(3) 0.035(2) 0.101(5) 0.006(3) 0.022(3) 0.001(2)
C4T 0.036(3) 0.072(4) 0.067(4) 0.030(3) 0.007(3) -0.010(2)
C5T 0.053(3) 0.076(4) 0.067(4) -0.015(3) 0.016(3) -0.018(3)
C6T 0.056(3) 0.045(3) 0.109(6) -0.010(3) 0.031(4) -0.008(3)
C7T 0.041(3) 0.053(3) 0.084(4) 0.026(3) 0.013(3) 0.003(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
Y1 O2 3.155(3) 2_655 ?
Y1 O3 2.344(3) . ?
Y1 O4 2.316(3) . ?
Y1 O5 2.331(2) . ?
Y1 O6 2.299(3) . ?
Y1 O7 2.332(3) . ?
Y1 O8 2.338(3) . ?
Y1 N1 2.501(3) . ?
Y1 N2 2.552(3) . ?
F1 C13 1.367(5) . ?
F2 C13 1.301(5) . ?
F3 C13 1.317(5) . ?
F4 C17 1.331(5) . ?
F5 C17 1.338(5) . ?
F6 C17 1.329(5) . ?
F7 C18 1.316(5) . ?
F8 C18 1.310(5) . ?
F9 C18 1.326(5) . ?
F10 C22 1.328(5) . ?
F11 C22 1.341(5) . ?
F12 C22 1.327(5) . ?
F13 C23 1.397(6) . ?
F14 C23 1.295(6) . ?
F15 C23 1.318(6) . ?
F16 C27 1.311(5) . ?
F16 C27A 1.398(17) . ?
F17 C27 1.333(6) . ?
F18 C27 1.332(6) . ?
O1 C5 1.213(5) . ?
O2 C6 1.216(5) . ?
O3 C14 1.256(5) . ?
O4 C16 1.249(5) . ?
O5 C19 1.257(4) . ?
O6 C21 1.256(4) . ?
O7 C24 1.257(5) . ?
O8 C26 1.251(5) . ?
N1 C1 1.345(5) . ?
N1 C12 1.350(5) . ?
N2 C10 1.335(5) . ?
N2 C11 1.340(5) . ?
C1 H1 0.9300 . ?
C1 C2 1.384(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.377(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.382(6) . ?
C4 C5 1.488(5) . ?
C4 C12 1.394(5) . ?
C5 C6 1.524(6) . ?
C6 C7 1.476(6) . ?
C7 C8 1.387(6) . ?
C7 C11 1.401(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.380(6) . ?
C9 H9 0.9300 . ?
C9 C10 1.391(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.479(5) . ?
C13 C14 1.525(6) . ?
C13 F1A 1.271(15) . ?
C13 F2A 1.364(14) . ?
C13 F3A 1.299(16) . ?
C14 C15 1.394(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.390(5) . ?
C16 C17 1.533(5) . ?
C18 C19 1.538(5) . ?
C18 F7A 1.297(15) . ?
C18 F8A 1.309(13) . ?
C18 F9A 1.347(14) . ?
C19 C20 1.388(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.385(5) . ?
C21 C22 1.538(6) . ?
C23 C24 1.521(6) . ?
C23 F13A 1.171(13) . ?
C23 F14A 1.550(14) . ?
C23 F15A 1.323(16) . ?
C24 C25 1.378(6) . ?
C25 H25 0.9300 . ?
C25 C26 1.391(6) . ?
C26 C27 1.528(6) . ?
C26 C27A 1.70(3) . ?
F17A C27A 1.303(18) . ?
F18A C27A 1.338(18) . ?
C1T H1TA 0.9600 . ?
C1T H1TB 0.9600 . ?
C1T H1TC 0.9600 . ?
C1T C2T 1.522(9) . ?
C2T C3T 1.384(8) . ?
C2T C7T 1.370(8) . ?
C3T H3T 0.9300 . ?
C3T C4T 1.378(9) . ?
C4T H4T 0.9300 . ?
C4T C5T 1.362(9) . ?
C5T H5T 0.9300 . ?
C5T C6T 1.352(9) . ?
C6T H6T 0.9300 . ?
C6T C7T 1.373(9) . ?
C7T H7T 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Y1 O2 62.55(9) . 2_655 ?
O3 Y1 N1 129.46(9) . . ?
O3 Y1 N2 73.77(9) . . ?
O4 Y1 O2 59.94(9) . 2_655 ?
O4 Y1 O3 73.97(9) . . ?
O4 Y1 O5 78.89(9) . . ?
O4 Y1 O7 143.59(9) . . ?
O4 Y1 O8 136.59(10) . . ?
O4 Y1 N1 69.92(10) . . ?
O4 Y1 N2 75.77(9) . . ?
O5 Y1 O2 64.43(9) . 2_655 ?
O5 Y1 O3 126.95(9) . . ?
O5 Y1 O7 137.38(9) . . ?
O5 Y1 O8 73.30(10) . . ?
O5 Y1 N1 78.84(9) . . ?
O5 Y1 N2 140.31(10) . . ?
O6 Y1 O2 61.93(9) . 2_655 ?
O6 Y1 O3 82.14(9) . . ?
O6 Y1 O4 121.82(9) . . ?
O6 Y1 O5 74.82(9) . . ?
O6 Y1 O7 76.18(9) . . ?
O6 Y1 O8 82.09(10) . . ?
O6 Y1 N1 147.59(10) . . ?
O6 Y1 N2 144.85(10) . . ?
O7 Y1 O2 124.75(9) . 2_655 ?
O7 Y1 O3 78.28(9) . . ?
O7 Y1 O8 72.35(9) . . ?
O7 Y1 N1 113.24(10) . . ?
O7 Y1 N2 74.16(10) . . ?
O8 Y1 O2 129.65(9) . 2_655 ?
O8 Y1 O3 149.21(9) . . ?
O8 Y1 N1 72.44(10) . . ?
O8 Y1 N2 106.09(10) . . ?
N1 Y1 O2 121.55(9) . 2_655 ?
N1 Y1 N2 64.02(10) . . ?
N2 Y1 O2 123.78(9) . 2_655 ?
C14 O3 Y1 133.5(3) . . ?
C16 O4 Y1 134.1(2) . . ?
C19 O5 Y1 131.6(2) . . ?
C21 O6 Y1 133.1(2) . . ?
C24 O7 Y1 135.1(3) . . ?
C26 O8 Y1 135.9(3) . . ?
C1 N1 Y1 122.0(2) . . ?
C1 N1 C12 117.2(3) . . ?
C12 N1 Y1 119.1(2) . . ?
C10 N2 Y1 122.8(3) . . ?
C10 N2 C11 118.2(3) . . ?
C11 N2 Y1 116.9(2) . . ?
N1 C1 H1 118.2 . . ?
N1 C1 C2 123.6(4) . . ?
C2 C1 H1 118.2 . . ?
C1 C2 H2 120.7 . . ?
C3 C2 C1 118.6(4) . . ?
C3 C2 H2 120.7 . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 119.0(4) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C5 121.0(4) . . ?
C3 C4 C12 119.1(4) . . ?
C12 C4 C5 119.9(4) . . ?
O1 C5 C4 122.7(4) . . ?
O1 C5 C6 119.4(4) . . ?
C4 C5 C6 117.9(3) . . ?
O2 C6 C5 119.2(4) . . ?
O2 C6 C7 122.6(4) . . ?
C7 C6 C5 118.1(3) . . ?
C8 C7 C6 121.1(4) . . ?
C8 C7 C11 119.0(4) . . ?
C11 C7 C6 119.9(4) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 C7 118.9(4) . . ?
C9 C8 H8 120.5 . . ?
C8 C9 H9 120.7 . . ?
C8 C9 C10 118.5(4) . . ?
C10 C9 H9 120.7 . . ?
N2 C10 C9 123.2(4) . . ?
N2 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
N2 C11 C7 122.0(4) . . ?
N2 C11 C12 116.9(3) . . ?
C7 C11 C12 121.1(3) . . ?
N1 C12 C4 122.3(3) . . ?
N1 C12 C11 116.0(3) . . ?
C4 C12 C11 121.6(3) . . ?
F1 C13 C14 109.5(3) . . ?
F2 C13 F1 105.5(4) . . ?
F2 C13 F3 109.8(4) . . ?
F2 C13 C14 112.2(3) . . ?
F3 C13 F1 105.1(4) . . ?
F3 C13 C14 114.2(4) . . ?
F1A C13 C14 112.8(10) . . ?
F1A C13 F2A 109.2(13) . . ?
F1A C13 F3A 107.3(14) . . ?
F2A C13 C14 110.2(9) . . ?
F3A C13 C14 115.3(12) . . ?
F3A C13 F2A 101.2(13) . . ?
O3 C14 C13 115.0(3) . . ?
O3 C14 C15 127.7(4) . . ?
C15 C14 C13 117.3(3) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.3(4) . . ?
C16 C15 H15 119.3 . . ?
O4 C16 C15 128.3(4) . . ?
O4 C16 C17 112.8(3) . . ?
C15 C16 C17 118.8(3) . . ?
F4 C17 F5 107.3(3) . . ?
F4 C17 C16 109.8(3) . . ?
F5 C17 C16 113.7(3) . . ?
F6 C17 F4 107.4(3) . . ?
F6 C17 F5 107.2(3) . . ?
F6 C17 C16 111.2(3) . . ?
F7 C18 F9 106.9(4) . . ?
F7 C18 C19 112.6(3) . . ?
F8 C18 F7 107.5(4) . . ?
F8 C18 F9 107.6(4) . . ?
F8 C18 C19 110.6(3) . . ?
F9 C18 C19 111.3(3) . . ?
F7A C18 C19 111.0(11) . . ?
F7A C18 F8A 112.3(13) . . ?
F7A C18 F9A 100.7(13) . . ?
F8A C18 C19 115.7(8) . . ?
F8A C18 F9A 103.6(12) . . ?
F9A C18 C19 112.3(8) . . ?
O5 C19 C18 115.2(3) . . ?
O5 C19 C20 128.3(4) . . ?
C20 C19 C18 116.5(3) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 C19 121.4(3) . . ?
C21 C20 H20 119.3 . . ?
O6 C21 C20 128.3(4) . . ?
O6 C21 C22 113.5(3) . . ?
C20 C21 C22 118.1(3) . . ?
F10 C22 F11 107.2(4) . . ?
F10 C22 C21 112.9(4) . . ?
F11 C22 C21 109.7(3) . . ?
F12 C22 F10 108.4(3) . . ?
F12 C22 F11 107.4(4) . . ?
F12 C22 C21 110.9(3) . . ?
F13 C23 C24 107.9(4) . . ?
F14 C23 F13 102.6(4) . . ?
F14 C23 F15 111.2(6) . . ?
F14 C23 C24 113.6(4) . . ?
F15 C23 F13 106.3(5) . . ?
F15 C23 C24 114.2(5) . . ?
C24 C23 F14A 98.3(8) . . ?
F13A C23 C24 125.4(9) . . ?
F13A C23 F14A 94.9(13) . . ?
F13A C23 F15A 117.8(16) . . ?
F15A C23 C24 113.2(17) . . ?
F15A C23 F14A 95.7(12) . . ?
O7 C24 C23 114.8(4) . . ?
O7 C24 C25 128.1(4) . . ?
C25 C24 C23 117.1(4) . . ?
C24 C25 H25 119.6 . . ?
C24 C25 C26 120.8(4) . . ?
C26 C25 H25 119.6 . . ?
O8 C26 C25 127.0(4) . . ?
O8 C26 C27 114.8(4) . . ?
O8 C26 C27A 109.5(7) . . ?
C25 C26 C27 118.0(4) . . ?
C25 C26 C27A 119.3(7) . . ?
F16 C27 F17 105.9(4) . . ?
F16 C27 F18 108.7(4) . . ?
F16 C27 C26 113.9(4) . . ?
F17 C27 C26 110.0(4) . . ?
F18 C27 F17 106.7(5) . . ?
F18 C27 C26 111.3(4) . . ?
F16 C27A C26 100.0(14) . . ?
F17A C27A F16 111(2) . . ?
F17A C27A C26 104(2) . . ?
F17A C27A F18A 105(2) . . ?
F18A C27A F16 119.4(19) . . ?
F18A C27A C26 116.6(18) . . ?
H1TA C1T H1TB 109.5 . . ?
H1TA C1T H1TC 109.5 . . ?
H1TB C1T H1TC 109.5 . . ?
C2T C1T H1TA 109.5 . . ?
C2T C1T H1TB 109.5 . . ?
C2T C1T H1TC 109.5 . . ?
C3T C2T C1T 122.2(5) . . ?
C7T C2T C1T 119.4(6) . . ?
C7T C2T C3T 118.3(5) . . ?
C2T C3T H3T 119.9 . . ?
C4T C3T C2T 120.2(5) . . ?
C4T C3T H3T 119.9 . . ?
C3T C4T H4T 119.9 . . ?
C5T C4T C3T 120.3(5) . . ?
C5T C4T H4T 119.9 . . ?
C4T C5T H5T 120.1 . . ?
C6T C5T C4T 119.8(6) . . ?
C6T C5T H5T 120.1 . . ?
C5T C6T H6T 119.7 . . ?
C5T C6T C7T 120.6(6) . . ?
C7T C6T H6T 119.7 . . ?
C2T C7T C6T 120.8(5) . . ?
C2T C7T H7T 119.6 . . ?
C6T C7T H7T 119.6 . . ?
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
Y1 O3 C14 C13 -170.6(2) . . . . ?
Y1 O3 C14 C15 6.8(6) . . . . ?
Y1 O4 C16 C15 -9.9(6) . . . . ?
Y1 O4 C16 C17 167.5(2) . . . . ?
Y1 O5 C19 C18 -167.9(2) . . . . ?
Y1 O5 C19 C20 14.3(6) . . . . ?
Y1 O6 C21 C20 -6.6(6) . . . . ?
Y1 O6 C21 C22 176.3(3) . . . . ?
Y1 O7 C24 C23 -170.3(3) . . . . ?
Y1 O7 C24 C25 8.4(7) . . . . ?
Y1 O8 C26 C25 -2.3(7) . . . . ?
Y1 O8 C26 C27 -177.8(3) . . . . ?
Y1 O8 C26 C27A 154.1(8) . . . . ?
Y1 N1 C1 C2 163.1(3) . . . . ?
Y1 N1 C12 C4 -163.1(3) . . . . ?
Y1 N1 C12 C11 19.8(4) . . . . ?
Y1 N2 C10 C9 -161.1(3) . . . . ?
Y1 N2 C11 C7 159.9(3) . . . . ?
Y1 N2 C11 C12 -21.6(4) . . . . ?
F1 C13 C14 O3 51.3(5) . . . . ?
F1 C13 C14 C15 -126.4(4) . . . . ?
F2 C13 C14 O3 -65.5(5) . . . . ?
F2 C13 C14 C15 116.9(5) . . . . ?
F3 C13 C14 O3 168.9(4) . . . . ?
F3 C13 C14 C15 -8.8(6) . . . . ?
F7 C18 C19 O5 4.9(5) . . . . ?
F7 C18 C19 C20 -177.0(4) . . . . ?
F8 C18 C19 O5 -115.5(5) . . . . ?
F8 C18 C19 C20 62.6(5) . . . . ?
F9 C18 C19 O5 124.9(4) . . . . ?
F9 C18 C19 C20 -57.0(5) . . . . ?
F13 C23 C24 O7 88.9(4) . . . . ?
F13 C23 C24 C25 -89.9(5) . . . . ?
F14 C23 C24 O7 -24.1(6) . . . . ?
F14 C23 C24 C25 157.1(4) . . . . ?
F15 C23 C24 O7 -153.2(6) . . . . ?
F15 C23 C24 C25 28.0(8) . . . . ?
O1 C5 C6 O2 15.3(6) . . . . ?
O1 C5 C6 C7 -165.1(4) . . . . ?
O2 C6 C7 C8 -13.2(6) . . . . ?
O2 C6 C7 C11 166.5(4) . . . . ?
O3 C14 C15 C16 1.1(6) . . . . ?
O4 C16 C17 F4 -66.0(4) . . . . ?
O4 C16 C17 F5 173.8(3) . . . . ?
O4 C16 C17 F6 52.8(4) . . . . ?
O5 C19 C20 C21 1.2(7) . . . . ?
O6 C21 C22 F10 -162.6(4) . . . . ?
O6 C21 C22 F11 77.8(4) . . . . ?
O6 C21 C22 F12 -40.7(5) . . . . ?
O7 C24 C25 C26 0.7(7) . . . . ?
O8 C26 C27 F16 -163.0(4) . . . . ?
O8 C26 C27 F17 -44.3(6) . . . . ?
O8 C26 C27 F18 73.7(5) . . . . ?
O8 C26 C27A F16 165.5(9) . . . . ?
O8 C26 C27A F17A 50.9(18) . . . . ?
O8 C26 C27A F18A -64.2(19) . . . . ?
N1 C1 C2 C3 -0.6(6) . . . . ?
N2 C11 C12 N1 1.8(5) . . . . ?
N2 C11 C12 C4 -175.4(3) . . . . ?
C1 N1 C12 C4 2.2(5) . . . . ?
C1 N1 C12 C11 -175.0(3) . . . . ?
C1 C2 C3 C4 2.3(6) . . . . ?
C2 C3 C4 C5 176.8(4) . . . . ?
C2 C3 C4 C12 -1.8(6) . . . . ?
C3 C4 C5 O1 -6.2(6) . . . . ?
C3 C4 C5 C6 175.2(4) . . . . ?
C3 C4 C12 N1 -0.5(6) . . . . ?
C3 C4 C12 C11 176.5(3) . . . . ?
C4 C5 C6 O2 -165.9(4) . . . . ?
C4 C5 C6 C7 13.6(5) . . . . ?
C5 C4 C12 N1 -179.1(3) . . . . ?
C5 C4 C12 C11 -2.1(5) . . . . ?
C5 C6 C7 C8 167.3(4) . . . . ?
C5 C6 C7 C11 -13.0(5) . . . . ?
C6 C7 C8 C9 -179.7(4) . . . . ?
C6 C7 C11 N2 -176.7(3) . . . . ?
C6 C7 C11 C12 4.9(5) . . . . ?
C7 C8 C9 C10 -2.6(6) . . . . ?
C7 C11 C12 N1 -179.7(3) . . . . ?
C7 C11 C12 C4 3.1(5) . . . . ?
C8 C7 C11 N2 3.0(6) . . . . ?
C8 C7 C11 C12 -175.4(3) . . . . ?
C8 C9 C10 N2 1.3(6) . . . . ?
C10 N2 C11 C7 -4.3(5) . . . . ?
C10 N2 C11 C12 174.2(3) . . . . ?
C11 N2 C10 C9 2.2(6) . . . . ?
C11 C7 C8 C9 0.6(6) . . . . ?
C12 N1 C1 C2 -1.7(6) . . . . ?
C12 C4 C5 O1 172.5(4) . . . . ?
C12 C4 C5 C6 -6.2(5) . . . . ?
C13 C14 C15 C16 178.4(3) . . . . ?
C14 C15 C16 O4 0.4(6) . . . . ?
C14 C15 C16 C17 -176.9(3) . . . . ?
C15 C16 C17 F4 111.8(4) . . . . ?
C15 C16 C17 F5 -8.5(5) . . . . ?
C15 C16 C17 F6 -129.5(4) . . . . ?
C18 C19 C20 C21 -176.6(4) . . . . ?
C19 C20 C21 O6 -5.4(7) . . . . ?
C19 C20 C21 C22 171.6(4) . . . . ?
C20 C21 C22 F10 19.9(6) . . . . ?
C20 C21 C22 F11 -99.7(4) . . . . ?
C20 C21 C22 F12 141.9(4) . . . . ?
C23 C24 C25 C26 179.4(4) . . . . ?
C24 C25 C26 O8 -3.7(7) . . . . ?
C24 C25 C26 C27 171.6(4) . . . . ?
C24 C25 C26 C27A -158.1(9) . . . . ?
C25 C26 C27 F16 21.1(6) . . . . ?
C25 C26 C27 F17 139.8(4) . . . . ?
C25 C26 C27 F18 -102.2(5) . . . . ?
C25 C26 C27A F16 -36.0(15) . . . . ?
C25 C26 C27A F17A -150.6(16) . . . . ?
C25 C26 C27A F18A 94.3(17) . . . . ?
F1A C13 C14 O3 86.9(11) . . . . ?
F1A C13 C14 C15 -90.7(11) . . . . ?
F2A C13 C14 O3 -150.7(10) . . . . ?
F2A C13 C14 C15 31.6(10) . . . . ?
F3A C13 C14 O3 -36.9(11) . . . . ?
F3A C13 C14 C15 145.5(11) . . . . ?
F7A C18 C19 O5 43.6(12) . . . . ?
F7A C18 C19 C20 -138.3(11) . . . . ?
F8A C18 C19 O5 173.1(10) . . . . ?
F8A C18 C19 C20 -8.9(11) . . . . ?
F9A C18 C19 O5 -68.3(10) . . . . ?
F9A C18 C19 C20 109.8(10) . . . . ?
F13A C23 C24 O7 30.2(14) . . . . ?
F13A C23 C24 C25 -148.7(13) . . . . ?
F14A C23 C24 O7 -71.9(8) . . . . ?
F14A C23 C24 C25 109.3(8) . . . . ?
F15A C23 C24 O7 -171.8(13) . . . . ?
F15A C23 C24 C25 9.4(14) . . . . ?
C1T C2T C3T C4T -175.1(5) . . . . ?
C1T C2T C7T C6T 176.0(5) . . . . ?
C2T C3T C4T C5T -1.0(8) . . . . ?
C3T C2T C7T C6T -1.1(8) . . . . ?
C3T C4T C5T C6T -0.6(8) . . . . ?
C4T C5T C6T C7T 1.4(9) . . . . ?
C5T C6T C7T C2T -0.6(9) . . . . ?
C7T C2T C3T C4T 1.8(8) . . . . ?
_shelx_res_file
;
TITL mo_jhgla020_r1_0m_a.res in P2(1)/c
mo_jhgla020_r1_0m.res
created by SHELXL-2016/6 at 11:14:57 on 22-Mar-2018
REM Old TITL
REM SHELXT solution in P2(1)/c
REM R1 0.159, Rweak 0.009, Alpha 0.077, Orientation as input
REM Formula found by SHELXT: C34 N2 O6 F20 Y
CELL 0.71073 12.9792 16.4628 17.8859 90 103.679 90
ZERR 4 0.0009 0.0013 0.0013 0 0.003 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H F N O Y
UNIT 136 68 72 8 32 4
EQIV $1 1-X,0.5+Y,0.5-Z
DFIX 1.336 F3 C13 F2A C13 F2 C13 F3A C13 F1A C13 F1 C13 F15A C23 F13A C23 =
F14A C23 F14 C23 F13 C23 F15 C23 F16 C27A F16 C27 F18 C27 F17A C27A F17 C27 =
F18A C27A F9 C18 F8A C18 F8 C18 F7A C18 F7 C18 F9A C18
SADI F14A F15A F15 F13 F13A F15A F13 F14
L.S. 8 0 0
PLAN 50
TEMP 20.53
BIND Y1 O2_$1
BOND $H
conf
list 4
fmap 2 53
acta
OMIT -6 3 21
OMIT -6 2 21
OMIT -7 4 20
REM
REM
REM
WGHT 0.059000 10.043000
FVAR 0.09123
Y1 6 0.301116 0.765417 0.256593 11.00000 0.02211 0.02214 =
0.02079 0.00142 0.00602 0.00294
PART 1
F1 3 0.476136 0.670271 0.514534 10.80000 0.05607 0.07716 =
0.02787 0.02504 0.00199 -0.01689
F2 3 0.540042 0.789532 0.529062 10.80000 0.07157 0.03900 =
0.02360 -0.00108 0.00018 0.00747
F3 3 0.638459 0.689268 0.514356 10.80000 0.04848 0.08403 =
0.02559 0.01047 0.00004 0.03684
PART 0
F4 3 0.613910 0.641953 0.195267 11.00000 0.03831 0.04396 =
0.06031 -0.02028 0.01964 0.00188
F5 3 0.738357 0.695278 0.282439 11.00000 0.02206 0.05739 =
0.04233 0.00173 0.00744 0.00864
F6 3 0.651509 0.768190 0.189174 11.00000 0.03191 0.04850 =
0.03897 0.00501 0.01656 -0.00077
PART 1
F7 3 0.304177 0.928828 0.033144 10.80000 0.09374 0.04471 =
0.03276 0.01289 0.03507 0.02215
F8 3 0.327490 1.041900 0.091211 10.80000 0.11823 0.05537 =
0.03306 0.00122 0.01848 -0.05387
F9 3 0.171119 0.999776 0.042203 10.80000 0.04806 0.09635 =
0.03025 0.02744 0.00478 0.02058
PART 0
F10 3 0.133096 1.072661 0.303141 11.00000 0.07123 0.03977 =
0.05251 0.01355 0.02902 0.03071
F11 3 0.274970 1.039299 0.386484 11.00000 0.06607 0.03480 =
0.03421 -0.00517 0.01640 -0.00233
F12 3 0.131719 0.970911 0.378632 11.00000 0.05333 0.04345 =
0.04962 0.01008 0.03459 0.01384
PART 1
F13 3 0.040109 0.766325 0.432389 10.80000 0.06270 0.07415 =
0.03868 -0.01167 0.03180 0.00270
F14 3 0.112403 0.651577 0.437598 10.80000 0.04293 0.07134 =
0.03378 0.02324 0.01502 0.00600
F15 3 -0.049978 0.664027 0.373807 10.80000 0.03350 0.08866 =
0.03859 0.01068 0.01017 -0.02498
PART 0
F16 3 -0.144644 0.787298 0.126801 11.00000 0.02472 0.11196 =
0.03868 0.00574 0.00366 0.01221
PART 1
F17 3 -0.031006 0.841399 0.075422 10.80000 0.03966 0.05810 =
0.03717 0.02397 -0.00107 0.00699
F18 3 -0.054566 0.712882 0.066805 10.80000 0.04885 0.06699 =
0.02816 -0.01677 -0.00503 0.00666
PART 0
O1 5 0.439630 0.448344 0.042808 11.00000 0.05061 0.04104 =
0.04549 -0.00902 0.01714 0.01370
O2 5 0.526968 0.402322 0.190697 11.00000 0.04665 0.02775 =
0.05197 -0.00080 0.01070 0.01218
O3 5 0.412896 0.754084 0.379969 11.00000 0.02359 0.02336 =
0.02805 0.00227 0.00466 0.00040
O4 5 0.470746 0.748472 0.238653 11.00000 0.02493 0.02589 =
0.02894 0.00017 0.00555 0.00054
O5 5 0.305629 0.865979 0.165695 11.00000 0.03252 0.02589 =
0.02204 0.00382 0.00861 0.00063
O6 5 0.250478 0.882714 0.307819 11.00000 0.03214 0.02483 =
0.02662 0.00216 0.01052 0.00253
O7 5 0.183652 0.720581 0.328273 11.00000 0.02392 0.03201 =
0.02849 -0.00029 0.00495 0.00209
O8 5 0.129646 0.774736 0.178250 11.00000 0.02233 0.03788 =
0.02707 0.00092 0.00364 0.00428
N1 4 0.295538 0.681589 0.139116 11.00000 0.02460 0.02621 =
0.02176 0.00019 0.00627 0.00033
N2 4 0.338336 0.614103 0.279333 11.00000 0.02584 0.02603 =
0.02759 0.00026 0.00618 -0.00182
C1 1 0.264859 0.712753 0.067816 11.00000 0.02770 0.02665 =
0.03198 0.00001 0.00482 0.00359
AFIX 43
H1 2 0.227852 0.761616 0.061582 11.00000 -1.20000
AFIX 0
C2 1 0.285316 0.676125 0.003207 11.00000 0.03085 0.03682 =
0.02353 -0.00007 0.00938 0.00210
AFIX 43
H2 2 0.262036 0.699652 -0.045119 11.00000 -1.20000
AFIX 0
C3 1 0.340843 0.604138 0.011945 11.00000 0.03167 0.03509 =
0.02773 -0.00577 0.01109 -0.00035
AFIX 43
H3 2 0.357923 0.579170 -0.030184 11.00000 -1.20000
AFIX 0
C4 1 0.370845 0.569499 0.084243 11.00000 0.02211 0.02914 =
0.03203 0.00036 0.00740 -0.00172
C5 1 0.426062 0.489649 0.095818 11.00000 0.02929 0.03180 =
0.03811 -0.00636 0.01386 0.00025
C6 1 0.464574 0.458605 0.177938 11.00000 0.03372 0.02115 =
0.03988 -0.00242 0.01272 -0.00124
C7 1 0.424658 0.498975 0.239164 11.00000 0.02477 0.02339 =
0.03752 0.00121 0.00847 -0.00128
C8 1 0.439351 0.464642 0.311717 11.00000 0.03321 0.02372 =
0.04802 0.00667 0.00867 0.00099
AFIX 43
H8 2 0.475059 0.415531 0.322980 11.00000 -1.20000
AFIX 0
C9 1 0.400123 0.504542 0.366916 11.00000 0.04520 0.02755 =
0.03670 0.00880 0.01091 0.00151
AFIX 43
H9 2 0.406289 0.481864 0.415398 11.00000 -1.20000
AFIX 0
C10 1 0.351123 0.579476 0.348429 11.00000 0.03601 0.02855 =
0.03061 0.00392 0.01202 -0.00111
AFIX 43
H10 2 0.326040 0.606793 0.386061 11.00000 -1.20000
AFIX 0
C11 1 0.371396 0.573394 0.224466 11.00000 0.02455 0.02379 =
0.02845 -0.00220 0.00945 -0.00283
C12 1 0.346707 0.609580 0.146595 11.00000 0.02042 0.02417 =
0.02479 -0.00280 0.00463 -0.00008
C13 1 0.544070 0.722591 0.491189 11.00000 0.03187 0.03895 =
0.02910 0.00900 0.00712 0.00789
C14 1 0.508663 0.734989 0.404364 11.00000 0.02784 0.02530 =
0.02837 0.00348 0.00271 0.00174
C15 1 0.583557 0.721113 0.361359 11.00000 0.02337 0.03312 =
0.03093 0.00493 0.00467 0.00355
AFIX 43
H15 2 0.652186 0.706332 0.386441 11.00000 -1.20000
AFIX 0
C16 1 0.557695 0.728934 0.281693 11.00000 0.02493 0.02356 =
0.02476 0.00186 0.00783 0.00130
C17 1 0.641935 0.708619 0.237221 11.00000 0.02579 0.03407 =
0.03145 -0.00120 0.00809 0.00218
C18 1 0.267507 0.976940 0.079627 11.00000 0.03839 0.02836 =
0.02723 0.00266 0.00709 -0.00122
C19 1 0.265559 0.935823 0.156500 11.00000 0.02613 0.02565 =
0.02586 0.00245 0.00447 -0.00308
C20 1 0.223240 0.980928 0.207621 11.00000 0.03522 0.02550 =
0.03102 0.00582 0.01053 0.00699
AFIX 43
H20 2 0.194696 1.031912 0.192905 11.00000 -1.20000
AFIX 0
C21 1 0.222639 0.951580 0.280112 11.00000 0.02723 0.02572 =
0.02965 0.00064 0.00730 0.00247
C22 1 0.188825 1.009638 0.337309 11.00000 0.04227 0.03038 =
0.04199 0.00874 0.02031 0.01137
C23 1 0.045691 0.696185 0.389532 11.00000 0.02991 0.07883 =
0.04061 0.01218 0.00868 0.00074
C24 1 0.084564 0.720670 0.318935 11.00000 0.02683 0.03242 =
0.03210 -0.00075 0.01001 0.00165
C25 1 0.008719 0.741441 0.253855 11.00000 0.02176 0.04906 =
0.03375 -0.00177 0.00823 0.00412
AFIX 43
H25 2 -0.062633 0.739470 0.254621 11.00000 -1.20000
AFIX 0
C26 1 0.037562 0.765316 0.187038 11.00000 0.02518 0.03960 =
0.02322 -0.00299 0.00089 0.00636
PART 1
C27 1 -0.050295 0.776022 0.113971 10.80000 0.02228 0.04111 =
0.02586 -0.00023 0.00565 0.00458
PART 0
PART 2
F1A 3 0.528231 0.650648 0.511690 10.20000 0.06881
F2A 3 0.648967 0.741058 0.516599 10.20000 0.06486
F3A 3 0.501770 0.771726 0.532296 10.20000 0.06288
F7A 3 0.240476 0.926216 0.022868 10.20000 0.07684
F8A 3 0.216165 1.045858 0.065894 10.20000 0.06080
F9A 3 0.366553 0.996146 0.074743 10.20000 0.06367
F13A 3 0.091490 0.706936 0.453473 10.20000 0.06182
F14A 3 0.071921 0.604336 0.389681 10.20000 0.07513
F15A 3 -0.058364 0.686735 0.375235 10.20000 0.06786
F17A 3 -0.026456 0.801582 0.055567 10.20000 0.10142
F18A 3 -0.036302 0.902332 0.125242 10.20000 0.09475
C27A 1 -0.048542 0.821668 0.120487 10.20000 0.04822
PART 0
C1T 1 0.103682 0.489396 0.290333 11.00000 0.07277 0.06797 =
0.09351 -0.00020 0.03466 -0.00581
AFIX 137
H1TA 2 0.110515 0.546097 0.303074 11.00000 -1.50000
H1TB 2 0.153107 0.458794 0.328362 11.00000 -1.50000
H1TC 2 0.032807 0.471774 0.289148 11.00000 -1.50000
AFIX 0
C2T 1 0.126849 0.475957 0.211734 11.00000 0.03395 0.06203 =
0.05784 -0.00161 0.01539 -0.00922
C3T 1 0.100938 0.532797 0.153314 11.00000 0.03823 0.03451 =
0.10095 0.00603 0.02201 0.00124
AFIX 43
H3T 2 0.073227 0.582849 0.162682 11.00000 -1.20000
AFIX 0
C4T 1 0.116071 0.515468 0.081272 11.00000 0.03603 0.07225 =
0.06746 0.03000 0.00654 -0.01008
AFIX 43
H4T 2 0.097457 0.553551 0.041986 11.00000 -1.20000
AFIX 0
C5T 1 0.158179 0.442791 0.067364 11.00000 0.05326 0.07650 =
0.06650 -0.01454 0.01581 -0.01787
AFIX 43
H5T 2 0.167677 0.431060 0.018574 11.00000 -1.20000
AFIX 0
C6T 1 0.186112 0.387781 0.124718 11.00000 0.05576 0.04524 =
0.10877 -0.00998 0.03143 -0.00780
AFIX 43
H6T 2 0.216288 0.338684 0.115450 11.00000 -1.20000
AFIX 0
C7T 1 0.170324 0.403759 0.196500 11.00000 0.04066 0.05294 =
0.08440 0.02604 0.01253 0.00271
AFIX 43
H7T 2 0.189355 0.365133 0.235257 11.00000 -1.20000
AFIX 0
HKLF 4
REM mo_jhgla020_r1_0m_a.res in P2(1)/c
REM R1 = 0.0510 for 6690 Fo > 4sig(Fo) and 0.0661 for all 8274 data
REM 617 parameters refined using 30 restraints
END
WGHT 0.0550 10.1012
REM Highest difference peak 0.833, deepest hole -0.872, 1-sigma level 0.093
Q1 1 0.4027 0.4590 0.4344 11.00000 0.05 0.83
Q2 1 0.1786 0.3631 0.0187 11.00000 0.05 0.79
Q3 1 0.3574 0.7607 0.2420 11.00000 0.05 0.75
Q4 1 0.0693 0.5773 0.3763 11.00000 0.05 0.74
Q5 1 0.1784 0.7616 0.2607 11.00000 0.05 0.69
Q6 1 0.1854 0.7635 0.3184 11.00000 0.05 0.66
Q7 1 0.4183 0.7648 0.2000 11.00000 0.05 0.64
Q8 1 0.6443 0.7827 0.5200 11.00000 0.05 0.63
Q9 1 0.4245 0.7667 0.2562 11.00000 0.05 0.54
Q10 1 0.2119 0.7381 0.2198 11.00000 0.05 0.53
Q11 1 0.3981 0.7727 0.3016 11.00000 0.05 0.51
Q12 1 0.2010 0.7845 0.2155 11.00000 0.05 0.49
Q13 1 0.1006 0.7647 0.3015 11.00000 0.05 0.46
Q14 1 0.2890 0.8226 0.2008 11.00000 0.05 0.46
Q15 1 0.3448 0.7597 0.3397 11.00000 0.05 0.43
Q16 1 0.3361 0.7637 0.1866 11.00000 0.05 0.42
Q17 1 0.3760 0.7164 0.2813 11.00000 0.05 0.40
Q18 1 -0.0280 0.7449 0.4025 11.00000 0.05 0.39
Q19 1 0.2598 1.0625 0.0816 11.00000 0.05 0.38
Q20 1 0.2551 0.7585 0.3237 11.00000 0.05 0.38
Q21 1 0.1904 0.9442 0.0272 11.00000 0.05 0.38
Q22 1 0.5851 0.6554 0.5079 11.00000 0.05 0.37
Q23 1 0.3760 0.6988 0.3789 11.00000 0.05 0.37
Q24 1 0.3744 0.9590 0.0572 11.00000 0.05 0.37
Q25 1 0.2589 0.7634 0.1810 11.00000 0.05 0.37
Q26 1 0.4651 0.7178 0.2396 11.00000 0.05 0.35
Q27 1 0.6001 0.7191 0.2582 11.00000 0.05 0.34
Q28 1 0.3052 0.7205 0.3186 11.00000 0.05 0.34
Q29 1 0.2143 0.7394 0.1198 11.00000 0.05 0.34
Q30 1 0.1785 0.7747 0.3648 11.00000 0.05 0.33
Q31 1 0.0007 0.8875 0.0906 11.00000 0.05 0.33
Q32 1 0.5366 0.7211 0.3800 11.00000 0.05 0.33
Q33 1 0.4823 0.7251 0.5208 11.00000 0.05 0.33
Q34 1 0.2425 0.7601 0.2759 11.00000 0.05 0.33
Q35 1 0.2580 0.8424 0.2438 11.00000 0.05 0.33
Q36 1 0.0721 0.7598 0.2431 11.00000 0.05 0.32
Q37 1 0.2174 0.8232 0.1802 11.00000 0.05 0.32
Q38 1 0.2230 0.7126 0.2983 11.00000 0.05 0.32
Q39 1 0.4728 0.7792 0.2576 11.00000 0.05 0.32
Q40 1 0.1401 0.8203 0.1666 11.00000 0.05 0.32
Q41 1 0.2963 0.7143 0.1996 11.00000 0.05 0.31
Q42 1 0.0813 0.7018 0.4344 11.00000 0.05 0.31
Q43 1 0.2596 0.6793 0.0415 11.00000 0.05 0.31
Q44 1 0.3871 0.7712 0.4397 11.00000 0.05 0.31
Q45 1 0.3816 0.8217 0.2187 11.00000 0.05 0.30
Q46 1 0.4989 0.7663 0.2173 11.00000 0.05 0.30
Q47 1 0.2937 0.8241 0.1013 11.00000 0.05 0.29
Q48 1 0.2379 0.7725 0.3781 11.00000 0.05 0.29
Q49 1 -0.0542 0.7639 0.0570 11.00000 0.05 0.29
Q50 1 0.1928 0.8042 0.1199 11.00000 0.05 0.29
;
_shelx_res_checksum 84327
_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_3
_database_code_depnum_ccdc_archive 'CCDC 1832433'
_audit_update_record
;
2018-03-26 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;
# mo_jhgla075_0m
# [Y(hfac)3(N.N'-O,O'-pd)VCp2]
_audit_creation_date 2018-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2016/6
# start Validation Reply Form
_vrf_PLAT201_mo_jhgla075_0m
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 20 Report
RESPONSE: One Cp ring and two fo the hfac groups are disordered and many of the
atoms were refined with isotropic adps. In addition the carbon of the CF3 groups
were refined with isotropic adps even when fully occupied.
;
_vrf_PLAT241_mo_jhgla075_0m
;
PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of F13 Check
RESPONSE: Fluorine atoms of CFs groups show large displacements. F13 is
modelled as common to two partially occupied CF3 groups and may be accounted
for two very closely adjacent sites.
;
# end Validation Reply Form
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C37 H14 F18 N2 O8 V Y'
_chemical_formula_sum 'C37 H19 F18 N2 O8 V Y'
_chemical_formula_weight 1101.39
_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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 '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 33
_space_group_name_H-M_alt 'P n 21 a'
_space_group_name_Hall 'P -2ac -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
_cell_length_a 14.0879(7)
_cell_length_b 14.8963(9)
_cell_length_c 19.6006(12)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 4113.3(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 6096
_cell_measurement_temperature 100
_cell_measurement_theta_max 24.334
_cell_measurement_theta_min 2.244
_shelx_estimated_absorpt_T_max 0.983
_shelx_estimated_absorpt_T_min 0.730
_exptl_absorpt_coefficient_mu 1.766
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.6517
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0600 before and 0.0479 after correction. The Ratio of minimum to maximum transmission is 0.8741. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 1.779
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description shard
_exptl_crystal_F_000 2172
_exptl_crystal_size_max 0.19
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.01
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0481
_diffrn_reflns_av_unetI/netI 0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 28166
_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 25.350
_diffrn_reflns_theta_min 2.488
_diffrn_ambient_temperature 100.0
_diffrn_detector 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type 'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 VENTURE'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_collimation 'focusing mirrors'
_diffrn_radiation_monochromator 'multilayer mirror optics'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed tube'
_diffrn_source_type 'INCOATEC I\ms 3.0'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.920
_reflns_Friedel_fraction_full 0.999
_reflns_Friedel_fraction_max 0.999
_reflns_number_gt 4805
_reflns_number_total 6898
_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 V8.37A (Bruker-AXS, 2016)'
_computing_data_collection 'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction 'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'XM (Sheldrick, 2008)'
_refine_diff_density_max 0.688
_refine_diff_density_min -0.478
_refine_diff_density_rms 0.099
_refine_ls_abs_structure_details
;
Flack x determined using 1728 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack -0.010(7)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.024
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 594
_refine_ls_number_reflns 6898
_refine_ls_number_restraints 995
_refine_ls_R_factor_all 0.1030
_refine_ls_R_factor_gt 0.0687
_refine_ls_restrained_S_all 1.042
_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^)+(0.1260P)^2^+8.1630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1852
_refine_ls_wR_factor_ref 0.2180
_refine_special_details
;
The structure is close to having the mirror symmetry of Pnma with the mirror through the
two metal centres and perpendicular to the dp ligand plane. However this requires disordered of
two of the hfac ligands and one Cp ring is positioned off to the side of the mirror. Initial
modelling suggested that this disorder is present but that it is not the 50:50 required by
mirror symmetry. The occupancy of the disorder components was modelled competitively and
ultimately refined to 0.58(1)/0.42(1). Distance and planarity restraints were applied and
all partially occupied atoms and the carbons of the CF3 groups were refined with isotropic
adps.
A twin law corresponding to a 2-fold along the 110 direction was also used.
The disordered Cp hydrogen atoms were not included in the model but are included in the
unit cell contents and values derived from them.
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.48(3)
0.52(3)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups
3. Restrained distances
F2-C13 = F1-C13 = F3-C13 = F4-C17 = F5-C17 = F6-C17 = F9-C18A = F8-C18A = F8A-
C18A = F7-C18A = F7A-C18A = F9A-C18A = F10A-C22A = F13-C22A = F13-C23 = F14-
C23 = F11A-C22A = F15-C23 = F17A-C22 = F11-C22 = F18A-C22 = F12-C22 = F16A-C22
= F10-C22 = F13A-C23A = F14A-C23A = F15A-C23A = F17-C27 = F16-C27 = F18-C27
1.33 with sigma of 0.02
C37-C38 = C34-C38 = C34-C39 = C39-C40 = C37-C40 = C37-C36 = C33-C37 = C34-C33
= C34-C35 = C36-C35
1.42 with sigma of 0.01
C31-C30 \\sim C29-C30 \\sim C29-C28 \\sim C32-C28 \\sim C31-C32
with sigma of 0.02
F1-F2 \\sim F1-F3 \\sim F2-F3 \\sim F4-F5 \\sim F4-F6 \\sim F5-F6 \\sim F7-F8
\\sim F7-F9 \\sim F8-F9 \\sim F10-
F11 \\sim F10-F12 \\sim F11-F12 \\sim F13-F14 \\sim F13-F15 \\sim F14-F15
\\sim F16-F17 \\sim F16-F18 ~
F17-F18 \\sim F7A-F8A \\sim F7A-F9A \\sim F8A-F9A \\sim F16A-F17A \\sim
F16A-F18A \\sim F17A-F18A ~
F13-F10A \\sim F13-F11A \\sim F10A-F11A \\sim F13A-F14A \\sim F13A-F15A \\sim
F14A-F15A
with sigma of 0.02
4. Restrained planarity
O8, C24A, C25A, C26A, O6, C22
with sigma of 0.1
C33, C34, C35, C36, C37
with sigma of 0.1
5. Rigid body (RIGU) restrains
All non-hydrogen atoms
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
Sof(C38)=Sof(C39)=Sof(C40)=Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(C22A)=
Sof(C23A)=Sof(C24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=
Sof(F10A)=Sof(F11A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(F16A)=Sof(F17A)=
Sof(F18A)=1-FVAR(1)
Sof(F10)=Sof(F11)=Sof(F12)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(F17)=Sof(F18)=
Sof(C19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(C23)=Sof(C24)=Sof(C25)=Sof(H25)=
Sof(C26)=Sof(C27)=Sof(C33)=Sof(C35)=Sof(C36)=Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C15(H15), C20(H20),
C25(H25), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C20A(H20A),
C25A(H25A)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.23721(6) 0.9499(3) 0.06501(4) 0.0478(3) Uani 1 1 d . U . . .
V1 V 0.07300(11) 0.9505(5) -0.34233(8) 0.0650(6) Uani 1 1 d . U . . .
F10 F 0.0225(15) 0.7231(15) 0.1996(10) 0.094(7) Uiso 0.580(12) 1 d D U P A 1
F11 F 0.1547(19) 0.661(2) 0.2077(15) 0.152(13) Uiso 0.580(12) 1 d D U P A 1
F12 F 0.081(2) 0.6530(19) 0.1160(11) 0.134(10) Uiso 0.580(12) 1 d D U P A 1
F13 F 0.0350(12) 1.1848(12) 0.2027(9) 0.148(7) Uiso 1 1 d D U . . .
F14 F 0.1626(12) 1.2454(16) 0.1694(13) 0.123(7) Uiso 0.580(12) 1 d D U P A 1
F15 F 0.0317(14) 1.2743(13) 0.1198(10) 0.110(6) Uiso 0.580(12) 1 d D U P A 1
F16 F -0.1493(13) 1.0347(11) 0.0049(9) 0.084(5) Uiso 0.580(12) 1 d D U P A 1
F17 F -0.1133(16) 0.9004(11) 0.0245(10) 0.090(6) Uiso 0.580(12) 1 d D U P A 1
F18 F -0.0604(12) 0.9665(12) -0.0640(7) 0.052(5) Uiso 0.580(12) 1 d D U P A 1
O1 O 0.1130(10) 1.0395(10) -0.2736(6) 0.066(3) Uani 1 1 d . U . . .
O2 O 0.1142(11) 0.8650(11) -0.2715(7) 0.072(4) Uani 1 1 d . U . . .
O3 O 0.3693(11) 1.0427(9) 0.0703(6) 0.050(3) Uani 1 1 d . U . . .
O4 O 0.3717(11) 0.8554(10) 0.0739(7) 0.057(3) Uani 1 1 d . U . . .
O5 O 0.2746(5) 0.9504(14) 0.1815(3) 0.066(2) Uani 1 1 d . U . . .
O6 O 0.1746(10) 0.8210(9) 0.1098(7) 0.067(4) Uani 1 1 d . U . . .
O7 O 0.1727(10) 1.0797(9) 0.1114(6) 0.060(3) Uani 1 1 d . U . . .
O8 O 0.0772(4) 0.9508(13) 0.0365(3) 0.0557(16) Uani 1 1 d . U . . .
N1 N 0.2269(11) 1.0387(11) -0.0414(9) 0.047(3) Uani 1 1 d . U . . .
N2 N 0.2302(10) 0.8569(11) -0.0400(8) 0.043(3) Uani 1 1 d . U . . .
C1 C 0.2321(16) 1.1324(15) -0.0417(15) 0.061(5) Uani 1 1 d . U . . .
H1 H 0.250622 1.162206 -0.000943 0.073 Uiso 1 1 calc R . . . .
C2 C 0.2115(18) 1.1834(15) -0.0983(12) 0.068(6) Uani 1 1 d . U . . .
H2 H 0.217086 1.246952 -0.096609 0.081 Uiso 1 1 calc R . . . .
C3 C 0.1828(16) 1.1419(15) -0.1574(11) 0.065(5) Uani 1 1 d . U . . .
H3 H 0.170029 1.176970 -0.196814 0.078 Uiso 1 1 calc R . . . .
C4 C 0.1719(14) 1.0462(13) -0.1604(9) 0.050(4) Uani 1 1 d . U . . .
C5 C 0.1441(14) 0.9958(14) -0.2143(9) 0.052(4) Uani 1 1 d . U . . .
C6 C 0.1421(14) 0.9023(15) -0.2184(9) 0.056(4) Uani 1 1 d . U . . .
C7 C 0.1761(14) 0.8554(13) -0.1557(9) 0.048(4) Uani 1 1 d . U . . .
C8 C 0.1813(18) 0.7619(14) -0.1562(9) 0.061(5) Uani 1 1 d . U . . .
H8 H 0.162257 0.728467 -0.195206 0.073 Uiso 1 1 calc R . . . .
C9 C 0.2141(17) 0.7201(16) -0.0999(11) 0.064(5) Uani 1 1 d . U . . .
H9 H 0.222663 0.656844 -0.099631 0.077 Uiso 1 1 calc R . . . .
C10 C 0.2355(13) 0.7707(14) -0.0418(12) 0.050(4) Uani 1 1 d . U . . .
H10 H 0.254939 0.739979 -0.001690 0.060 Uiso 1 1 calc R . . . .
C11 C 0.2016(12) 0.9007(12) -0.0998(9) 0.039(3) Uani 1 1 d . U . . .
C12 C 0.2001(13) 0.9967(12) -0.0960(9) 0.043(3) Uani 1 1 d . U . . .
C13 C 0.5016(14) 1.1259(14) 0.1164(10) 0.092(6) Uani 1 1 d D U . . .
C14 C 0.444(2) 1.038(2) 0.1025(15) 0.110(8) Uani 1 1 d . U . . .
C15 C 0.4901(9) 0.950(2) 0.1196(5) 0.078(3) Uani 1 1 d . U . . .
H15 H 0.549525 0.949817 0.142589 0.094 Uiso 1 1 calc R . . . .
C16 C 0.4481(12) 0.8692(14) 0.1028(7) 0.055(3) Uani 1 1 d . U . . .
C17 C 0.4982(14) 0.7869(15) 0.1166(11) 0.093(5) Uani 1 1 d D U . . .
C19 C 0.288(4) 0.915(3) 0.227(2) 0.149(17) Uani 0.580(12) 1 d . U P A 1
C20 C 0.215(3) 0.838(3) 0.232(2) 0.100(11) Uani 0.580(12) 1 d . U P A 1
H20 H 0.198775 0.815453 0.275740 0.120 Uiso 0.580(12) 1 calc R . P A 1
C21 C 0.163(3) 0.796(3) 0.165(2) 0.102(13) Uani 0.580(12) 1 d . U P A 1
C22 C 0.1016(17) 0.7042(16) 0.1651(11) 0.129(10) Uiso 1 1 d D U . . .
C23 C 0.0830(14) 1.2089(14) 0.1468(11) 0.048(5) Uiso 0.580(12) 1 d D U P A 1
C24 C 0.096(2) 1.118(2) 0.1045(15) 0.063(7) Uani 0.580(12) 1 d . U P A 1
C25 C 0.018(2) 1.100(3) 0.0709(19) 0.077(9) Uani 0.580(12) 1 d . U P A 1
H25 H -0.032553 1.142375 0.069702 0.092 Uiso 0.580(12) 1 calc R . P A 1
C26 C 0.0085(19) 1.016(2) 0.0366(13) 0.057(6) Uani 0.580(12) 1 d . U P A 1
C27 C -0.0778(15) 0.9777(13) 0.0015(10) 0.052(7) Uiso 0.580(12) 1 d D U P A 1
C28 C -0.0713(14) 1.0234(16) -0.3335(11) 0.080(5) Uani 1 1 d D U . . .
H28 H -0.077842 1.084446 -0.320381 0.096 Uiso 1 1 calc R . . . .
C29 C -0.0620(15) 0.995(2) -0.4008(12) 0.083(5) Uani 1 1 d D U . . .
H29 H -0.055407 1.030334 -0.441066 0.100 Uiso 1 1 calc R . . . .
C30 C -0.0649(18) 0.901(2) -0.3933(13) 0.096(6) Uani 1 1 d D U . . .
H30 H -0.066199 0.861451 -0.431040 0.115 Uiso 1 1 calc R . . . .
C31 C -0.0659(15) 0.8724(19) -0.3258(13) 0.086(5) Uani 1 1 d D U . . .
H31 H -0.064163 0.812302 -0.309604 0.104 Uiso 1 1 calc R . . . .
C32 C -0.0699(7) 0.951(2) -0.2870(7) 0.088(4) Uani 1 1 d D U . . .
H32 H -0.071432 0.955589 -0.238656 0.105 Uiso 1 1 calc R . . . .
C33 C 0.1738(13) 1.0312(11) -0.4114(9) 0.044(5) Uiso 0.580(12) 1 d D U P A 1
C34 C 0.1227(10) 0.9710(8) -0.4534(7) 0.076(4) Uiso 1 1 d D U . . .
C35 C 0.1363(19) 0.8786(11) -0.4425(14) 0.077(8) Uiso 0.580(12) 1 d D U P A 1
C36 C 0.206(3) 0.8831(14) -0.3904(19) 0.114(12) Uiso 0.580(12) 1 d D U P A 1
C37 C 0.2312(9) 0.9725(8) -0.3722(7) 0.068(4) Uiso 1 1 d D U . . .
C38 C 0.1839(17) 0.9123(13) -0.4167(12) 0.048(7) Uiso 0.420(12) 1 d D U P A 2
C39 C 0.118(3) 1.0638(14) -0.438(2) 0.103(15) Uiso 0.420(12) 1 d D U P A 2
C40 C 0.196(3) 1.0578(16) -0.393(2) 0.066(9) Uiso 0.420(12) 1 d D U P A 2
F1 F 0.5182(15) 1.1705(13) 0.0643(7) 0.156(8) Uani 1 1 d D U . . .
F2 F 0.5803(12) 1.1082(13) 0.1487(11) 0.166(8) Uani 1 1 d D U . . .
F3 F 0.4505(15) 1.1742(13) 0.1604(7) 0.160(7) Uani 1 1 d D U . . .
F4 F 0.5774(10) 0.7904(14) 0.1529(8) 0.135(7) Uani 1 1 d D U . . .
F5 F 0.5224(17) 0.7477(16) 0.0608(8) 0.214(13) Uani 1 1 d D U . . .
F6 F 0.4465(10) 0.7282(12) 0.1498(13) 0.214(11) Uani 1 1 d D U . . .
F7 F 0.3945(14) 0.9789(17) 0.3017(14) 0.159(11) Uiso 0.580(12) 1 d D U P A 2
F8 F 0.3027(17) 0.8694(13) 0.3070(13) 0.126(8) Uiso 0.580(12) 1 d D U P A 2
F9 F 0.2539(17) 0.9962(17) 0.3389(17) 0.150(11) Uiso 0.580(12) 1 d D U P A 2
C18A C 0.3067(10) 0.9507(16) 0.2963(5) 0.100(5) Uani 1 1 d D U . . .
C19A C 0.2569(16) 0.9913(19) 0.2304(14) 0.026(5) Uiso 0.420(12) 1 d . U P A 2
C20A C 0.206(3) 1.079(3) 0.226(2) 0.060(11) Uiso 0.420(12) 1 d . U P A 2
H20A H 0.197768 1.114408 0.265711 0.072 Uiso 0.420(12) 1 calc R . P A 2
C21A C 0.176(3) 1.103(2) 0.1733(19) 0.042(8) Uiso 0.420(12) 1 d . U P A 2
C22A C 0.121(2) 1.194(2) 0.1793(15) 0.073(11) Uiso 0.420(12) 1 d D U P A 2
C23A C -0.076(2) 0.904(2) -0.0005(16) 0.070(13) Uiso 0.420(12) 1 d D U P A 2
C24A C 0.020(3) 0.893(3) 0.0385(18) 0.052(11) Uiso 0.420(12) 1 d . U P A 2
C25A C 0.011(4) 0.807(3) 0.069(2) 0.053(11) Uiso 0.420(12) 1 d . U P A 2
H25A H -0.045226 0.772534 0.063149 0.064 Uiso 0.420(12) 1 calc R . P A 2
C26A C 0.090(3) 0.774(3) 0.112(2) 0.050(10) Uiso 0.420(12) 1 d . U P A 2
F7A F 0.343(2) 1.0270(16) 0.3121(18) 0.124(12) Uiso 0.420(12) 1 d D U P A 1
F8A F 0.3740(15) 0.8889(15) 0.3108(13) 0.079(7) Uiso 0.420(12) 1 d D U P A 1
F9A F 0.2418(14) 0.931(2) 0.3472(13) 0.104(10) Uiso 0.420(12) 1 d D U P A 1
F10A F 0.1595(19) 1.253(2) 0.2207(13) 0.110(11) Uiso 0.420(12) 1 d D U P A 2
F11A F 0.1099(19) 1.2379(17) 0.1190(10) 0.081(7) Uiso 0.420(12) 1 d D U P A 2
F13A F -0.120(2) 0.9757(16) 0.0251(12) 0.098(9) Uiso 0.420(12) 1 d D U P A 2
F14A F -0.056(2) 0.9230(19) -0.0654(12) 0.067(8) Uiso 0.420(12) 1 d D U P A 2
F15A F -0.1404(19) 0.8400(14) -0.0036(15) 0.098(9) Uiso 0.420(12) 1 d D U P A 2
F16A F 0.0181(18) 0.668(3) 0.169(2) 0.195(19) Uiso 0.420(12) 1 d D U P A 2
F17A F 0.139(3) 0.698(3) 0.2249(14) 0.162(17) Uiso 0.420(12) 1 d D U P A 2
F18A F 0.152(2) 0.643(2) 0.1255(14) 0.116(10) Uiso 0.420(12) 1 d D U P A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Y1 0.0414(5) 0.0708(7) 0.0312(5) -0.0001(11) -0.0030(3) -0.0022(13)
V1 0.0335(8) 0.1285(17) 0.0329(8) 0.002(3) -0.0033(6) 0.002(3)
O1 0.065(8) 0.091(7) 0.040(7) 0.021(6) -0.010(6) -0.008(7)
O2 0.076(9) 0.097(7) 0.043(7) -0.015(6) -0.023(7) 0.003(8)
O3 0.049(6) 0.067(7) 0.036(6) -0.012(5) -0.005(5) -0.002(6)
O4 0.049(7) 0.078(7) 0.045(7) 0.004(6) -0.007(5) 0.007(6)
O5 0.068(4) 0.096(6) 0.034(3) -0.002(8) -0.002(3) 0.023(9)
O6 0.051(7) 0.089(8) 0.061(8) 0.026(7) 0.004(7) -0.007(7)
O7 0.050(6) 0.097(8) 0.032(6) -0.004(6) 0.001(6) 0.004(6)
O8 0.044(3) 0.081(5) 0.042(3) 0.015(8) -0.002(3) -0.007(7)
N1 0.044(8) 0.058(6) 0.038(6) -0.002(5) 0.009(6) -0.006(6)
N2 0.037(8) 0.057(6) 0.036(6) 0.007(5) -0.008(5) -0.004(6)
C1 0.059(14) 0.060(8) 0.064(12) 0.003(8) 0.000(10) -0.008(9)
C2 0.078(15) 0.052(10) 0.074(13) 0.006(7) -0.009(11) -0.003(10)
C3 0.049(11) 0.068(8) 0.076(12) 0.012(8) -0.018(10) -0.009(9)
C4 0.046(10) 0.069(7) 0.036(7) 0.006(6) 0.003(7) 0.001(8)
C5 0.043(10) 0.082(6) 0.032(7) 0.008(6) 0.001(7) -0.002(9)
C6 0.046(11) 0.086(6) 0.035(8) -0.005(6) -0.014(7) 0.005(9)
C7 0.038(9) 0.068(7) 0.039(7) -0.010(6) -0.012(7) 0.007(7)
C8 0.082(14) 0.062(8) 0.039(9) -0.011(6) -0.001(9) -0.008(9)
C9 0.071(13) 0.061(10) 0.061(11) 0.001(7) -0.007(10) 0.011(10)
C10 0.044(11) 0.060(7) 0.046(9) 0.019(7) -0.006(8) -0.003(7)
C11 0.032(9) 0.055(5) 0.031(7) 0.000(5) -0.003(6) 0.004(7)
C12 0.037(9) 0.056(5) 0.036(7) 0.002(5) 0.003(7) 0.004(7)
C13 0.098(13) 0.127(12) 0.052(10) -0.024(8) -0.016(8) -0.054(10)
C14 0.092(13) 0.103(9) 0.14(2) 0.010(12) -0.059(13) -0.025(10)
C15 0.066(7) 0.116(7) 0.053(6) -0.004(14) -0.012(5) -0.004(11)
C16 0.047(7) 0.095(7) 0.023(7) -0.003(6) 0.001(5) 0.002(6)
C17 0.076(11) 0.122(11) 0.080(13) 0.037(10) 0.001(9) 0.038(9)
C19 0.28(4) 0.10(2) 0.065(12) 0.018(11) -0.07(2) -0.05(2)
C20 0.13(3) 0.12(2) 0.050(14) 0.011(14) 0.001(14) 0.000(19)
C21 0.10(3) 0.15(3) 0.056(12) 0.032(13) -0.006(12) -0.03(2)
C24 0.043(9) 0.112(18) 0.034(12) -0.008(11) 0.020(8) 0.007(9)
C25 0.030(9) 0.117(17) 0.082(19) -0.017(14) 0.018(9) 0.001(11)
C26 0.028(9) 0.111(14) 0.032(11) 0.002(9) 0.010(8) 0.003(8)
C28 0.041(9) 0.094(9) 0.103(11) 0.016(10) 0.028(9) 0.002(8)
C29 0.035(9) 0.130(10) 0.085(9) 0.013(10) -0.001(8) -0.003(11)
C30 0.056(13) 0.131(10) 0.101(12) -0.010(11) -0.032(11) -0.022(13)
C31 0.034(9) 0.105(10) 0.120(14) 0.018(12) 0.008(10) 0.004(9)
C32 0.044(5) 0.134(10) 0.085(8) 0.020(12) 0.026(5) -0.002(13)
F1 0.22(2) 0.155(14) 0.098(10) 0.007(8) 0.002(10) -0.105(14)
F2 0.120(12) 0.155(17) 0.22(2) -0.035(12) -0.086(12) -0.040(10)
F3 0.227(18) 0.159(15) 0.093(9) -0.041(9) 0.024(10) 0.006(12)
F4 0.080(9) 0.20(2) 0.124(13) 0.013(11) -0.017(8) 0.029(10)
F5 0.27(3) 0.25(2) 0.123(13) -0.052(13) -0.070(12) 0.20(2)
F6 0.094(10) 0.154(15) 0.39(3) 0.169(18) -0.034(13) 0.005(9)
C18A 0.127(13) 0.140(15) 0.033(6) 0.026(14) -0.020(7) -0.03(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
Y1 O3 2.320(14) . ?
Y1 O4 2.367(15) . ?
Y1 O5 2.343(7) . ?
Y1 O6 2.288(13) . ?
Y1 O7 2.323(13) . ?
Y1 O8 2.323(6) . ?
Y1 N1 2.474(17) . ?
Y1 N2 2.482(17) . ?
V1 O1 1.972(16) . ?
V1 O2 1.971(16) . ?
V1 C28 2.31(2) . ?
V1 C29 2.32(2) . ?
V1 C30 2.30(2) . ?
V1 C31 2.30(2) . ?
V1 C32 2.287(10) . ?
V1 C33 2.30(2) . ?
V1 C34 2.308(14) . ?
V1 C36 2.32(4) . ?
V1 C37 2.328(13) . ?
V1 C38 2.21(3) . ?
F10 C22 1.33(2) . ?
F11 C22 1.29(2) . ?
F12 C22 1.26(2) . ?
F13 C23 1.336(19) . ?
F13 C22A 1.31(2) . ?
F14 C23 1.32(2) . ?
F15 C23 1.32(2) . ?
F16 C27 1.32(2) . ?
F17 C27 1.34(2) . ?
F18 C27 1.317(19) . ?
O1 C5 1.40(2) . ?
O2 C6 1.24(2) . ?
O3 C14 1.23(3) . ?
O4 C16 1.23(2) . ?
O5 C19 1.06(4) . ?
O5 C19A 1.16(3) . ?
O6 C21 1.16(4) . ?
O6 C26A 1.39(4) . ?
O7 C24 1.23(3) . ?
O7 C21A 1.26(4) . ?
O8 C26 1.37(3) . ?
O8 C24A 1.18(4) . ?
N1 C1 1.40(3) . ?
N1 C12 1.30(2) . ?
N2 C10 1.29(3) . ?
N2 C11 1.40(2) . ?
C1 C2 1.38(3) . ?
C2 C3 1.37(3) . ?
C3 C4 1.44(3) . ?
C4 C5 1.35(3) . ?
C4 C12 1.52(2) . ?
C5 C6 1.396(15) . ?
C6 C7 1.49(3) . ?
C7 C8 1.39(3) . ?
C7 C11 1.34(2) . ?
C8 C9 1.35(3) . ?
C9 C10 1.40(3) . ?
C11 C12 1.431(13) . ?
C13 C14 1.56(3) . ?
C13 F1 1.240(19) . ?
C13 F2 1.304(18) . ?
C13 F3 1.334(19) . ?
C14 C15 1.50(4) . ?
C15 C16 1.38(3) . ?
C16 C17 1.44(3) . ?
C17 F4 1.325(19) . ?
C17 F5 1.29(2) . ?
C17 F6 1.311(19) . ?
C19 C20 1.54(6) . ?
C19 C18A 1.48(4) . ?
C20 C21 1.62(6) . ?
C21 C22 1.62(5) . ?
C22 C26A 1.48(5) . ?
C22 F16A 1.30(2) . ?
C22 F17A 1.29(2) . ?
C22 F18A 1.39(2) . ?
C23 C24 1.59(4) . ?
C24 C25 1.32(5) . ?
C25 C26 1.42(5) . ?
C26 C27 1.51(4) . ?
C28 C29 1.388(17) . ?
C28 C32 1.408(17) . ?
C29 C30 1.407(15) . ?
C30 C31 1.393(18) . ?
C31 C32 1.403(17) . ?
C33 C34 1.415(13) . ?
C33 C37 1.418(13) . ?
C34 C35 1.406(14) . ?
C34 C38 1.423(13) . ?
C34 C39 1.415(14) . ?
C34 C40 2.03(4) . ?
C35 C36 1.417(14) . ?
C36 C37 1.424(14) . ?
C37 C38 1.417(13) . ?
C37 C40 1.426(14) . ?
C39 C40 1.413(14) . ?
F7 C18A 1.309(19) . ?
F8 C18A 1.23(2) . ?
F9 C18A 1.31(2) . ?
C18A C19A 1.59(3) . ?
C18A F7A 1.29(2) . ?
C18A F8A 1.351(19) . ?
C18A F9A 1.383(19) . ?
C19A C20A 1.49(5) . ?
C20A C21A 1.17(5) . ?
C21A C22A 1.57(5) . ?
C22A F10A 1.31(2) . ?
C22A F11A 1.36(2) . ?
C23A C24A 1.56(6) . ?
C23A F13A 1.34(2) . ?
C23A F14A 1.33(2) . ?
C23A F15A 1.31(2) . ?
C24A C25A 1.42(6) . ?
C25A C26A 1.48(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
O3 Y1 O4 73.1(2) . . ?
O3 Y1 O5 77.0(5) . . ?
O3 Y1 O7 78.5(5) . . ?
O3 Y1 O8 141.8(6) . . ?
O3 Y1 N1 76.5(5) . . ?
O3 Y1 N2 113.7(5) . . ?
O4 Y1 N1 115.3(5) . . ?
O4 Y1 N2 76.2(5) . . ?
O5 Y1 O4 75.5(5) . . ?
O5 Y1 N1 146.4(7) . . ?
O5 Y1 N2 144.9(6) . . ?
O6 Y1 O3 142.4(5) . . ?
O6 Y1 O4 77.4(5) . . ?
O6 Y1 O5 73.5(6) . . ?
O6 Y1 O7 113.4(3) . . ?
O6 Y1 O8 73.9(5) . . ?
O6 Y1 N1 138.5(5) . . ?
O6 Y1 N2 80.5(5) . . ?
O7 Y1 O4 141.2(5) . . ?
O7 Y1 O5 72.8(5) . . ?
O7 Y1 O8 73.1(5) . . ?
O7 Y1 N1 82.1(5) . . ?
O7 Y1 N2 140.7(5) . . ?
O8 Y1 O4 143.0(6) . . ?
O8 Y1 O5 116.9(2) . . ?
O8 Y1 N1 74.8(5) . . ?
O8 Y1 N2 76.4(5) . . ?
N1 Y1 N2 66.2(3) . . ?
O1 V1 C28 83.3(8) . . ?
O1 V1 C29 112.2(9) . . ?
O1 V1 C30 138.6(10) . . ?
O1 V1 C31 119.1(8) . . ?
O1 V1 C32 85.6(8) . . ?
O1 V1 C33 82.8(6) . . ?
O1 V1 C34 118.0(5) . . ?
O1 V1 C36 109.7(7) . . ?
O1 V1 C37 78.7(5) . . ?
O1 V1 C38 114.9(6) . . ?
O2 V1 O1 82.5(3) . . ?
O2 V1 C28 120.7(7) . . ?
O2 V1 C29 140.9(9) . . ?
O2 V1 C30 110.5(9) . . ?
O2 V1 C31 79.9(8) . . ?
O2 V1 C32 86.0(7) . . ?
O2 V1 C33 124.8(6) . . ?
O2 V1 C34 131.4(6) . . ?
O2 V1 C36 76.6(10) . . ?
O2 V1 C37 89.2(6) . . ?
O2 V1 C38 95.2(7) . . ?
C28 V1 C29 34.9(5) . . ?
C28 V1 C36 160.4(10) . . ?
C28 V1 C37 142.6(7) . . ?
C29 V1 C36 125.8(10) . . ?
C29 V1 C37 128.3(7) . . ?
C30 V1 C28 55.9(10) . . ?
C30 V1 C29 35.4(4) . . ?
C30 V1 C34 83.6(7) . . ?
C30 V1 C36 111.5(10) . . ?
C30 V1 C37 138.0(8) . . ?
C31 V1 C28 58.6(5) . . ?
C31 V1 C29 61.2(9) . . ?
C31 V1 C30 35.2(5) . . ?
C31 V1 C33 150.7(7) . . ?
C31 V1 C34 117.3(7) . . ?
C31 V1 C36 121.6(9) . . ?
C31 V1 C37 157.2(8) . . ?
C32 V1 C28 35.7(4) . . ?
C32 V1 C29 60.7(7) . . ?
C32 V1 C30 57.7(9) . . ?
C32 V1 C31 35.6(5) . . ?
C32 V1 C33 145.0(8) . . ?
C32 V1 C34 135.5(5) . . ?
C32 V1 C36 154.7(10) . . ?
C32 V1 C37 164.0(7) . . ?
C33 V1 C28 109.9(7) . . ?
C33 V1 C29 93.7(7) . . ?
C33 V1 C30 115.5(7) . . ?
C33 V1 C34 35.8(4) . . ?
C33 V1 C36 59.4(8) . . ?
C33 V1 C37 35.7(4) . . ?
C34 V1 C28 105.9(6) . . ?
C34 V1 C29 75.2(7) . . ?
C34 V1 C36 55.3(9) . . ?
C34 V1 C37 56.9(5) . . ?
C36 V1 C37 35.7(4) . . ?
C38 V1 C28 142.3(7) . . ?
C38 V1 C29 109.1(7) . . ?
C38 V1 C30 103.2(9) . . ?
C38 V1 C31 124.3(9) . . ?
C38 V1 C32 159.4(8) . . ?
C38 V1 C34 36.6(4) . . ?
C38 V1 C37 36.3(4) . . ?
C5 O1 V1 110.1(12) . . ?
C6 O2 V1 113.2(14) . . ?
C14 O3 Y1 132.5(16) . . ?
C16 O4 Y1 129.3(13) . . ?
C19 O5 Y1 150(3) . . ?
C19A O5 Y1 139.2(17) . . ?
C21 O6 Y1 133(3) . . ?
C26A O6 Y1 140.3(19) . . ?
C24 O7 Y1 133.7(18) . . ?
C21A O7 Y1 126.0(17) . . ?
C26 O8 Y1 133.4(17) . . ?
C24A O8 Y1 131(2) . . ?
C1 N1 Y1 122.3(15) . . ?
C12 N1 Y1 117.1(13) . . ?
C12 N1 C1 120(2) . . ?
C10 N2 Y1 125.3(14) . . ?
C10 N2 C11 117.2(18) . . ?
C11 N2 Y1 116.5(12) . . ?
C2 C1 N1 123(2) . . ?
C3 C2 C1 120(2) . . ?
C2 C3 C4 121(2) . . ?
C3 C4 C12 114.9(16) . . ?
C5 C4 C3 127.8(18) . . ?
C5 C4 C12 117.2(17) . . ?
C4 C5 O1 118.7(18) . . ?
C4 C5 C6 127(2) . . ?
C6 C5 O1 114(2) . . ?
O2 C6 C5 120(2) . . ?
O2 C6 C7 126(2) . . ?
C5 C6 C7 114(2) . . ?
C8 C7 C6 118.6(17) . . ?
C11 C7 C6 121.6(18) . . ?
C11 C7 C8 119.8(17) . . ?
C9 C8 C7 118.2(18) . . ?
C8 C9 C10 119(2) . . ?
N2 C10 C9 123(2) . . ?
N2 C11 C12 115.1(18) . . ?
C7 C11 N2 121.9(17) . . ?
C7 C11 C12 123.0(19) . . ?
N1 C12 C4 122.0(17) . . ?
N1 C12 C11 121(2) . . ?
C11 C12 C4 116.5(19) . . ?
F1 C13 C14 113.8(18) . . ?
F1 C13 F2 110.4(17) . . ?
F1 C13 F3 110.1(17) . . ?
F2 C13 C14 110.9(19) . . ?
F2 C13 F3 104.7(14) . . ?
F3 C13 C14 106.5(19) . . ?
O3 C14 C13 119(2) . . ?
O3 C14 C15 122(2) . . ?
C15 C14 C13 117.8(19) . . ?
C16 C15 C14 121.4(10) . . ?
O4 C16 C15 129.0(19) . . ?
O4 C16 C17 111.8(18) . . ?
C15 C16 C17 119.1(18) . . ?
F4 C17 C16 119(2) . . ?
F5 C17 C16 110.9(17) . . ?
F5 C17 F4 104.6(16) . . ?
F5 C17 F6 105.5(19) . . ?
F6 C17 C16 112.9(16) . . ?
F6 C17 F4 103.2(15) . . ?
O5 C19 C20 107(4) . . ?
O5 C19 C18A 129(4) . . ?
C18A C19 C20 109(3) . . ?
C19 C20 C21 123(3) . . ?
O6 C21 C20 124(4) . . ?
O6 C21 C22 110(3) . . ?
C22 C21 C20 125(3) . . ?
F10 C22 C21 105(2) . . ?
F11 C22 F10 105.1(19) . . ?
F11 C22 C21 96(3) . . ?
F12 C22 F10 109(2) . . ?
F12 C22 F11 109(2) . . ?
F12 C22 C21 130(3) . . ?
F16A C22 C26A 104(3) . . ?
F16A C22 F18A 103(2) . . ?
F17A C22 C26A 138(3) . . ?
F17A C22 F16A 106(2) . . ?
F17A C22 F18A 104(2) . . ?
F18A C22 C26A 97(2) . . ?
F13 C23 C24 105.0(19) . . ?
F14 C23 F13 105.4(17) . . ?
F14 C23 F15 107.1(17) . . ?
F14 C23 C24 115(2) . . ?
F15 C23 F13 104.4(16) . . ?
F15 C23 C24 119(2) . . ?
O7 C24 C23 116(3) . . ?
O7 C24 C25 134(3) . . ?
C25 C24 C23 110(3) . . ?
C24 C25 C26 120(4) . . ?
O8 C26 C25 124(3) . . ?
O8 C26 C27 107(2) . . ?
C25 C26 C27 129(3) . . ?
F16 C27 F17 104.6(16) . . ?
F16 C27 C26 110(2) . . ?
F17 C27 C26 118(2) . . ?
F18 C27 F16 105.9(16) . . ?
F18 C27 F17 106.9(17) . . ?
F18 C27 C26 110.0(18) . . ?
C29 C28 V1 72.9(12) . . ?
C29 C28 C32 112.7(19) . . ?
C32 C28 V1 71.2(9) . . ?
C28 C29 V1 72.2(12) . . ?
C28 C29 C30 101(3) . . ?
C30 C29 V1 71.7(16) . . ?
C29 C30 V1 72.9(16) . . ?
C31 C30 V1 72.2(13) . . ?
C31 C30 C29 114(3) . . ?
C30 C31 V1 72.6(13) . . ?
C30 C31 C32 105(2) . . ?
C32 C31 V1 71.7(10) . . ?
C28 C32 V1 73.1(10) . . ?
C31 C32 V1 72.7(11) . . ?
C31 C32 C28 106.8(13) . . ?
C34 C33 V1 72.4(9) . . ?
C34 C33 C37 102.4(13) . . ?
C37 C33 V1 73.2(9) . . ?
C33 C34 V1 71.9(9) . . ?
C35 C34 V1 76.5(12) . . ?
C35 C34 C33 117.5(17) . . ?
C38 C34 V1 68.0(13) . . ?
C38 C34 C40 77.9(10) . . ?
C39 C34 V1 85(2) . . ?
C39 C34 C38 121.6(18) . . ?
C39 C34 C40 44.1(12) . . ?
C40 C34 V1 71.8(11) . . ?
C34 C35 V1 68.8(11) . . ?
C34 C35 C36 99(2) . . ?
C36 C35 V1 69.4(18) . . ?
C35 C36 V1 75.8(17) . . ?
C35 C36 C37 113(2) . . ?
C37 C36 V1 72.4(16) . . ?
C33 C37 V1 71.1(9) . . ?
C33 C37 C36 107.4(18) . . ?
C36 C37 V1 72.0(18) . . ?
C38 C37 V1 67.4(13) . . ?
C38 C37 C40 102.8(19) . . ?
C40 C37 V1 81.9(16) . . ?
C34 C38 V1 75.4(12) . . ?
C37 C38 V1 76.4(12) . . ?
C37 C38 C34 102.0(14) . . ?
C40 C39 C34 92(2) . . ?
C34 C40 V1 59.1(10) . . ?
C37 C40 V1 64.5(13) . . ?
C37 C40 C34 77.2(16) . . ?
C39 C40 V1 76(2) . . ?
C39 C40 C34 44.1(12) . . ?
C39 C40 C37 121(3) . . ?
F7 C18A C19A 111.1(19) . . ?
F8 C18A F7 110.3(17) . . ?
F8 C18A F9 112.1(18) . . ?
F8 C18A C19A 119(2) . . ?
F9 C18A F7 108.7(17) . . ?
F9 C18A C19A 94(2) . . ?
F7A C18A C19 128(3) . . ?
F7A C18A F8A 105.7(16) . . ?
F7A C18A F9A 106.0(17) . . ?
F8A C18A C19 94(3) . . ?
F8A C18A F9A 99.8(14) . . ?
F9A C18A C19 118(3) . . ?
O5 C19A C18A 112(2) . . ?
O5 C19A C20A 121(3) . . ?
C20A C19A C18A 126(3) . . ?
C21A C20A C19A 120(4) . . ?
O7 C21A C22A 107(3) . . ?
C20A C21A O7 141(4) . . ?
C20A C21A C22A 112(4) . . ?
F13 C22A C21A 113(3) . . ?
F13 C22A F10A 104(2) . . ?
F13 C22A F11A 104(2) . . ?
F10A C22A C21A 115(3) . . ?
F10A C22A F11A 105(2) . . ?
F11A C22A C21A 114(3) . . ?
F13A C23A C24A 107(3) . . ?
F14A C23A C24A 108(3) . . ?
F14A C23A F13A 106(2) . . ?
F15A C23A C24A 123(3) . . ?
F15A C23A F13A 106(2) . . ?
F15A C23A F14A 105(2) . . ?
O8 C24A C23A 120(3) . . ?
O8 C24A C25A 137(4) . . ?
C25A C24A C23A 103(3) . . ?
C24A C25A C26A 118(4) . . ?
O6 C26A C22 106(3) . . ?
O6 C26A C25A 117(3) . . ?
C22 C26A C25A 136(4) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Y1 O3 C14 C13 -157.3(14) . . . . ?
Y1 O3 C14 C15 33(4) . . . . ?
Y1 O4 C16 C15 -22(3) . . . . ?
Y1 O4 C16 C17 160.4(12) . . . . ?
Y1 O5 C19 C20 -43(9) . . . . ?
Y1 O5 C19 C18A -176.8(11) . . . . ?
Y1 O5 C19A C18A 178.0(14) . . . . ?
Y1 O5 C19A C20A -11(4) . . . . ?
Y1 O6 C21 C20 -17(7) . . . . ?
Y1 O6 C21 C22 172.1(14) . . . . ?
Y1 O6 C26A C22 -167.9(15) . . . . ?
Y1 O6 C26A C25A 6(5) . . . . ?
Y1 O7 C24 C23 -179.1(12) . . . . ?
Y1 O7 C24 C25 5(5) . . . . ?
Y1 O7 C21A C20A 0(7) . . . . ?
Y1 O7 C21A C22A -179.0(14) . . . . ?
Y1 O8 C26 C25 -15(3) . . . . ?
Y1 O8 C26 C27 170.9(10) . . . . ?
Y1 O8 C24A C23A -164.3(17) . . . . ?
Y1 O8 C24A C25A 16(3) . . . . ?
Y1 N1 C1 C2 -169.3(18) . . . . ?
Y1 N1 C12 C4 167.4(13) . . . . ?
Y1 N1 C12 C11 -17(3) . . . . ?
Y1 N2 C10 C9 167.9(16) . . . . ?
Y1 N2 C11 C7 -165.8(14) . . . . ?
Y1 N2 C11 C12 13(2) . . . . ?
V1 O1 C5 C4 -178.1(15) . . . . ?
V1 O1 C5 C6 2(3) . . . . ?
V1 O2 C6 C5 -2(3) . . . . ?
V1 O2 C6 C7 179.0(16) . . . . ?
V1 C28 C29 C30 66.4(19) . . . . ?
V1 C28 C32 C31 -65.4(10) . . . . ?
V1 C29 C30 C31 61(2) . . . . ?
V1 C30 C31 C32 65.0(14) . . . . ?
V1 C31 C32 C28 65.7(9) . . . . ?
V1 C33 C34 C35 -63.4(14) . . . . ?
V1 C33 C37 C36 63(2) . . . . ?
V1 C34 C35 C36 -63.6(18) . . . . ?
V1 C34 C38 C37 -72.3(15) . . . . ?
V1 C34 C39 C40 69(3) . . . . ?
V1 C35 C36 C37 -63(2) . . . . ?
V1 C36 C37 C33 -62.7(14) . . . . ?
V1 C37 C38 C34 71.5(15) . . . . ?
V1 C37 C40 C34 -61.7(8) . . . . ?
V1 C37 C40 C39 -54(4) . . . . ?
F13 C23 C24 O7 -97(3) . . . . ?
F13 C23 C24 C25 80(3) . . . . ?
F14 C23 C24 O7 18(3) . . . . ?
F14 C23 C24 C25 -165(3) . . . . ?
F15 C23 C24 O7 147(2) . . . . ?
F15 C23 C24 C25 -36(3) . . . . ?
O1 C5 C6 O2 0(4) . . . . ?
O1 C5 C6 C7 179.4(12) . . . . ?
O2 C6 C7 C8 3(3) . . . . ?
O2 C6 C7 C11 -177(2) . . . . ?
O3 C14 C15 C16 -3(3) . . . . ?
O4 C16 C17 F4 -174.0(17) . . . . ?
O4 C16 C17 F5 65(2) . . . . ?
O4 C16 C17 F6 -53(2) . . . . ?
O5 C19 C20 C21 25(7) . . . . ?
O5 C19 C18A F7A -28(8) . . . . ?
O5 C19 C18A F8A -141(6) . . . . ?
O5 C19 C18A F9A 116(6) . . . . ?
O5 C19A C20A C21A 6(6) . . . . ?
O6 C21 C22 F10 -119(3) . . . . ?
O6 C21 C22 F11 134(3) . . . . ?
O6 C21 C22 F12 12(5) . . . . ?
O7 C24 C25 C26 5(6) . . . . ?
O7 C21A C22A F13 100(3) . . . . ?
O7 C21A C22A F10A -141(3) . . . . ?
O7 C21A C22A F11A -19(3) . . . . ?
O8 C26 C27 F16 174.7(16) . . . . ?
O8 C26 C27 F17 54(2) . . . . ?
O8 C26 C27 F18 -69(2) . . . . ?
O8 C24A C25A C26A 0(3) . . . . ?
N1 C1 C2 C3 1(4) . . . . ?
N2 C11 C12 N1 2(3) . . . . ?
N2 C11 C12 C4 178.5(12) . . . . ?
C1 N1 C12 C4 -1(3) . . . . ?
C1 N1 C12 C11 175(2) . . . . ?
C1 C2 C3 C4 1(4) . . . . ?
C2 C3 C4 C5 180(2) . . . . ?
C2 C3 C4 C12 -4(3) . . . . ?
C3 C4 C5 O1 -7(3) . . . . ?
C3 C4 C5 C6 174(3) . . . . ?
C3 C4 C12 N1 4(3) . . . . ?
C3 C4 C12 C11 -172(2) . . . . ?
C4 C5 C6 O2 179.6(16) . . . . ?
C4 C5 C6 C7 -1(4) . . . . ?
C5 C4 C12 N1 -179.4(18) . . . . ?
C5 C4 C12 C11 5(3) . . . . ?
C5 C6 C7 C8 -177(2) . . . . ?
C5 C6 C7 C11 3(3) . . . . ?
C6 C7 C8 C9 179(2) . . . . ?
C6 C7 C11 N2 177.6(17) . . . . ?
C6 C7 C11 C12 -1(3) . . . . ?
C7 C8 C9 C10 4(3) . . . . ?
C7 C11 C12 N1 -178.7(14) . . . . ?
C7 C11 C12 C4 -3(3) . . . . ?
C8 C7 C11 N2 -3(3) . . . . ?
C8 C7 C11 C12 179(2) . . . . ?
C8 C9 C10 N2 -4(3) . . . . ?
C10 N2 C11 C7 3(2) . . . . ?
C10 N2 C11 C12 -178(2) . . . . ?
C11 N2 C10 C9 0(3) . . . . ?
C11 C7 C8 C9 -1(3) . . . . ?
C12 N1 C1 C2 -1(3) . . . . ?
C12 C4 C5 O1 176.8(16) . . . . ?
C12 C4 C5 C6 -3(4) . . . . ?
C13 C14 C15 C16 -174(2) . . . . ?
C14 C15 C16 O4 -1(2) . . . . ?
C14 C15 C16 C17 176(2) . . . . ?
C15 C16 C17 F4 9(2) . . . . ?
C15 C16 C17 F5 -112(2) . . . . ?
C15 C16 C17 F6 129.4(19) . . . . ?
C19 C20 C21 O6 -2(8) . . . . ?
C19 C20 C21 C22 167(4) . . . . ?
C20 C19 C18A F7A -161(3) . . . . ?
C20 C19 C18A F8A 86(4) . . . . ?
C20 C19 C18A F9A -17(5) . . . . ?
C20 C21 C22 F10 70(5) . . . . ?
C20 C21 C22 F11 -37(5) . . . . ?
C20 C21 C22 F12 -158(4) . . . . ?
C23 C24 C25 C26 -172(2) . . . . ?
C24 C25 C26 O8 1(4) . . . . ?
C24 C25 C26 C27 173(3) . . . . ?
C25 C26 C27 F16 1(3) . . . . ?
C25 C26 C27 F17 -119(3) . . . . ?
C25 C26 C27 F18 118(3) . . . . ?
C28 C29 C30 V1 -66.8(16) . . . . ?
C28 C29 C30 C31 -6(4) . . . . ?
C29 C28 C32 V1 61.4(16) . . . . ?
C29 C28 C32 C31 -4.0(17) . . . . ?
C29 C30 C31 V1 -61(2) . . . . ?
C29 C30 C31 C32 4(3) . . . . ?
C30 C31 C32 V1 -65.6(16) . . . . ?
C30 C31 C32 C28 0.1(17) . . . . ?
C32 C28 C29 V1 -60.4(15) . . . . ?
C32 C28 C29 C30 6(3) . . . . ?
C33 C34 C35 V1 60.9(12) . . . . ?
C33 C34 C35 C36 -3(2) . . . . ?
C34 C33 C37 V1 -67.1(11) . . . . ?
C34 C33 C37 C36 -4(2) . . . . ?
C34 C35 C36 V1 63.2(13) . . . . ?
C34 C35 C36 C37 0(3) . . . . ?
C34 C39 C40 V1 -60(2) . . . . ?
C34 C39 C40 C37 -11(4) . . . . ?
C35 C36 C37 V1 65(2) . . . . ?
C35 C36 C37 C33 3(4) . . . . ?
C37 C33 C34 V1 67.7(11) . . . . ?
C37 C33 C34 C35 4.2(18) . . . . ?
C38 C34 C39 C40 8(4) . . . . ?
C38 C37 C40 V1 64.5(15) . . . . ?
C38 C37 C40 C34 2.8(19) . . . . ?
C38 C37 C40 C39 11(4) . . . . ?
C39 C34 C38 V1 69(3) . . . . ?
C39 C34 C38 C37 -3(4) . . . . ?
C40 C34 C38 V1 75.1(12) . . . . ?
C40 C34 C38 C37 2.8(19) . . . . ?
C40 C37 C38 V1 -75.5(18) . . . . ?
C40 C37 C38 C34 -4(3) . . . . ?
F1 C13 C14 O3 -52(3) . . . . ?
F1 C13 C14 C15 118(2) . . . . ?
F2 C13 C14 O3 -178(3) . . . . ?
F2 C13 C14 C15 -7(3) . . . . ?
F3 C13 C14 O3 69(3) . . . . ?
F3 C13 C14 C15 -120(2) . . . . ?
F7 C18A C19A O5 83(3) . . . . ?
F7 C18A C19A C20A -87(3) . . . . ?
F8 C18A C19A O5 -47(3) . . . . ?
F8 C18A C19A C20A 143(3) . . . . ?
F9 C18A C19A O5 -165(2) . . . . ?
F9 C18A C19A C20A 24(3) . . . . ?
C18A C19 C20 C21 168(4) . . . . ?
C18A C19A C20A C21A 176(3) . . . . ?
C19A C20A C21A O7 -2(8) . . . . ?
C19A C20A C21A C22A 178(3) . . . . ?
C20A C21A C22A F13 -79(4) . . . . ?
C20A C21A C22A F10A 40(4) . . . . ?
C20A C21A C22A F11A 162(3) . . . . ?
C23A C24A C25A C26A 180(3) . . . . ?
C24A C25A C26A O6 -10(4) . . . . ?
C24A C25A C26A C22 161(4) . . . . ?
F13A C23A C24A O8 -60(3) . . . . ?
F13A C23A C24A C25A 119(2) . . . . ?
F14A C23A C24A O8 54(3) . . . . ?
F14A C23A C24A C25A -127(2) . . . . ?
F15A C23A C24A O8 176(2) . . . . ?
F15A C23A C24A C25A -4(3) . . . . ?
F16A C22 C26A O6 174(3) . . . . ?
F16A C22 C26A C25A 2(5) . . . . ?
F17A C22 C26A O6 40(5) . . . . ?
F17A C22 C26A C25A -132(5) . . . . ?
F18A C22 C26A O6 -81(3) . . . . ?
F18A C22 C26A C25A 108(5) . . . . ?
_shelx_res_file
;
TITL mo_JHGLA075_0m in Pn21a #33
mo_jhgla075_0m.res
created by SHELXL-2016/6 at 09:28:45 on 26-Mar-2018
REM Best SHELXD solution FINAL CC 73.01
REM Fragments: 51 7 2 1 1 1
REM reset to Pn21a #33
CELL 0.71073 14.0879 14.8963 19.6006 90 90 90
ZERR 4 0.0007 0.0009 0.0012 0 0 0
LATT -1
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,+Y,0.5-Z
SYMM 0.5-X,0.5+Y,0.5+Z
SFAC C H F N O V Y
UNIT 148 76 72 8 32 4 4
DFIX 1.33 F2 C13 F1 C13 F3 C13 F4 C17 F5 C17 F6 C17 F9 C18A F8 C18A F8A =
C18A F7 C18A F7A C18A F9A C18A F10A C22A F13 C22A F13 C23 F14 C23 F11A C22A =
F15 C23 F17A C22 F11 C22 F18A C22 F12 C22 F16A C22 F10 C22 F13A C23A F14A =
C23A F15A C23A F17 C27 F16 C27 F18 C27
DFIX 1.42 0.01 C37 C38 C34 C38 C34 C39 C39 C40 C37 C40 C37 C36 C33 C37 C34 =
C33 C34 C35 C36 C35
SADI C31 C30 C29 C30 C29 C28 C32 C28 C31 C32
SADI F1 F2 F1 F3 F2 F3 F4 F5 F4 F6 F5 F6 F7 F8 F7 F9 F8 F9 F10 F11 F10 F12 =
F11 F12 F13 F14 F13 F15 F14 F15 F16 F17 F16 F18 F17 F18 F7A F8A F7A F9A F8A =
F9A F16A F17A F16A F18A F17A F18A F13 F10A F13 F11A F10A F11A F13A F14A =
F13A F15A F14A F15A
FLAT O8 C24A C25A C26A O6 C22
FLAT C33 C34 C35 C36 C37
RIGU
L.S. 10
PLAN 15
SIZE 0.01 0.08 0.19
TEMP -173.15
conf
list 4
fmap 2
acta
SHEL 100 0.83
TWIN -1 0 0 0 -1 0 0 0 1 2
OMIT 1 -1 1
REM
REM
REM
WGHT 0.126000 8.163013
BASF 0.52375
FVAR 0.28187 0.58033
Y1 7 0.237209 0.949907 0.065012 11.00000 0.04140 0.07077 =
0.03117 -0.00006 -0.00304 -0.00224
V1 6 0.072997 0.950468 -0.342332 11.00000 0.03353 0.12849 =
0.03292 0.00200 -0.00332 0.00221
PART 1
F10 3 0.022513 0.723109 0.199571 21.00000 0.09433
F11 3 0.154736 0.661255 0.207666 21.00000 0.15163
F12 3 0.080913 0.652971 0.116037 21.00000 0.13427
PART 0
F13 3 0.034986 1.184769 0.202663 11.00000 0.14824
PART 1
F14 3 0.162561 1.245441 0.169405 21.00000 0.12292
F15 3 0.031697 1.274326 0.119808 21.00000 0.11039
F16 3 -0.149276 1.034687 0.004884 21.00000 0.08351
F17 3 -0.113296 0.900352 0.024542 21.00000 0.09010
F18 3 -0.060437 0.966528 -0.064012 21.00000 0.05195
PART 0
O1 5 0.112952 1.039486 -0.273628 11.00000 0.06534 0.09122 =
0.04040 0.02131 -0.00956 -0.00779
O2 5 0.114219 0.864987 -0.271523 11.00000 0.07624 0.09686 =
0.04301 -0.01524 -0.02269 0.00271
O3 5 0.369265 1.042739 0.070297 11.00000 0.04866 0.06683 =
0.03598 -0.01245 -0.00545 -0.00248
O4 5 0.371718 0.855419 0.073925 11.00000 0.04911 0.07761 =
0.04457 0.00389 -0.00693 0.00683
O5 5 0.274559 0.950382 0.181478 11.00000 0.06756 0.09639 =
0.03446 -0.00183 -0.00165 0.02314
O6 5 0.174613 0.821018 0.109792 11.00000 0.05088 0.08863 =
0.06141 0.02618 0.00444 -0.00665
O7 5 0.172671 1.079748 0.111406 11.00000 0.05038 0.09749 =
0.03228 -0.00395 0.00139 0.00393
O8 5 0.077179 0.950810 0.036508 11.00000 0.04442 0.08114 =
0.04156 0.01457 -0.00199 -0.00664
N1 4 0.226933 1.038658 -0.041407 11.00000 0.04380 0.05797 =
0.03799 -0.00240 0.00947 -0.00611
N2 4 0.230219 0.856933 -0.039961 11.00000 0.03672 0.05676 =
0.03648 0.00694 -0.00827 -0.00400
C1 1 0.232089 1.132405 -0.041671 11.00000 0.05904 0.05959 =
0.06431 0.00286 0.00013 -0.00832
AFIX 43
H1 2 0.250622 1.162206 -0.000943 11.00000 -1.20000
AFIX 0
C2 1 0.211495 1.183439 -0.098344 11.00000 0.07783 0.05189 =
0.07386 0.00584 -0.00870 -0.00288
AFIX 43
H2 2 0.217086 1.246952 -0.096609 11.00000 -1.20000
AFIX 0
C3 1 0.182812 1.141877 -0.157401 11.00000 0.04930 0.06840 =
0.07639 0.01202 -0.01760 -0.00935
AFIX 43
H3 2 0.170029 1.176970 -0.196814 11.00000 -1.20000
AFIX 0
C4 1 0.171882 1.046161 -0.160394 11.00000 0.04594 0.06920 =
0.03580 0.00649 0.00257 0.00107
C5 1 0.144118 0.995818 -0.214324 11.00000 0.04283 0.08177 =
0.03226 0.00785 0.00074 -0.00225
C6 1 0.142124 0.902264 -0.218443 11.00000 0.04643 0.08613 =
0.03458 -0.00492 -0.01393 0.00547
C7 1 0.176088 0.855356 -0.155722 11.00000 0.03767 0.06821 =
0.03869 -0.01006 -0.01232 0.00721
C8 1 0.181298 0.761852 -0.156244 11.00000 0.08208 0.06167 =
0.03894 -0.01060 -0.00118 -0.00814
AFIX 43
H8 2 0.162257 0.728467 -0.195206 11.00000 -1.20000
AFIX 0
C9 1 0.214145 0.720106 -0.099858 11.00000 0.07110 0.06134 =
0.06057 0.00094 -0.00749 0.01073
AFIX 43
H9 2 0.222663 0.656844 -0.099631 11.00000 -1.20000
AFIX 0
C10 1 0.235528 0.770746 -0.041786 11.00000 0.04447 0.05981 =
0.04563 0.01861 -0.00628 -0.00303
AFIX 43
H10 2 0.254939 0.739979 -0.001690 11.00000 -1.20000
AFIX 0
C11 1 0.201565 0.900720 -0.099825 11.00000 0.03162 0.05509 =
0.03108 -0.00040 -0.00324 0.00412
C12 1 0.200083 0.996663 -0.095984 11.00000 0.03675 0.05562 =
0.03616 0.00153 0.00302 0.00409
C13 1 0.501558 1.125877 0.116369 11.00000 0.09805 0.12716 =
0.05168 -0.02447 -0.01559 -0.05358
C14 1 0.443906 1.038002 0.102456 11.00000 0.09181 0.10271 =
0.13553 0.00996 -0.05876 -0.02509
C15 1 0.490130 0.949936 0.119639 11.00000 0.06581 0.11598 =
0.05315 -0.00414 -0.01174 -0.00355
AFIX 43
H15 2 0.549525 0.949817 0.142589 11.00000 -1.20000
AFIX 0
C16 1 0.448123 0.869234 0.102784 11.00000 0.04737 0.09549 =
0.02337 -0.00263 0.00132 0.00243
C17 1 0.498185 0.786904 0.116588 11.00000 0.07630 0.12166 =
0.07963 0.03709 0.00138 0.03837
PART 1
C19 1 0.288388 0.914741 0.227054 21.00000 0.27754 0.10361 =
0.06536 0.01764 -0.07392 -0.04631
C20 1 0.214525 0.838499 0.231988 21.00000 0.12998 0.11969 =
0.05037 0.01079 0.00116 0.00049
AFIX 43
H20 2 0.198775 0.815453 0.275740 21.00000 -1.20000
AFIX 0
C21 1 0.162679 0.796117 0.165427 21.00000 0.09924 0.15045 =
0.05645 0.03194 -0.00584 -0.02824
PART 0
C22 1 0.101605 0.704239 0.165052 11.00000 0.12929
PART 1
C23 1 0.083036 1.208909 0.146817 21.00000 0.04777
C24 1 0.096376 1.118497 0.104472 21.00000 0.04338 0.11218 =
0.03384 -0.00827 0.01972 0.00688
C25 1 0.017797 1.099983 0.070947 21.00000 0.03031 0.11716 =
0.08217 -0.01691 0.01790 0.00058
AFIX 43
H25 2 -0.032553 1.142375 0.069702 21.00000 -1.20000
AFIX 0
C26 1 0.008505 1.016397 0.036621 21.00000 0.02822 0.11103 =
0.03245 0.00197 0.01039 0.00344
C27 1 -0.077831 0.977714 0.001456 21.00000 0.05200
PART 0
C28 1 -0.071280 1.023385 -0.333547 11.00000 0.04142 0.09439 =
0.10307 0.01618 0.02838 0.00227
AFIX 43
H28 2 -0.077842 1.084446 -0.320381 11.00000 -1.20000
AFIX 0
C29 1 -0.061994 0.995411 -0.400788 11.00000 0.03508 0.13009 =
0.08474 0.01255 -0.00136 -0.00345
AFIX 43
H29 2 -0.055407 1.030334 -0.441066 11.00000 -1.20000
AFIX 0
C30 1 -0.064949 0.901491 -0.393325 11.00000 0.05648 0.13101 =
0.10051 -0.00966 -0.03192 -0.02178
AFIX 43
H30 2 -0.066199 0.861451 -0.431040 11.00000 -1.20000
AFIX 0
C31 1 -0.065880 0.872386 -0.325803 11.00000 0.03386 0.10484 =
0.12017 0.01839 0.00830 0.00437
AFIX 43
H31 2 -0.064163 0.812302 -0.309604 11.00000 -1.20000
AFIX 0
C32 1 -0.069914 0.951427 -0.287008 11.00000 0.04443 0.13354 =
0.08507 0.01992 0.02627 -0.00207
AFIX 43
H32 2 -0.071432 0.955589 -0.238656 11.00000 -1.20000
AFIX 0
PART 1
C33 1 0.173758 1.031220 -0.411391 21.00000 0.04361
PART 0
C34 1 0.122677 0.970990 -0.453433 11.00000 0.07618
PART 1
C35 1 0.136261 0.878584 -0.442460 21.00000 0.07666
C36 1 0.205820 0.883073 -0.390362 21.00000 0.11432
PART 0
C37 1 0.231227 0.972496 -0.372247 11.00000 0.06845
PART 2
C38 1 0.183887 0.912334 -0.416737 -21.00000 0.04831
C39 1 0.117777 1.063772 -0.438404 -21.00000 0.10292
C40 1 0.195504 1.057787 -0.393061 -21.00000 0.06554
PART 0
F1 3 0.518165 1.170535 0.064332 11.00000 0.21556 0.15548 =
0.09834 0.00717 0.00168 -0.10451
F2 3 0.580270 1.108191 0.148732 11.00000 0.12002 0.15461 =
0.22370 -0.03525 -0.08615 -0.03969
F3 3 0.450470 1.174158 0.160358 11.00000 0.22655 0.15904 =
0.09295 -0.04081 0.02427 0.00573
F4 3 0.577444 0.790432 0.152913 11.00000 0.07960 0.19991 =
0.12401 0.01292 -0.01694 0.02894
F5 3 0.522408 0.747732 0.060799 11.00000 0.26642 0.25166 =
0.12311 -0.05238 -0.07011 0.20412
F6 3 0.446456 0.728243 0.149799 11.00000 0.09377 0.15395 =
0.39374 0.16946 -0.03400 0.00543
PART 2
F7 3 0.394466 0.978912 0.301681 21.00000 0.15870
F8 3 0.302658 0.869388 0.306952 21.00000 0.12592
F9 3 0.253943 0.996157 0.338858 21.00000 0.14999
PART 0
C18A 1 0.306748 0.950706 0.296323 11.00000 0.12683 0.13987 =
0.03282 0.02579 -0.02039 -0.02977
PART 2
C19A 1 0.256927 0.991334 0.230390 -21.00000 0.02616
C20A 1 0.206106 1.078620 0.226044 -21.00000 0.05967
AFIX 43
H20A 2 0.197768 1.114408 0.265711 -21.00000 -1.20000
AFIX 0
C21A 1 0.176389 1.102983 0.173328 -21.00000 0.04153
C22A 1 0.121390 1.193991 0.179315 -21.00000 0.07305
C23A 1 -0.075943 0.903545 -0.000515 -21.00000 0.06993
C24A 1 0.019736 0.892815 0.038510 -21.00000 0.05179
C25A 1 0.010565 0.807392 0.069420 -21.00000 0.05322
AFIX 43
H25A 2 -0.045226 0.772534 0.063149 -21.00000 -1.20000
AFIX 0
C26A 1 0.089911 0.773624 0.111745 -21.00000 0.04981
PART 0
PART 1
F7A 3 0.343315 1.027025 0.312094 -21.00000 0.12406
F8A 3 0.373972 0.888909 0.310845 -21.00000 0.07914
F9A 3 0.241826 0.931396 0.347202 -21.00000 0.10358
PART 0
PART 2
F10A 3 0.159497 1.253040 0.220728 -21.00000 0.11014
F11A 3 0.109929 1.237856 0.119034 -21.00000 0.08076
F13A 3 -0.119644 0.975726 0.025118 -21.00000 0.09846
F14A 3 -0.055711 0.922994 -0.065378 -21.00000 0.06672
F15A 3 -0.140356 0.840010 -0.003618 -21.00000 0.09780
F16A 3 0.018104 0.667683 0.169450 -21.00000 0.19468
F17A 3 0.139146 0.697677 0.224934 -21.00000 0.16224
F18A 3 0.151794 0.643189 0.125532 -21.00000 0.11610
HKLF 4
REM mo_JHGLA075_0m in Pn21a #33
REM R1 = 0.0687 for 4805 Fo > 4sig(Fo) and 0.1030 for all 6898 data
REM 594 parameters refined using 995 restraints
END
WGHT 0.1211 8.7556
REM Highest difference peak 0.688, deepest hole -0.478, 1-sigma level 0.099
Q1 1 0.1646 0.6931 0.1863 11.00000 0.05 0.69
Q2 1 0.2157 0.9440 -0.3960 11.00000 0.05 0.66
Q3 1 0.1851 1.3013 0.1970 11.00000 0.05 0.60
Q4 1 0.2180 1.1566 0.1343 11.00000 0.05 0.60
Q5 1 0.1854 0.6029 0.1955 11.00000 0.05 0.58
Q6 1 0.1981 0.6163 -0.0750 11.00000 0.05 0.57
Q7 1 0.3829 0.7808 0.1026 11.00000 0.05 0.56
Q8 1 0.3852 1.1203 0.1043 11.00000 0.05 0.56
Q9 1 0.1261 1.2360 0.2264 11.00000 0.05 0.56
Q10 1 0.1933 1.2874 -0.0742 11.00000 0.05 0.56
Q11 1 0.0722 1.2021 0.1080 11.00000 0.05 0.55
Q12 1 0.3048 0.7350 0.1398 11.00000 0.05 0.55
Q13 1 0.2213 0.7430 0.1359 11.00000 0.05 0.54
Q14 1 0.1638 1.0757 -0.4150 11.00000 0.05 0.54
Q15 1 0.0912 1.0171 -0.4576 11.00000 0.05 0.53
;
_shelx_res_checksum 17387
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.48(3)
2 0.52(3)