# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
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data_xdpm66
_database_code_depnum_ccdc_archive 'CCDC 1880942'
loop_
_audit_author_name
_audit_author_address
'Hannah Nicholas'
;The University of Manchester
United Kingdom
;
_audit_update_record
;
2018-11-23 deposited with the CCDC. 2019-09-18 downloaded from the CCDC.
;
_audit_creation_date 2018-08-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number 2013-2
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C24 B F20, C36 H84 N2 Si4 Sm'
_chemical_formula_sum 'C60 H84 B F20 N2 Si4 Sm'
_chemical_formula_weight 1486.81
_chemical_melting_point ?
_chemical_oxdiff_formula Sm(N(SiC9H21)2)2B(C6F5)4
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'
B B 0.0090 0.0039 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -5.3236 12.2178 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 19.9284(3)
_cell_length_b 17.0513(2)
_cell_length_c 21.1049(4)
_cell_angle_alpha 90
_cell_angle_beta 114.818(2)
_cell_angle_gamma 90
_cell_volume 6509.2(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 41785
_cell_measurement_temperature 100.0(2)
_cell_measurement_theta_max 73.4170
_cell_measurement_theta_min 2.5410
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 8.338
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.01770
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour 'clear red'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.517
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 3044
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.17
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0790
_diffrn_reflns_av_unetI/netI 0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 71543
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 68.251
_diffrn_reflns_theta_min 2.561
_diffrn_ambient_temperature 100.0(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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 70.71 257.71 1.00 10.00 -- 100.00 73.87 -25.79 187
2 \w 77.92 261.92 1.00 10.00 -- 105.00 73.87 129.21 184
3 \f 54.43 325.77 1.00 10.00 14.82 -70.00 73.87 -- 271
4 \f -23.96 326.48 1.00 10.00 158.57 105.00 73.87 -- 350
5 \f -19.93 277.26 1.00 10.00 74.83 55.00 73.87 -- 297
6 \w 32.88 103.88 1.00 10.00 -- -35.00 73.87 89.21 71
7 \f -25.10 265.26 1.00 10.00 167.64 80.00 73.87 -- 290
8 \w -71.60 62.40 1.00 10.00 -- -75.00 73.87-165.79 134
9 \f -25.79 181.34 1.00 10.00 136.84 95.00 73.87 -- 207
10 \w 58.71 197.71 1.00 10.00 -- 40.00 73.87 169.21 139
11 \f 85.32 325.47 1.00 10.00 85.84 110.00 73.87 -- 240
12 \w 123.21 268.21 1.00 10.00 -- 111.00 73.87 74.21 145
13 \w 122.34 256.34 1.00 10.00 -- 110.00 73.87 -40.79 134
14 \w 92.08 209.08 1.00 10.00 -- 80.00 73.87 29.21 117
15 \w -27.47 116.53 1.00 10.00 -- -2.00 73.87 149.21 144
16 \f 136.94 333.06 1.00 10.00 144.21 110.00 73.87 -- 196
;
_diffrn_measurement_device 'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0077671000
_diffrn_orient_matrix_UB_12 0.0595386000
_diffrn_orient_matrix_UB_13 -0.0514425000
_diffrn_orient_matrix_UB_21 -0.0668276000
_diffrn_orient_matrix_UB_22 0.0458092000
_diffrn_orient_matrix_UB_23 -0.0007480000
_diffrn_orient_matrix_UB_31 0.0522606000
_diffrn_orient_matrix_UB_32 0.0501507000
_diffrn_orient_matrix_UB_33 0.0618695000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 10921
_reflns_number_total 11897
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XH (Sheldrick, 2008)'
_computing_structure_solution 'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max 0.641
_refine_diff_density_min -1.339
_refine_diff_density_rms 0.086
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.052
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 817
_refine_ls_number_reflns 11897
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0405
_refine_ls_R_factor_gt 0.0361
_refine_ls_restrained_S_all 1.052
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+2.8187P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0919
_refine_ls_wR_factor_ref 0.0944
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16), C19(H19), C22(H22),
C25(H25), C28(H28), C31(H31), C34(H34)
2.b Idealised Me refined as rotating group:
C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,
H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C),
C36(H36A,H36B,H36C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.57842(2) 0.16770(2) 0.83163(2) 0.01724(6) Uani 1 1 d . . . . .
Si1 Si 0.41771(4) 0.15526(4) 0.83568(4) 0.01393(16) Uani 1 1 d . . . . .
Si2 Si 0.53609(4) 0.27973(4) 0.93881(4) 0.01457(16) Uani 1 1 d . . . . .
Si3 Si 0.60563(4) 0.08272(4) 0.70173(4) 0.01415(15) Uani 1 1 d . . . . .
Si4 Si 0.56476(4) 0.26429(4) 0.68877(4) 0.01336(15) Uani 1 1 d . . . . .
N1 N 0.49608(13) 0.21402(13) 0.87007(12) 0.0151(5) Uani 1 1 d . . . . .
N2 N 0.57857(14) 0.17107(12) 0.72615(12) 0.0136(5) Uani 1 1 d . . . . .
C1 C 0.45863(17) 0.05914(16) 0.81865(16) 0.0185(6) Uani 1 1 d . . . . .
H1 H 0.4795 0.0721 0.7844 0.022 Uiso 1 1 calc R . . . .
C2 C 0.52243(18) 0.02469(17) 0.88301(16) 0.0213(6) Uani 1 1 d . . . . .
H2A H 0.5605 0.0648 0.9043 0.032 Uiso 1 1 calc GR . . . .
H2B H 0.5438 -0.0202 0.8689 0.032 Uiso 1 1 calc GR . . . .
H2C H 0.5037 0.0074 0.9169 0.032 Uiso 1 1 calc GR . . . .
C3 C 0.40024(19) -0.00568(17) 0.78461(19) 0.0268(7) Uani 1 1 d . . . . .
H3A H 0.3745 -0.0166 0.8143 0.040 Uiso 1 1 calc GR . . . .
H3B H 0.4248 -0.0535 0.7793 0.040 Uiso 1 1 calc GR . . . .
H3C H 0.3645 0.0120 0.7386 0.040 Uiso 1 1 calc GR . . . .
C4 C 0.35019(16) 0.19125(17) 0.74643(15) 0.0175(6) Uani 1 1 d . . . . .
H4 H 0.3733 0.1782 0.7138 0.021 Uiso 1 1 calc R . . . .
C5 C 0.27356(18) 0.1518(2) 0.71544(18) 0.0273(7) Uani 1 1 d . . . . .
H5A H 0.2796 0.0947 0.7154 0.041 Uiso 1 1 calc GR . . . .
H5B H 0.2455 0.1702 0.6675 0.041 Uiso 1 1 calc GR . . . .
H5C H 0.2469 0.1653 0.7438 0.041 Uiso 1 1 calc GR . . . .
C6 C 0.33829(18) 0.28044(17) 0.74108(16) 0.0221(6) Uani 1 1 d . . . . .
H6A H 0.3086 0.2957 0.7661 0.033 Uiso 1 1 calc GR . . . .
H6B H 0.3124 0.2955 0.6919 0.033 Uiso 1 1 calc GR . . . .
H6C H 0.3863 0.3070 0.7619 0.033 Uiso 1 1 calc GR . . . .
C7 C 0.36142(17) 0.12980(17) 0.88590(15) 0.0190(6) Uani 1 1 d . . . . .
H7 H 0.3207 0.0961 0.8530 0.023 Uiso 1 1 calc R . . . .
C8 C 0.39592(18) 0.08037(18) 0.95278(16) 0.0228(6) Uani 1 1 d . . . . .
H8A H 0.4133 0.0304 0.9422 0.034 Uiso 1 1 calc GR . . . .
H8B H 0.3588 0.0704 0.9709 0.034 Uiso 1 1 calc GR . . . .
H8C H 0.4377 0.1088 0.9879 0.034 Uiso 1 1 calc GR . . . .
C9 C 0.32116(18) 0.20137(17) 0.89778(17) 0.0220(6) Uani 1 1 d . . . . .
H9A H 0.3571 0.2360 0.9327 0.033 Uiso 1 1 calc GR . . . .
H9B H 0.2846 0.1838 0.9145 0.033 Uiso 1 1 calc GR . . . .
H9C H 0.2961 0.2300 0.8538 0.033 Uiso 1 1 calc GR . . . .
C10 C 0.63709(17) 0.28284(17) 0.94956(15) 0.0191(6) Uani 1 1 d . . . . .
H10 H 0.6338 0.2892 0.9012 0.023 Uiso 1 1 calc R . . . .
C11 C 0.68367(17) 0.20766(19) 0.97849(16) 0.0235(7) Uani 1 1 d . . . . .
H11A H 0.7057 0.2089 1.0296 0.035 Uiso 1 1 calc GR . . . .
H11B H 0.7229 0.2051 0.9621 0.035 Uiso 1 1 calc GR . . . .
H11C H 0.6518 0.1614 0.9620 0.035 Uiso 1 1 calc GR . . . .
C12 C 0.68341(19) 0.3535(2) 0.99131(18) 0.0275(7) Uani 1 1 d . . . . .
H12A H 0.6603 0.4024 0.9679 0.041 Uiso 1 1 calc GR . . . .
H12B H 0.7335 0.3499 0.9938 0.041 Uiso 1 1 calc GR . . . .
H12C H 0.6857 0.3529 1.0386 0.041 Uiso 1 1 calc GR . . . .
C13 C 0.50064(17) 0.38406(16) 0.92125(15) 0.0190(6) Uani 1 1 d . . . . .
H13 H 0.5332 0.4153 0.9630 0.023 Uiso 1 1 calc R . . . .
C14 C 0.50679(19) 0.42269(17) 0.85802(17) 0.0247(7) Uani 1 1 d . . . . .
H14A H 0.5588 0.4242 0.8656 0.037 Uiso 1 1 calc GR . . . .
H14B H 0.4873 0.4762 0.8523 0.037 Uiso 1 1 calc GR . . . .
H14C H 0.4783 0.3922 0.8159 0.037 Uiso 1 1 calc GR . . . .
C15 C 0.42177(18) 0.39368(17) 0.91552(18) 0.0250(7) Uani 1 1 d . . . . .
H15A H 0.3872 0.3650 0.8746 0.038 Uiso 1 1 calc GR . . . .
H15B H 0.4086 0.4494 0.9106 0.038 Uiso 1 1 calc GR . . . .
H15C H 0.4191 0.3728 0.9577 0.038 Uiso 1 1 calc GR . . . .
C16 C 0.53121(17) 0.24774(17) 1.02314(15) 0.0187(6) Uani 1 1 d . . . . .
H16 H 0.4779 0.2366 1.0106 0.022 Uiso 1 1 calc R . . . .
C17 C 0.5731(2) 0.17245(17) 1.05729(17) 0.0249(7) Uani 1 1 d . . . . .
H17A H 0.5644 0.1324 1.0213 0.037 Uiso 1 1 calc GR . . . .
H17B H 0.5556 0.1532 1.0914 0.037 Uiso 1 1 calc GR . . . .
H17C H 0.6262 0.1837 1.0809 0.037 Uiso 1 1 calc GR . . . .
C18 C 0.55352(19) 0.31279(19) 1.07897(16) 0.0239(7) Uani 1 1 d . . . . .
H18A H 0.6051 0.3277 1.0920 0.036 Uiso 1 1 calc GR . . . .
H18B H 0.5480 0.2934 1.1203 0.036 Uiso 1 1 calc GR . . . .
H18C H 0.5216 0.3586 1.0601 0.036 Uiso 1 1 calc GR . . . .
C19 C 0.63195(16) 0.02013(15) 0.78396(15) 0.0157(6) Uani 1 1 d . . . . .
H19 H 0.5868 0.0184 0.7933 0.019 Uiso 1 1 calc R . . . .
C20 C 0.69425(17) 0.05383(17) 0.85138(15) 0.0204(6) Uani 1 1 d . . . . .
H20A H 0.7413 0.0288 0.8592 0.031 Uiso 1 1 calc GR . . . .
H20B H 0.6826 0.0434 0.8913 0.031 Uiso 1 1 calc GR . . . .
H20C H 0.6982 0.1105 0.8462 0.031 Uiso 1 1 calc GR . . . .
C21 C 0.65045(18) -0.06584(16) 0.77626(17) 0.0235(7) Uani 1 1 d . . . . .
H21A H 0.6095 -0.0895 0.7364 0.035 Uiso 1 1 calc GR . . . .
H21B H 0.6580 -0.0947 0.8189 0.035 Uiso 1 1 calc GR . . . .
H21C H 0.6956 -0.0681 0.7686 0.035 Uiso 1 1 calc GR . . . .
C22 C 0.52805(17) 0.03027(16) 0.62798(15) 0.0189(6) Uani 1 1 d . . . . .
H22 H 0.5490 -0.0205 0.6209 0.023 Uiso 1 1 calc R . . . .
C23 C 0.46202(18) 0.00948(18) 0.64389(17) 0.0244(7) Uani 1 1 d . . . . .
H23A H 0.4779 -0.0272 0.6833 0.037 Uiso 1 1 calc GR . . . .
H23B H 0.4233 -0.0150 0.6027 0.037 Uiso 1 1 calc GR . . . .
H23C H 0.4426 0.0573 0.6559 0.037 Uiso 1 1 calc GR . . . .
C24 C 0.50320(18) 0.07596(17) 0.55874(16) 0.0221(6) Uani 1 1 d . . . . .
H24A H 0.4859 0.1282 0.5644 0.033 Uiso 1 1 calc GR . . . .
H24B H 0.4629 0.0476 0.5218 0.033 Uiso 1 1 calc GR . . . .
H24C H 0.5450 0.0812 0.5460 0.033 Uiso 1 1 calc GR . . . .
C25 C 0.68577(16) 0.08941(16) 0.67579(15) 0.0167(6) Uani 1 1 d . . . . .
H25 H 0.6733 0.1327 0.6407 0.020 Uiso 1 1 calc R . . . .
C26 C 0.69568(18) 0.01482(17) 0.63914(16) 0.0217(6) Uani 1 1 d . . . . .
H26A H 0.7082 -0.0295 0.6716 0.033 Uiso 1 1 calc GR . . . .
H26B H 0.7355 0.0231 0.6242 0.033 Uiso 1 1 calc GR . . . .
H26C H 0.6495 0.0035 0.5983 0.033 Uiso 1 1 calc GR . . . .
C27 C 0.76019(17) 0.11144(19) 0.73540(17) 0.0243(7) Uani 1 1 d . . . . .
H27A H 0.7532 0.1560 0.7614 0.036 Uiso 1 1 calc GR . . . .
H27B H 0.7954 0.1259 0.7160 0.036 Uiso 1 1 calc GR . . . .
H27C H 0.7795 0.0666 0.7669 0.036 Uiso 1 1 calc GR . . . .
C28 C 0.46370(16) 0.28767(16) 0.66407(15) 0.0177(6) Uani 1 1 d . . . . .
H28 H 0.4559 0.2722 0.7062 0.021 Uiso 1 1 calc R . . . .
C29 C 0.40854(17) 0.23651(17) 0.60522(16) 0.0228(6) Uani 1 1 d . . . . .
H29A H 0.4118 0.2489 0.5612 0.034 Uiso 1 1 calc GR . . . .
H29B H 0.3583 0.2470 0.6004 0.034 Uiso 1 1 calc GR . . . .
H29C H 0.4204 0.1810 0.6165 0.034 Uiso 1 1 calc GR . . . .
C30 C 0.43766(18) 0.37350(17) 0.65101(17) 0.0231(7) Uani 1 1 d . . . . .
H30A H 0.4656 0.4047 0.6929 0.035 Uiso 1 1 calc GR . . . .
H30B H 0.3848 0.3761 0.6402 0.035 Uiso 1 1 calc GR . . . .
H30C H 0.4460 0.3944 0.6116 0.035 Uiso 1 1 calc GR . . . .
C31 C 0.61828(17) 0.33152(15) 0.76575(15) 0.0163(6) Uani 1 1 d . . . . .
H31 H 0.5899 0.3319 0.7951 0.020 Uiso 1 1 calc R . . . .
C32 C 0.69658(17) 0.30366(17) 0.81400(15) 0.0194(6) Uani 1 1 d . . . . .
H32A H 0.6944 0.2496 0.8288 0.029 Uiso 1 1 calc GR . . . .
H32B H 0.7171 0.3377 0.8552 0.029 Uiso 1 1 calc GR . . . .
H32C H 0.7282 0.3059 0.7889 0.029 Uiso 1 1 calc GR . . . .
C33 C 0.62364(18) 0.41772(17) 0.74698(17) 0.0242(7) Uani 1 1 d . . . . .
H33A H 0.6588 0.4222 0.7258 0.036 Uiso 1 1 calc GR . . . .
H33B H 0.6407 0.4498 0.7894 0.036 Uiso 1 1 calc GR . . . .
H33C H 0.5749 0.4360 0.7138 0.036 Uiso 1 1 calc GR . . . .
C34 C 0.59360(16) 0.27739(16) 0.61479(15) 0.0162(6) Uani 1 1 d . . . . .
H34 H 0.5814 0.2273 0.5876 0.019 Uiso 1 1 calc R . . . .
C35 C 0.54899(19) 0.34259(17) 0.56416(16) 0.0225(7) Uani 1 1 d . . . . .
H35A H 0.4962 0.3302 0.5455 0.034 Uiso 1 1 calc GR . . . .
H35B H 0.5641 0.3463 0.5257 0.034 Uiso 1 1 calc GR . . . .
H35C H 0.5583 0.3927 0.5891 0.034 Uiso 1 1 calc GR . . . .
C36 C 0.67673(17) 0.29283(17) 0.63660(16) 0.0207(6) Uani 1 1 d . . . . .
H36A H 0.6892 0.3458 0.6560 0.031 Uiso 1 1 calc GR . . . .
H36B H 0.6878 0.2880 0.5957 0.031 Uiso 1 1 calc GR . . . .
H36C H 0.7060 0.2544 0.6720 0.031 Uiso 1 1 calc GR . . . .
F1 F 0.63599(9) 0.23478(9) 0.25825(9) 0.0207(4) Uani 1 1 d . . . . .
F2 F 0.73129(10) 0.11632(10) 0.30566(10) 0.0244(4) Uani 1 1 d . . . . .
F3 F 0.76131(10) 0.05054(10) 0.43241(11) 0.0310(4) Uani 1 1 d . . . . .
F4 F 0.69234(11) 0.10764(11) 0.51063(10) 0.0293(4) Uani 1 1 d . . . . .
F5 F 0.59630(10) 0.22246(10) 0.46460(9) 0.0223(4) Uani 1 1 d . . . . .
F6 F 0.46822(10) 0.18319(9) 0.34969(10) 0.0230(4) Uani 1 1 d . . . . .
F7 F 0.36781(10) 0.19084(11) 0.40131(10) 0.0284(4) Uani 1 1 d . . . . .
F8 F 0.32907(11) 0.33231(10) 0.43712(11) 0.0296(4) Uani 1 1 d . . . . .
F9 F 0.39806(11) 0.46461(10) 0.42345(10) 0.0283(4) Uani 1 1 d . . . . .
F10 F 0.50414(10) 0.45828(9) 0.37932(9) 0.0204(4) Uani 1 1 d . . . . .
F11 F 0.59325(10) 0.39824(9) 0.22009(8) 0.0199(4) Uani 1 1 d . . . . .
F12 F 0.69116(10) 0.51264(10) 0.25094(10) 0.0263(4) Uani 1 1 d . . . . .
F13 F 0.76597(10) 0.56338(10) 0.38539(10) 0.0291(4) Uani 1 1 d . . . . .
F14 F 0.73837(11) 0.49505(11) 0.48834(9) 0.0300(4) Uani 1 1 d . . . . .
F15 F 0.64037(10) 0.37893(10) 0.45946(9) 0.0234(4) Uani 1 1 d . . . . .
F16 F 0.50173(10) 0.16054(8) 0.23146(9) 0.0201(4) Uani 1 1 d . . . . .
F17 F 0.39909(11) 0.15674(9) 0.10171(9) 0.0254(4) Uani 1 1 d . . . . .
F18 F 0.32623(11) 0.28904(11) 0.03761(9) 0.0295(4) Uani 1 1 d . . . . .
F19 F 0.36117(10) 0.42870(10) 0.10766(9) 0.0255(4) Uani 1 1 d . . . . .
F20 F 0.46448(9) 0.43457(9) 0.23792(9) 0.0203(4) Uani 1 1 d . . . . .
C37 C 0.60817(16) 0.23388(15) 0.35691(15) 0.0158(6) Uani 1 1 d . . . . .
C38 C 0.64656(16) 0.20376(16) 0.32098(15) 0.0166(6) Uani 1 1 d . . . . .
C39 C 0.69711(17) 0.14318(17) 0.34434(16) 0.0193(6) Uani 1 1 d . . . . .
C40 C 0.71279(16) 0.11011(16) 0.40886(17) 0.0207(6) Uani 1 1 d . . . . .
C41 C 0.67788(17) 0.13905(17) 0.44767(16) 0.0208(6) Uani 1 1 d . . . . .
C42 C 0.62754(17) 0.19924(16) 0.42196(15) 0.0182(6) Uani 1 1 d . . . . .
C43 C 0.49321(17) 0.31973(16) 0.36211(15) 0.0158(6) Uani 1 1 d . . . . .
C44 C 0.45418(17) 0.25493(16) 0.36873(15) 0.0182(6) Uani 1 1 d . . . . .
C45 C 0.40040(17) 0.25741(17) 0.39364(15) 0.0195(6) Uani 1 1 d . . . . .
C46 C 0.38114(18) 0.32843(17) 0.41177(17) 0.0214(7) Uani 1 1 d . . . . .
C47 C 0.41641(17) 0.39499(17) 0.40538(16) 0.0200(6) Uani 1 1 d . . . . .
C48 C 0.47145(16) 0.38969(16) 0.38196(15) 0.0164(6) Uani 1 1 d . . . . .
C49 C 0.60870(16) 0.38381(15) 0.33784(15) 0.0160(6) Uani 1 1 d . . . . .
C50 C 0.62651(17) 0.41984(16) 0.28802(15) 0.0170(6) Uani 1 1 d . . . . .
C51 C 0.67812(17) 0.47963(16) 0.30260(16) 0.0196(6) Uani 1 1 d . . . . .
C52 C 0.71592(17) 0.50507(16) 0.37020(17) 0.0212(6) Uani 1 1 d . . . . .
C53 C 0.70159(17) 0.47019(17) 0.42176(16) 0.0209(6) Uani 1 1 d . . . . .
C54 C 0.65017(17) 0.41122(16) 0.40531(15) 0.0184(6) Uani 1 1 d . . . . .
C55 C 0.49160(16) 0.29909(16) 0.24207(14) 0.0147(6) Uani 1 1 d . . . . .
C56 C 0.47014(17) 0.22983(16) 0.20394(16) 0.0179(6) Uani 1 1 d . . . . .
C57 C 0.41569(17) 0.22609(17) 0.13619(15) 0.0196(6) Uani 1 1 d . . . . .
C58 C 0.37882(17) 0.29255(18) 0.10308(15) 0.0201(6) Uani 1 1 d . . . . .
C59 C 0.39675(17) 0.36270(17) 0.13885(16) 0.0186(6) Uani 1 1 d . . . . .
C60 C 0.45090(16) 0.36384(16) 0.20600(15) 0.0158(6) Uani 1 1 d . . . . .
B1 B 0.55129(19) 0.30896(18) 0.32513(17) 0.0155(6) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sm1 0.01722(10) 0.02056(10) 0.01537(9) 0.00013(6) 0.00824(7) 0.00438(6)
Si1 0.0149(4) 0.0117(3) 0.0172(4) -0.0002(3) 0.0087(3) 0.0003(3)
Si2 0.0170(4) 0.0122(3) 0.0157(4) -0.0004(3) 0.0081(3) -0.0007(3)
Si3 0.0160(4) 0.0103(3) 0.0168(4) -0.0008(3) 0.0074(3) 0.0007(3)
Si4 0.0156(4) 0.0099(3) 0.0157(4) 0.0006(3) 0.0076(3) 0.0010(3)
N1 0.0173(12) 0.0134(11) 0.0163(12) 0.0005(9) 0.0087(10) 0.0012(10)
N2 0.0163(12) 0.0119(11) 0.0144(12) 0.0004(8) 0.0082(10) -0.0006(9)
C1 0.0206(15) 0.0134(13) 0.0251(15) -0.0007(11) 0.0130(13) 0.0004(12)
C2 0.0253(16) 0.0152(14) 0.0283(16) 0.0037(12) 0.0160(14) 0.0025(12)
C3 0.0283(17) 0.0143(14) 0.042(2) -0.0085(13) 0.0185(16) -0.0046(13)
C4 0.0158(15) 0.0199(14) 0.0157(14) -0.0007(11) 0.0054(12) 0.0001(12)
C5 0.0196(17) 0.0309(16) 0.0265(17) -0.0005(14) 0.0048(14) -0.0032(14)
C6 0.0242(16) 0.0206(15) 0.0234(15) 0.0037(12) 0.0119(13) 0.0049(13)
C7 0.0219(15) 0.0168(14) 0.0216(15) -0.0012(11) 0.0126(13) -0.0030(12)
C8 0.0248(16) 0.0233(15) 0.0255(16) 0.0033(13) 0.0157(14) -0.0008(13)
C9 0.0220(16) 0.0212(15) 0.0286(16) -0.0003(12) 0.0162(14) -0.0003(13)
C10 0.0229(16) 0.0197(14) 0.0134(13) -0.0032(11) 0.0063(12) -0.0029(12)
C11 0.0188(15) 0.0309(17) 0.0207(15) 0.0011(13) 0.0082(13) 0.0033(13)
C12 0.0254(17) 0.0286(16) 0.0278(17) -0.0054(14) 0.0105(14) -0.0102(15)
C13 0.0233(16) 0.0136(13) 0.0214(15) -0.0023(11) 0.0108(13) -0.0005(12)
C14 0.0302(17) 0.0163(14) 0.0307(17) 0.0024(13) 0.0158(14) -0.0008(13)
C15 0.0285(18) 0.0169(14) 0.0308(17) 0.0004(13) 0.0136(14) 0.0030(13)
C16 0.0201(15) 0.0192(14) 0.0185(14) -0.0018(11) 0.0100(12) -0.0011(12)
C17 0.0301(19) 0.0265(17) 0.0220(16) 0.0045(12) 0.0147(15) 0.0025(13)
C18 0.0258(17) 0.0285(16) 0.0189(15) -0.0041(13) 0.0111(13) -0.0045(14)
C19 0.0174(14) 0.0114(13) 0.0207(14) 0.0017(11) 0.0102(12) 0.0031(11)
C20 0.0225(16) 0.0171(14) 0.0203(15) 0.0016(11) 0.0077(13) 0.0049(12)
C21 0.0291(17) 0.0125(14) 0.0294(17) 0.0039(12) 0.0126(14) 0.0009(13)
C22 0.0202(15) 0.0138(13) 0.0207(15) -0.0033(11) 0.0065(12) -0.0001(12)
C23 0.0254(17) 0.0184(14) 0.0278(17) -0.0035(12) 0.0095(14) -0.0032(13)
C24 0.0245(16) 0.0187(14) 0.0203(15) -0.0040(12) 0.0066(13) 0.0029(13)
C25 0.0174(14) 0.0152(13) 0.0195(14) 0.0004(11) 0.0095(12) 0.0016(11)
C26 0.0270(17) 0.0185(14) 0.0251(16) 0.0005(12) 0.0164(14) 0.0058(13)
C27 0.0202(16) 0.0265(16) 0.0271(16) -0.0024(13) 0.0109(13) 0.0025(13)
C28 0.0199(15) 0.0132(13) 0.0203(14) 0.0036(11) 0.0086(12) 0.0027(12)
C29 0.0208(16) 0.0208(15) 0.0266(16) 0.0014(12) 0.0097(13) 0.0008(13)
C30 0.0237(16) 0.0194(15) 0.0298(17) 0.0040(13) 0.0148(14) 0.0048(13)
C31 0.0185(15) 0.0150(14) 0.0146(14) -0.0023(10) 0.0063(12) 0.0000(11)
C32 0.0199(15) 0.0166(14) 0.0212(15) -0.0023(12) 0.0083(13) -0.0015(12)
C33 0.0273(17) 0.0152(14) 0.0275(17) -0.0043(12) 0.0088(14) 0.0002(13)
C34 0.0204(15) 0.0134(13) 0.0174(14) -0.0004(11) 0.0106(12) -0.0012(12)
C35 0.0273(18) 0.0237(15) 0.0194(16) 0.0032(12) 0.0125(14) 0.0000(13)
C36 0.0213(16) 0.0196(14) 0.0258(16) -0.0014(12) 0.0143(13) -0.0016(12)
F1 0.0238(9) 0.0207(8) 0.0210(9) 0.0029(7) 0.0128(7) 0.0027(7)
F2 0.0232(9) 0.0191(8) 0.0366(10) -0.0022(7) 0.0183(8) 0.0028(7)
F3 0.0272(10) 0.0222(9) 0.0437(12) 0.0102(8) 0.0151(9) 0.0105(8)
F4 0.0315(10) 0.0297(10) 0.0254(10) 0.0144(8) 0.0106(8) 0.0072(8)
F5 0.0288(10) 0.0225(8) 0.0185(8) 0.0020(7) 0.0129(7) 0.0035(7)
F6 0.0273(10) 0.0136(8) 0.0307(10) -0.0040(7) 0.0148(8) -0.0057(7)
F7 0.0239(10) 0.0250(9) 0.0377(11) 0.0056(8) 0.0144(9) -0.0084(8)
F8 0.0238(10) 0.0370(11) 0.0357(11) 0.0102(8) 0.0198(9) 0.0059(8)
F9 0.0339(11) 0.0217(9) 0.0395(11) 0.0025(8) 0.0254(9) 0.0087(8)
F10 0.0254(9) 0.0122(7) 0.0280(9) 0.0005(7) 0.0156(8) -0.0008(7)
F11 0.0264(9) 0.0187(8) 0.0175(8) -0.0002(6) 0.0121(7) -0.0026(7)
F12 0.0313(10) 0.0214(8) 0.0334(10) 0.0048(7) 0.0205(9) -0.0048(8)
F13 0.0277(10) 0.0181(8) 0.0420(11) -0.0042(8) 0.0150(9) -0.0093(8)
F14 0.0308(10) 0.0309(10) 0.0246(10) -0.0114(8) 0.0080(8) -0.0092(8)
F15 0.0278(10) 0.0271(9) 0.0178(8) -0.0013(7) 0.0121(8) -0.0060(8)
F16 0.0234(9) 0.0099(8) 0.0232(9) -0.0005(6) 0.0063(8) 0.0029(6)
F17 0.0320(11) 0.0167(8) 0.0226(9) -0.0078(7) 0.0065(8) 0.0001(7)
F18 0.0307(10) 0.0305(10) 0.0176(9) -0.0030(7) 0.0008(8) 0.0070(8)
F19 0.0280(10) 0.0185(8) 0.0238(9) 0.0045(7) 0.0048(8) 0.0099(8)
F20 0.0247(9) 0.0119(7) 0.0220(9) -0.0007(6) 0.0076(7) 0.0026(7)
C37 0.0152(14) 0.0116(13) 0.0194(14) -0.0027(11) 0.0060(12) -0.0042(11)
C38 0.0180(15) 0.0132(13) 0.0184(14) 0.0006(11) 0.0074(12) -0.0050(11)
C39 0.0174(15) 0.0121(13) 0.0304(17) -0.0048(12) 0.0120(13) -0.0027(12)
C40 0.0149(14) 0.0123(13) 0.0320(17) 0.0037(12) 0.0071(13) 0.0005(11)
C41 0.0218(16) 0.0177(14) 0.0194(15) 0.0037(12) 0.0051(12) -0.0035(13)
C42 0.0182(15) 0.0154(14) 0.0214(15) -0.0039(11) 0.0087(12) -0.0050(12)
C43 0.0174(15) 0.0150(13) 0.0130(13) 0.0010(11) 0.0044(12) -0.0002(11)
C44 0.0204(15) 0.0142(13) 0.0183(14) 0.0022(11) 0.0066(12) 0.0012(12)
C45 0.0181(15) 0.0187(14) 0.0196(15) 0.0043(11) 0.0057(12) -0.0051(12)
C46 0.0149(15) 0.0296(17) 0.0201(16) 0.0070(12) 0.0078(13) 0.0036(12)
C47 0.0225(16) 0.0184(14) 0.0205(15) 0.0024(11) 0.0104(13) 0.0060(12)
C48 0.0171(14) 0.0153(13) 0.0155(14) 0.0011(11) 0.0054(11) -0.0015(11)
C49 0.0185(15) 0.0103(12) 0.0205(14) -0.0023(11) 0.0096(12) 0.0022(11)
C50 0.0221(15) 0.0131(13) 0.0178(14) -0.0009(11) 0.0104(12) 0.0023(12)
C51 0.0241(16) 0.0132(13) 0.0271(16) 0.0036(11) 0.0163(13) 0.0035(12)
C52 0.0202(15) 0.0112(13) 0.0340(17) -0.0028(12) 0.0132(14) -0.0012(12)
C53 0.0216(16) 0.0177(14) 0.0229(15) -0.0054(12) 0.0090(13) 0.0003(12)
C54 0.0227(15) 0.0163(13) 0.0201(15) 0.0006(11) 0.0127(13) 0.0028(12)
C55 0.0169(14) 0.0138(13) 0.0172(14) 0.0006(11) 0.0108(12) -0.0010(11)
C56 0.0229(16) 0.0125(13) 0.0234(15) 0.0021(11) 0.0148(13) 0.0028(12)
C57 0.0230(16) 0.0176(14) 0.0203(15) -0.0051(11) 0.0109(13) 0.0001(12)
C58 0.0192(15) 0.0230(15) 0.0166(14) -0.0014(12) 0.0059(12) 0.0016(13)
C59 0.0207(15) 0.0165(14) 0.0214(15) 0.0040(12) 0.0116(13) 0.0051(12)
C60 0.0218(15) 0.0086(12) 0.0210(15) -0.0025(11) 0.0131(12) -0.0015(11)
B1 0.0183(17) 0.0100(14) 0.0192(16) -0.0015(12) 0.0089(13) -0.0033(13)
_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
Si1 N1 1.737(2) . ?
Si1 C1 1.930(3) . ?
Si1 C4 1.899(3) . ?
Si1 C7 1.889(3) . ?
Si2 N1 1.739(2) . ?
Si2 C10 1.929(3) . ?
Si2 C13 1.893(3) . ?
Si2 C16 1.903(3) . ?
Si3 N2 1.749(2) . ?
Si3 C19 1.913(3) . ?
Si3 C22 1.895(3) . ?
Si3 C25 1.897(3) . ?
Si4 N2 1.744(2) . ?
Si4 C28 1.899(3) . ?
Si4 C31 1.907(3) . ?
Si4 C34 1.890(3) . ?
C1 C2 1.535(4) . ?
C1 C3 1.546(4) . ?
C4 C5 1.541(4) . ?
C4 C6 1.536(4) . ?
C7 C8 1.536(4) . ?
C7 C9 1.538(4) . ?
C10 C11 1.550(4) . ?
C10 C12 1.548(4) . ?
C13 C14 1.539(4) . ?
C13 C15 1.534(4) . ?
C16 C17 1.536(4) . ?
C16 C18 1.542(4) . ?
C19 C20 1.554(4) . ?
C19 C21 1.537(4) . ?
C22 C23 1.530(4) . ?
C22 C24 1.543(4) . ?
C25 C26 1.544(4) . ?
C25 C27 1.535(4) . ?
C28 C29 1.538(4) . ?
C28 C30 1.539(4) . ?
C31 C32 1.537(4) . ?
C31 C33 1.538(4) . ?
C34 C35 1.540(4) . ?
C34 C36 1.545(4) . ?
F1 C38 1.357(3) . ?
F2 C39 1.344(3) . ?
F3 C40 1.346(3) . ?
F4 C41 1.347(3) . ?
F5 C42 1.351(3) . ?
F6 C44 1.353(3) . ?
F7 C45 1.351(3) . ?
F8 C46 1.354(4) . ?
F9 C47 1.344(3) . ?
F10 C48 1.351(3) . ?
F11 C50 1.354(3) . ?
F12 C51 1.346(3) . ?
F13 C52 1.348(3) . ?
F14 C53 1.352(3) . ?
F15 C54 1.355(3) . ?
F16 C56 1.350(3) . ?
F17 C57 1.355(3) . ?
F18 C58 1.340(3) . ?
F19 C59 1.346(3) . ?
F20 C60 1.352(3) . ?
C37 C38 1.382(4) . ?
C37 C42 1.392(4) . ?
C37 B1 1.654(4) . ?
C38 C39 1.381(4) . ?
C39 C40 1.383(4) . ?
C40 C41 1.370(4) . ?
C41 C42 1.377(4) . ?
C43 C44 1.392(4) . ?
C43 C48 1.392(4) . ?
C43 B1 1.656(4) . ?
C44 C45 1.378(4) . ?
C45 C46 1.372(4) . ?
C46 C47 1.371(4) . ?
C47 C48 1.382(4) . ?
C49 C50 1.386(4) . ?
C49 C54 1.393(4) . ?
C49 B1 1.659(4) . ?
C50 C51 1.388(4) . ?
C51 C52 1.374(4) . ?
C52 C53 1.371(4) . ?
C53 C54 1.372(4) . ?
C55 C56 1.392(4) . ?
C55 C60 1.392(4) . ?
C55 B1 1.663(4) . ?
C56 C57 1.387(4) . ?
C57 C58 1.372(4) . ?
C58 C59 1.379(4) . ?
C59 C60 1.375(4) . ?
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
N1 Si1 C1 101.05(12) . . ?
N1 Si1 C4 111.49(12) . . ?
N1 Si1 C7 122.65(12) . . ?
C4 Si1 C1 105.58(13) . . ?
C7 Si1 C1 107.83(13) . . ?
C7 Si1 C4 106.87(14) . . ?
N1 Si2 C10 101.90(12) . . ?
N1 Si2 C13 116.07(13) . . ?
N1 Si2 C16 114.21(12) . . ?
C13 Si2 C10 106.41(13) . . ?
C13 Si2 C16 106.93(13) . . ?
C16 Si2 C10 111.00(13) . . ?
N2 Si3 C19 102.37(12) . . ?
N2 Si3 C22 113.72(13) . . ?
N2 Si3 C25 115.74(12) . . ?
C22 Si3 C19 107.46(13) . . ?
C22 Si3 C25 106.66(13) . . ?
C25 Si3 C19 110.60(13) . . ?
N2 Si4 C28 105.27(12) . . ?
N2 Si4 C31 103.70(12) . . ?
N2 Si4 C34 115.88(12) . . ?
C28 Si4 C31 104.90(13) . . ?
C34 Si4 C28 113.81(13) . . ?
C34 Si4 C31 112.18(13) . . ?
Si1 N1 Si2 137.49(14) . . ?
Si4 N2 Si3 131.40(14) . . ?
C2 C1 Si1 114.7(2) . . ?
C2 C1 C3 108.7(2) . . ?
C3 C1 Si1 113.5(2) . . ?
C5 C4 Si1 116.3(2) . . ?
C6 C4 Si1 114.6(2) . . ?
C6 C4 C5 107.8(3) . . ?
C8 C7 Si1 120.0(2) . . ?
C8 C7 C9 110.4(2) . . ?
C9 C7 Si1 112.5(2) . . ?
C11 C10 Si2 116.5(2) . . ?
C12 C10 Si2 115.6(2) . . ?
C12 C10 C11 107.7(3) . . ?
C14 C13 Si2 114.4(2) . . ?
C15 C13 Si2 113.7(2) . . ?
C15 C13 C14 109.7(3) . . ?
C17 C16 Si2 116.6(2) . . ?
C17 C16 C18 108.5(3) . . ?
C18 C16 Si2 113.4(2) . . ?
C20 C19 Si3 115.71(19) . . ?
C21 C19 Si3 115.0(2) . . ?
C21 C19 C20 108.3(2) . . ?
C23 C22 Si3 114.2(2) . . ?
C23 C22 C24 111.2(3) . . ?
C24 C22 Si3 111.5(2) . . ?
C26 C25 Si3 113.3(2) . . ?
C27 C25 Si3 114.8(2) . . ?
C27 C25 C26 109.2(2) . . ?
C29 C28 Si4 114.8(2) . . ?
C29 C28 C30 108.8(2) . . ?
C30 C28 Si4 119.2(2) . . ?
C32 C31 Si4 115.33(19) . . ?
C32 C31 C33 107.8(2) . . ?
C33 C31 Si4 115.4(2) . . ?
C35 C34 Si4 111.8(2) . . ?
C35 C34 C36 108.6(2) . . ?
C36 C34 Si4 115.7(2) . . ?
C38 C37 C42 113.3(3) . . ?
C38 C37 B1 120.5(2) . . ?
C42 C37 B1 126.0(3) . . ?
F1 C38 C37 119.7(3) . . ?
F1 C38 C39 115.5(3) . . ?
C39 C38 C37 124.8(3) . . ?
F2 C39 C38 121.2(3) . . ?
F2 C39 C40 119.8(3) . . ?
C38 C39 C40 119.1(3) . . ?
F3 C40 C39 120.1(3) . . ?
F3 C40 C41 121.2(3) . . ?
C41 C40 C39 118.7(3) . . ?
F4 C41 C40 119.6(3) . . ?
F4 C41 C42 120.3(3) . . ?
C40 C41 C42 120.1(3) . . ?
F5 C42 C37 121.2(3) . . ?
F5 C42 C41 114.8(3) . . ?
C41 C42 C37 124.0(3) . . ?
C44 C43 C48 113.1(3) . . ?
C44 C43 B1 119.3(2) . . ?
C48 C43 B1 127.2(3) . . ?
F6 C44 C43 119.6(3) . . ?
F6 C44 C45 115.6(2) . . ?
C45 C44 C43 124.8(3) . . ?
F7 C45 C44 120.7(3) . . ?
F7 C45 C46 120.2(3) . . ?
C46 C45 C44 119.1(3) . . ?
F8 C46 C45 120.2(3) . . ?
F8 C46 C47 120.5(3) . . ?
C47 C46 C45 119.2(3) . . ?
F9 C47 C46 119.5(3) . . ?
F9 C47 C48 120.7(3) . . ?
C46 C47 C48 119.8(3) . . ?
F10 C48 C43 120.8(3) . . ?
F10 C48 C47 115.3(2) . . ?
C47 C48 C43 123.9(3) . . ?
C50 C49 C54 113.3(3) . . ?
C50 C49 B1 126.7(3) . . ?
C54 C49 B1 119.7(2) . . ?
F11 C50 C49 121.0(3) . . ?
F11 C50 C51 115.0(2) . . ?
C49 C50 C51 124.0(3) . . ?
F12 C51 C50 120.3(3) . . ?
F12 C51 C52 120.1(3) . . ?
C52 C51 C50 119.6(3) . . ?
F13 C52 C51 120.5(3) . . ?
F13 C52 C53 120.7(3) . . ?
C53 C52 C51 118.7(3) . . ?
F14 C53 C52 119.1(3) . . ?
F14 C53 C54 121.0(3) . . ?
C52 C53 C54 119.9(3) . . ?
F15 C54 C49 119.5(3) . . ?
F15 C54 C53 116.2(3) . . ?
C53 C54 C49 124.3(3) . . ?
C56 C55 C60 112.9(3) . . ?
C56 C55 B1 127.3(2) . . ?
C60 C55 B1 119.4(2) . . ?
F16 C56 C55 121.3(3) . . ?
F16 C56 C57 115.2(2) . . ?
C57 C56 C55 123.6(3) . . ?
F17 C57 C56 120.2(3) . . ?
F17 C57 C58 119.3(3) . . ?
C58 C57 C56 120.5(3) . . ?
F18 C58 C57 120.6(3) . . ?
F18 C58 C59 120.9(3) . . ?
C57 C58 C59 118.5(3) . . ?
F19 C59 C58 119.7(3) . . ?
F19 C59 C60 121.1(3) . . ?
C60 C59 C58 119.2(3) . . ?
F20 C60 C55 119.1(3) . . ?
F20 C60 C59 115.6(2) . . ?
C59 C60 C55 125.3(3) . . ?
C37 B1 C43 113.0(2) . . ?
C37 B1 C49 102.8(2) . . ?
C37 B1 C55 114.5(2) . . ?
C43 B1 C49 114.2(2) . . ?
C43 B1 C55 100.1(2) . . ?
C49 B1 C55 112.8(2) . . ?
_shelx_res_file
;
TITL xdpm66 in P21/n #14
REM reset to P21/n #14
CELL 1.54184 19.928379 17.051337 21.104883 90 114.8184 90
ZERR 4 0.000349 0.000214 0.000394 0 0.0022 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H B N F Si Sm
UNIT 240 336 4 8 80 16 4
L.S. 9
PLAN 20
TEMP -173.1(2)
CONN 20 Sm1
FREE Sm1 Si3
FREE Sm1 Si4
FREE Sm1 Si1
FREE Sm1 Si2
BOND
fmap 2 53
acta
SHEL 100 0.83
REM
REM
REM
WGHT 0.058900 2.818700
FVAR 1.04974
SM1 7 0.578423 0.167704 0.831628 11.00000 0.01722 0.02056 =
0.01537 0.00013 0.00824 0.00438
SI1 6 0.417712 0.155257 0.835680 11.00000 0.01486 0.01173 =
0.01724 -0.00018 0.00874 0.00025
SI2 6 0.536094 0.279726 0.938810 11.00000 0.01704 0.01216 =
0.01573 -0.00036 0.00807 -0.00075
SI3 6 0.605631 0.082722 0.701734 11.00000 0.01595 0.01030 =
0.01677 -0.00082 0.00744 0.00066
SI4 6 0.564761 0.264290 0.688767 11.00000 0.01559 0.00988 =
0.01568 0.00060 0.00762 0.00100
N1 4 0.496081 0.214024 0.870073 11.00000 0.01730 0.01342 =
0.01628 0.00054 0.00866 0.00116
N2 4 0.578574 0.171073 0.726147 11.00000 0.01629 0.01187 =
0.01439 0.00039 0.00820 -0.00056
C1 1 0.458631 0.059135 0.818652 11.00000 0.02063 0.01338 =
0.02507 -0.00071 0.01297 0.00039
AFIX 13
H1 2 0.479543 0.072148 0.784357 11.00000 -1.20000
AFIX 0
C2 1 0.522427 0.024689 0.883005 11.00000 0.02530 0.01517 =
0.02826 0.00369 0.01602 0.00247
AFIX 137
H2A 2 0.560519 0.064826 0.904330 11.00000 -1.50000
H2B 2 0.543753 -0.020154 0.868886 11.00000 -1.50000
H2C 2 0.503736 0.007404 0.916883 11.00000 -1.50000
AFIX 0
C3 1 0.400244 -0.005676 0.784610 11.00000 0.02832 0.01431 =
0.04160 -0.00853 0.01854 -0.00461
AFIX 137
H3A 2 0.374494 -0.016647 0.814287 11.00000 -1.50000
H3B 2 0.424755 -0.053462 0.779348 11.00000 -1.50000
H3C 2 0.364467 0.011992 0.738615 11.00000 -1.50000
AFIX 0
C4 1 0.350188 0.191250 0.746432 11.00000 0.01578 0.01988 =
0.01571 -0.00074 0.00541 0.00011
AFIX 13
H4 2 0.373283 0.178202 0.713847 11.00000 -1.20000
AFIX 0
C5 1 0.273557 0.151772 0.715440 11.00000 0.01962 0.03085 =
0.02651 -0.00049 0.00482 -0.00315
AFIX 137
H5A 2 0.279616 0.094741 0.715372 11.00000 -1.50000
H5B 2 0.245465 0.170162 0.667485 11.00000 -1.50000
H5C 2 0.246854 0.165307 0.743752 11.00000 -1.50000
AFIX 0
C6 1 0.338287 0.280445 0.741078 11.00000 0.02418 0.02056 =
0.02335 0.00375 0.01186 0.00494
AFIX 137
H6A 2 0.308551 0.295733 0.766091 11.00000 -1.50000
H6B 2 0.312432 0.295486 0.691875 11.00000 -1.50000
H6C 2 0.386283 0.307020 0.761851 11.00000 -1.50000
AFIX 0
C7 1 0.361419 0.129801 0.885898 11.00000 0.02190 0.01683 =
0.02164 -0.00117 0.01256 -0.00304
AFIX 13
H7 2 0.320655 0.096063 0.852963 11.00000 -1.20000
AFIX 0
C8 1 0.395916 0.080372 0.952775 11.00000 0.02478 0.02329 =
0.02552 0.00334 0.01567 -0.00078
AFIX 137
H8A 2 0.413253 0.030364 0.942241 11.00000 -1.50000
H8B 2 0.358763 0.070395 0.970872 11.00000 -1.50000
H8C 2 0.437736 0.108829 0.987869 11.00000 -1.50000
AFIX 0
C9 1 0.321164 0.201366 0.897777 11.00000 0.02204 0.02115 =
0.02856 -0.00034 0.01621 -0.00028
AFIX 137
H9A 2 0.357107 0.235954 0.932671 11.00000 -1.50000
H9B 2 0.284594 0.183782 0.914460 11.00000 -1.50000
H9C 2 0.296135 0.229973 0.853771 11.00000 -1.50000
AFIX 0
C10 1 0.637091 0.282845 0.949555 11.00000 0.02290 0.01975 =
0.01344 -0.00315 0.00632 -0.00290
AFIX 13
H10 2 0.633779 0.289233 0.901228 11.00000 -1.20000
AFIX 0
C11 1 0.683668 0.207657 0.978486 11.00000 0.01882 0.03091 =
0.02072 0.00108 0.00816 0.00332
AFIX 137
H11A 2 0.705744 0.208928 1.029628 11.00000 -1.50000
H11B 2 0.722937 0.205060 0.962126 11.00000 -1.50000
H11C 2 0.651774 0.161442 0.961995 11.00000 -1.50000
AFIX 0
C12 1 0.683408 0.353487 0.991308 11.00000 0.02538 0.02862 =
0.02777 -0.00537 0.01047 -0.01022
AFIX 137
H12A 2 0.660273 0.402389 0.967924 11.00000 -1.50000
H12B 2 0.733544 0.349929 0.993814 11.00000 -1.50000
H12C 2 0.685726 0.352863 1.038616 11.00000 -1.50000
AFIX 0
C13 1 0.500639 0.384058 0.921250 11.00000 0.02333 0.01364 =
0.02143 -0.00234 0.01078 -0.00045
AFIX 13
H13 2 0.533195 0.415284 0.962965 11.00000 -1.20000
AFIX 0
C14 1 0.506790 0.422694 0.858017 11.00000 0.03022 0.01626 =
0.03069 0.00236 0.01579 -0.00082
AFIX 137
H14A 2 0.558778 0.424226 0.865605 11.00000 -1.50000
H14B 2 0.487261 0.476244 0.852315 11.00000 -1.50000
H14C 2 0.478250 0.392219 0.815856 11.00000 -1.50000
AFIX 0
C15 1 0.421771 0.393680 0.915519 11.00000 0.02852 0.01691 =
0.03077 0.00043 0.01357 0.00298
AFIX 137
H15A 2 0.387236 0.364975 0.874586 11.00000 -1.50000
H15B 2 0.408553 0.449416 0.910635 11.00000 -1.50000
H15C 2 0.419128 0.372799 0.957674 11.00000 -1.50000
AFIX 0
C16 1 0.531215 0.247739 1.023141 11.00000 0.02015 0.01925 =
0.01849 -0.00182 0.01000 -0.00112
AFIX 13
H16 2 0.477877 0.236560 1.010595 11.00000 -1.20000
AFIX 0
C17 1 0.573115 0.172447 1.057286 11.00000 0.03006 0.02655 =
0.02197 0.00454 0.01468 0.00245
AFIX 137
H17A 2 0.564355 0.132445 1.021328 11.00000 -1.50000
H17B 2 0.555557 0.153189 1.091408 11.00000 -1.50000
H17C 2 0.626166 0.183671 1.080907 11.00000 -1.50000
AFIX 0
C18 1 0.553524 0.312785 1.078975 11.00000 0.02583 0.02854 =
0.01895 -0.00406 0.01111 -0.00452
AFIX 137
H18A 2 0.605137 0.327678 1.092036 11.00000 -1.50000
H18B 2 0.548007 0.293435 1.120256 11.00000 -1.50000
H18C 2 0.521610 0.358592 1.060127 11.00000 -1.50000
AFIX 0
C19 1 0.631947 0.020132 0.783956 11.00000 0.01741 0.01136 =
0.02072 0.00170 0.01020 0.00308
AFIX 13
H19 2 0.586780 0.018429 0.793345 11.00000 -1.20000
AFIX 0
C20 1 0.694251 0.053832 0.851382 11.00000 0.02251 0.01715 =
0.02031 0.00163 0.00773 0.00487
AFIX 137
H20A 2 0.741337 0.028784 0.859175 11.00000 -1.50000
H20B 2 0.682551 0.043423 0.891297 11.00000 -1.50000
H20C 2 0.698168 0.110547 0.846206 11.00000 -1.50000
AFIX 0
C21 1 0.650446 -0.065845 0.776263 11.00000 0.02907 0.01253 =
0.02939 0.00389 0.01264 0.00089
AFIX 137
H21A 2 0.609489 -0.089519 0.736404 11.00000 -1.50000
H21B 2 0.658036 -0.094699 0.818900 11.00000 -1.50000
H21C 2 0.695610 -0.068144 0.768581 11.00000 -1.50000
AFIX 0
C22 1 0.528051 0.030267 0.627983 11.00000 0.02023 0.01380 =
0.02071 -0.00332 0.00652 -0.00012
AFIX 13
H22 2 0.549007 -0.020545 0.620887 11.00000 -1.20000
AFIX 0
C23 1 0.462025 0.009484 0.643891 11.00000 0.02541 0.01842 =
0.02779 -0.00346 0.00947 -0.00318
AFIX 137
H23A 2 0.477855 -0.027169 0.683259 11.00000 -1.50000
H23B 2 0.423338 -0.014979 0.602747 11.00000 -1.50000
H23C 2 0.442586 0.057287 0.655859 11.00000 -1.50000
AFIX 0
C24 1 0.503204 0.075964 0.558738 11.00000 0.02451 0.01875 =
0.02028 -0.00399 0.00657 0.00289
AFIX 137
H24A 2 0.485921 0.128195 0.564377 11.00000 -1.50000
H24B 2 0.462935 0.047561 0.521836 11.00000 -1.50000
H24C 2 0.544973 0.081160 0.546016 11.00000 -1.50000
AFIX 0
C25 1 0.685767 0.089409 0.675793 11.00000 0.01739 0.01517 =
0.01946 0.00035 0.00954 0.00158
AFIX 13
H25 2 0.673300 0.132665 0.640693 11.00000 -1.20000
AFIX 0
C26 1 0.695677 0.014821 0.639139 11.00000 0.02699 0.01848 =
0.02513 0.00047 0.01638 0.00584
AFIX 137
H26A 2 0.708243 -0.029501 0.671649 11.00000 -1.50000
H26B 2 0.735532 0.023138 0.624206 11.00000 -1.50000
H26C 2 0.649546 0.003476 0.598293 11.00000 -1.50000
AFIX 0
C27 1 0.760186 0.111443 0.735399 11.00000 0.02018 0.02653 =
0.02713 -0.00244 0.01090 0.00251
AFIX 137
H27A 2 0.753236 0.155984 0.761379 11.00000 -1.50000
H27B 2 0.795360 0.125854 0.715995 11.00000 -1.50000
H27C 2 0.779468 0.066556 0.766872 11.00000 -1.50000
AFIX 0
C28 1 0.463705 0.287668 0.664069 11.00000 0.01987 0.01322 =
0.02033 0.00358 0.00865 0.00268
AFIX 13
H28 2 0.455906 0.272214 0.706195 11.00000 -1.20000
AFIX 0
C29 1 0.408536 0.236513 0.605217 11.00000 0.02077 0.02079 =
0.02657 0.00140 0.00969 0.00083
AFIX 137
H29A 2 0.411780 0.248920 0.561248 11.00000 -1.50000
H29B 2 0.358267 0.246997 0.600404 11.00000 -1.50000
H29C 2 0.420411 0.181032 0.616502 11.00000 -1.50000
AFIX 0
C30 1 0.437662 0.373500 0.651006 11.00000 0.02365 0.01943 =
0.02984 0.00395 0.01482 0.00481
AFIX 137
H30A 2 0.465568 0.404675 0.692884 11.00000 -1.50000
H30B 2 0.384836 0.376097 0.640167 11.00000 -1.50000
H30C 2 0.445995 0.394397 0.611646 11.00000 -1.50000
AFIX 0
C31 1 0.618283 0.331518 0.765752 11.00000 0.01852 0.01500 =
0.01465 -0.00234 0.00628 -0.00001
AFIX 13
H31 2 0.589878 0.331885 0.795143 11.00000 -1.20000
AFIX 0
C32 1 0.696580 0.303659 0.814004 11.00000 0.01992 0.01660 =
0.02119 -0.00229 0.00825 -0.00145
AFIX 137
H32A 2 0.694409 0.249584 0.828764 11.00000 -1.50000
H32B 2 0.717063 0.337713 0.855154 11.00000 -1.50000
H32C 2 0.728180 0.305921 0.788854 11.00000 -1.50000
AFIX 0
C33 1 0.623642 0.417716 0.746985 11.00000 0.02735 0.01519 =
0.02745 -0.00433 0.00883 0.00024
AFIX 137
H33A 2 0.658781 0.422246 0.725757 11.00000 -1.50000
H33B 2 0.640677 0.449803 0.789387 11.00000 -1.50000
H33C 2 0.574884 0.436040 0.713847 11.00000 -1.50000
AFIX 0
C34 1 0.593595 0.277389 0.614790 11.00000 0.02041 0.01341 =
0.01743 -0.00039 0.01055 -0.00121
AFIX 13
H34 2 0.581422 0.227312 0.587620 11.00000 -1.20000
AFIX 0
C35 1 0.548993 0.342587 0.564160 11.00000 0.02728 0.02365 =
0.01942 0.00320 0.01248 -0.00004
AFIX 137
H35A 2 0.496154 0.330188 0.545471 11.00000 -1.50000
H35B 2 0.564144 0.346343 0.525686 11.00000 -1.50000
H35C 2 0.558289 0.392728 0.589094 11.00000 -1.50000
AFIX 0
C36 1 0.676730 0.292828 0.636605 11.00000 0.02126 0.01959 =
0.02584 -0.00144 0.01434 -0.00161
AFIX 137
H36A 2 0.689164 0.345837 0.655968 11.00000 -1.50000
H36B 2 0.687815 0.288022 0.595712 11.00000 -1.50000
H36C 2 0.705957 0.254420 0.671975 11.00000 -1.50000
AFIX 0
F1 5 0.635987 0.234775 0.258247 11.00000 0.02382 0.02070 =
0.02101 0.00293 0.01283 0.00275
F2 5 0.731294 0.116319 0.305664 11.00000 0.02319 0.01915 =
0.03660 -0.00222 0.01828 0.00282
F3 5 0.761311 0.050540 0.432412 11.00000 0.02723 0.02222 =
0.04365 0.01016 0.01512 0.01045
F4 5 0.692341 0.107642 0.510630 11.00000 0.03149 0.02973 =
0.02540 0.01441 0.01061 0.00717
F5 5 0.596303 0.222457 0.464602 11.00000 0.02876 0.02255 =
0.01854 0.00202 0.01287 0.00354
F6 5 0.468221 0.183188 0.349690 11.00000 0.02733 0.01355 =
0.03072 -0.00400 0.01482 -0.00566
F7 5 0.367808 0.190845 0.401312 11.00000 0.02390 0.02503 =
0.03772 0.00556 0.01441 -0.00838
F8 5 0.329071 0.332305 0.437120 11.00000 0.02378 0.03698 =
0.03567 0.01016 0.01982 0.00595
F9 5 0.398062 0.464608 0.423445 11.00000 0.03390 0.02172 =
0.03955 0.00250 0.02539 0.00865
F10 5 0.504136 0.458279 0.379322 11.00000 0.02544 0.01219 =
0.02800 0.00053 0.01556 -0.00076
F11 5 0.593250 0.398242 0.220090 11.00000 0.02638 0.01868 =
0.01750 -0.00020 0.01210 -0.00257
F12 5 0.691156 0.512643 0.250937 11.00000 0.03128 0.02137 =
0.03341 0.00479 0.02051 -0.00482
F13 5 0.765969 0.563380 0.385391 11.00000 0.02768 0.01810 =
0.04204 -0.00416 0.01500 -0.00928
F14 5 0.738371 0.495055 0.488341 11.00000 0.03077 0.03088 =
0.02457 -0.01138 0.00803 -0.00920
F15 5 0.640369 0.378926 0.459460 11.00000 0.02779 0.02707 =
0.01784 -0.00135 0.01209 -0.00597
F16 5 0.501727 0.160536 0.231462 11.00000 0.02342 0.00994 =
0.02323 -0.00049 0.00627 0.00285
F17 5 0.399093 0.156743 0.101712 11.00000 0.03199 0.01667 =
0.02255 -0.00785 0.00654 0.00011
F18 5 0.326226 0.289042 0.037610 11.00000 0.03072 0.03051 =
0.01759 -0.00297 0.00077 0.00698
F19 5 0.361165 0.428703 0.107657 11.00000 0.02798 0.01852 =
0.02378 0.00448 0.00485 0.00995
F20 5 0.464483 0.434575 0.237917 11.00000 0.02466 0.01194 =
0.02202 -0.00070 0.00755 0.00256
C37 1 0.608168 0.233876 0.356909 11.00000 0.01521 0.01155 =
0.01945 -0.00270 0.00604 -0.00416
C38 1 0.646560 0.203761 0.320979 11.00000 0.01802 0.01321 =
0.01838 0.00063 0.00740 -0.00505
C39 1 0.697112 0.143180 0.344342 11.00000 0.01742 0.01212 =
0.03039 -0.00482 0.01204 -0.00274
C40 1 0.712785 0.110109 0.408861 11.00000 0.01494 0.01230 =
0.03203 0.00366 0.00707 0.00054
C41 1 0.677875 0.139051 0.447670 11.00000 0.02176 0.01765 =
0.01940 0.00370 0.00506 -0.00349
C42 1 0.627544 0.199241 0.421959 11.00000 0.01822 0.01543 =
0.02135 -0.00385 0.00866 -0.00501
C43 1 0.493210 0.319735 0.362109 11.00000 0.01744 0.01496 =
0.01299 0.00096 0.00443 -0.00018
C44 1 0.454178 0.254926 0.368727 11.00000 0.02039 0.01420 =
0.01835 0.00224 0.00660 0.00119
C45 1 0.400397 0.257407 0.393645 11.00000 0.01807 0.01867 =
0.01957 0.00426 0.00574 -0.00512
C46 1 0.381145 0.328430 0.411768 11.00000 0.01495 0.02957 =
0.02014 0.00695 0.00780 0.00360
C47 1 0.416413 0.394988 0.405384 11.00000 0.02251 0.01841 =
0.02052 0.00243 0.01043 0.00604
C48 1 0.471455 0.389687 0.381962 11.00000 0.01709 0.01526 =
0.01552 0.00107 0.00543 -0.00153
C49 1 0.608700 0.383810 0.337839 11.00000 0.01847 0.01030 =
0.02054 -0.00231 0.00958 0.00218
C50 1 0.626507 0.419838 0.288017 11.00000 0.02206 0.01313 =
0.01778 -0.00089 0.01044 0.00225
C51 1 0.678117 0.479634 0.302601 11.00000 0.02410 0.01323 =
0.02707 0.00364 0.01627 0.00349
C52 1 0.715924 0.505066 0.370201 11.00000 0.02021 0.01116 =
0.03399 -0.00276 0.01322 -0.00123
C53 1 0.701586 0.470192 0.421760 11.00000 0.02160 0.01774 =
0.02294 -0.00544 0.00900 0.00035
C54 1 0.650167 0.411220 0.405310 11.00000 0.02267 0.01626 =
0.02010 0.00063 0.01274 0.00278
C55 1 0.491604 0.299094 0.242073 11.00000 0.01691 0.01381 =
0.01723 0.00064 0.01080 -0.00095
C56 1 0.470143 0.229827 0.203938 11.00000 0.02290 0.01250 =
0.02344 0.00208 0.01481 0.00280
C57 1 0.415691 0.226090 0.136189 11.00000 0.02302 0.01757 =
0.02026 -0.00512 0.01095 0.00012
C58 1 0.378820 0.292545 0.103079 11.00000 0.01922 0.02304 =
0.01655 -0.00139 0.00592 0.00158
C59 1 0.396746 0.362701 0.138848 11.00000 0.02068 0.01645 =
0.02138 0.00399 0.01155 0.00507
C60 1 0.450895 0.363843 0.205999 11.00000 0.02183 0.00861 =
0.02104 -0.00250 0.01313 -0.00149
B1 3 0.551293 0.308959 0.325134 11.00000 0.01826 0.00998 =
0.01917 -0.00151 0.00885 -0.00325
HKLF 4
REM xdpm66 in P21/n #14
REM R1 = 0.0361 for 10921 Fo > 4sig(Fo) and 0.0405 for all 11897 data
REM 817 parameters refined using 0 restraints
END
WGHT 0.0589 2.8189
REM Highest difference peak 0.641, deepest hole -1.339, 1-sigma level 0.086
Q1 1 0.5642 0.2179 0.8200 11.00000 0.05 0.64
Q2 1 0.5856 0.1647 0.8757 11.00000 0.05 0.63
Q3 1 0.5925 0.2136 0.8461 11.00000 0.05 0.62
Q4 1 0.5814 0.1009 0.8289 11.00000 0.05 0.59
Q5 1 0.4961 0.1672 0.8064 11.00000 0.05 0.57
Q6 1 0.6624 0.1685 0.8645 11.00000 0.05 0.54
Q7 1 0.5733 0.1649 0.7842 11.00000 0.05 0.50
Q8 1 0.6242 0.0826 0.9044 11.00000 0.05 0.50
Q9 1 0.5302 0.2655 0.9859 11.00000 0.05 0.48
Q10 1 0.5337 0.0838 0.7578 11.00000 0.05 0.44
Q11 1 0.5025 0.2112 0.7439 11.00000 0.05 0.40
Q12 1 0.6216 0.2546 0.9050 11.00000 0.05 0.39
Q13 1 0.5762 0.2673 0.3432 11.00000 0.05 0.39
Q14 1 0.6571 0.2060 0.9179 11.00000 0.05 0.39
Q15 1 0.3830 0.1440 0.8616 11.00000 0.05 0.39
Q16 1 0.5645 0.2619 0.6426 11.00000 0.05 0.39
Q17 1 0.5336 0.2455 0.7549 11.00000 0.05 0.37
Q18 1 0.5184 0.3395 0.9241 11.00000 0.05 0.36
Q19 1 0.6580 0.2360 0.8621 11.00000 0.05 0.36
Q20 1 0.3775 0.1810 0.7918 11.00000 0.05 0.35
;
_shelx_res_checksum 99587
_manchester_internal_archive_date ?
_manchester_internal_coll_client CAPG
_manchester_internal_coll_date 15/2/17
_manchester_internal_coll_frame_method '\w and \f scans'
_manchester_internal_coll_frame_time 10.0
_manchester_internal_coll_frame_width 1.0
_manchester_internal_coll_name xdpm66
_manchester_internal_coll_type custom
_manchester_internal_coll_user CAPG
_manchester_internal_process_date 16/2/17
_manchester_internal_process_user CAPG
_manchester_internal_refinement_date 16/2/17
_manchester_internal_refinement_user CAPG
_manchester_internal_solution_date 16/2/17
_manchester_internal_solution_user CAPG
_manchester_internal_validation_date ?
_manchester_internal_validation_user ?
_olex2_exptl_crystal_mounting_method 'From fombin on a microscope slide.'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 36.154
_oxdiff_exptl_absorpt_empirical_full_min 0.306
#######################################################################
#
# 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_rdpm43
_database_code_depnum_ccdc_archive 'CCDC 1880945'
loop_
_audit_author_name
_audit_author_address
'Hannah Nicholas'
;The University of Manchester
United Kingdom
;
_audit_update_record
;
2018-11-23 deposited with the CCDC. 2019-09-18 downloaded from the CCDC.
;
_manchester_internal_coll_name rdpm43
_manchester_internal_coll_client CAPG/HN/SWL
_manchester_internal_coll_type custom
_manchester_internal_coll_frame_time 4s
_manchester_internal_coll_frame_width 0.5
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user CAPG
_manchester_internal_coll_date 22/07/17
_manchester_internal_process_user CAPG
_manchester_internal_process_date 22/07/17
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 22/07/17
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 23/07/17
_manchester_internal_validation_user ?
_manchester_internal_validation_date ?
_manchester_internal_archive_date ?
_vrf_PLAT910_rdpm43
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...
RESPONSE: Reduction of beam stop mask did not yield significant
improvement. Most of those missing strong reflections
appeared to be very strong and were treated as overflows.
;
_audit_creation_date 2017-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H84 Cl N2 Si4 Tm'
_chemical_formula_sum 'C36 H84 Cl N2 Si4 Tm'
_chemical_formula_weight 861.79
_chemical_melting_point ?
_chemical_oxdiff_formula Tm(N(SiC9H21)2)2Cl
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'
Cl Cl 0.1484 0.1585 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 '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 15.8309(4)
_cell_length_b 13.1077(3)
_cell_length_c 22.5379(6)
_cell_angle_alpha 90
_cell_angle_beta 109.043(3)
_cell_angle_gamma 90
_cell_volume 4420.8(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 17724
_cell_measurement_temperature 100.00(2)
_cell_measurement_theta_max 29.8500
_cell_measurement_theta_min 3.5910
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.201
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.382
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
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 'clear green'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary green
_exptl_crystal_density_diffrn 1.295
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1824
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -9 -25 0.1250
8 -17 4 0.1798
6 -1 26 0.1103
14 -4 -30 0.0970
-14 -13 18 0.1247
2 17 8 0.1252
-15 0 30 0.1087
14 9 12 0.0959
3 14 17 0.0809
-21 2 0 0.1568
19 3 -24 0.1166
-3 14 21 0.0911
2 1 -30 0.1483
-2 -5 30 0.0979
-10 -1 32 0.0871
_exptl_crystal_size_max 0.435
_exptl_crystal_size_mid 0.301
_exptl_crystal_size_min 0.217
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
-2.0161 -8.9978 -25.0031 0.0964 -0.5046 -0.8522
7.9850 -16.9893 3.9714 -0.1358 0.7440 -0.6839
6.0068 -0.9962 25.9634 -0.1513 0.8881 0.4239
13.9889 -3.9951 -29.8360 -0.6477 -0.4265 -0.6638
-14.0092 -12.9978 17.5578 0.7919 0.5390 -0.3258
2.0194 16.9933 8.4536 -0.2415 -0.1765 0.9285
-14.9930 -0.0035 29.6713 0.7331 0.5078 0.4757
14.0134 9.0012 11.9137 -0.6460 0.3978 0.6574
3.0190 13.9955 17.3070 -0.2200 0.1752 0.9488
-20.9999 1.9921 -0.2093 0.8599 -0.5174 0.0290
18.9978 3.0037 -24.4252 -0.9160 -0.3539 -0.2362
-2.9805 13.9937 20.8941 0.0446 0.1453 0.9947
1.9927 0.9986 -30.4175 -0.2003 -0.8391 -0.4793
-1.9967 -4.9968 30.3122 0.2439 0.9439 0.2950
-9.9929 -1.0012 31.9139 0.5417 0.7068 0.4831
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0260
_diffrn_reflns_av_unetI/netI 0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 31900
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.346
_diffrn_reflns_theta_min 3.528
_diffrn_ambient_temperature 100.00(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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 -45.00 -19.00 0.50 4.00 -- 5.00 -43.00 -7.00 52
2 \w 36.00 62.00 0.50 4.00 -- -7.50 43.00 143.00 52
3 \w 48.00 81.00 0.50 4.00 -- -7.50 57.00-150.00 66
4 \w -34.00 81.00 0.50 4.00 -- -7.50 57.00 60.00 230
5 \w -39.00 36.00 0.50 4.00 -- -7.50 57.00-150.00 150
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0420198000
_diffrn_orient_matrix_UB_12 -0.0109465000
_diffrn_orient_matrix_UB_13 0.0034730000
_diffrn_orient_matrix_UB_21 0.0217998000
_diffrn_orient_matrix_UB_22 -0.0269694000
_diffrn_orient_matrix_UB_23 0.0281282000
_diffrn_orient_matrix_UB_31 0.0027733000
_diffrn_orient_matrix_UB_32 0.0456349000
_diffrn_orient_matrix_UB_33 0.0174376000
_diffrn_oxdiff_ac3_digest_frames
;
01b77e4d215d63a35a73e869239285d3ca005508110
;
_diffrn_oxdiff_ac3_digest_hkl
;
0126995b4cf046dd8f7519cd58329d36bb86a8
;
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7461
_reflns_number_total 8039
_reflns_odcompleteness_completeness 98.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_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 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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 'XS (Sheldrick, 2008)'
_refine_diff_density_max 0.586
_refine_diff_density_min -0.601
_refine_diff_density_rms 0.064
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.029
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 421
_refine_ls_number_reflns 8039
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0210
_refine_ls_R_factor_gt 0.0185
_refine_ls_restrained_S_all 1.029
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+2.0752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0468
_refine_ls_wR_factor_ref 0.0476
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16), C19(H19), C22(H22),
C25(H25), C28(H28), C31(H31), C34(H34)
2.b Idealised Me refined as rotating group:
C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,
H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C),
C36(H36A,H36B,H36C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm1 Tm 0.67448(2) 0.46423(2) 0.77431(2) 0.01124(4) Uani 1 1 d . . . . .
Cl1 Cl 0.50892(3) 0.47653(4) 0.73840(2) 0.01684(10) Uani 1 1 d . . . . .
Si1 Si 0.77200(3) 0.28894(4) 0.87087(2) 0.01171(11) Uani 1 1 d . . . . .
Si2 Si 0.70975(3) 0.47220(4) 0.93635(3) 0.01133(11) Uani 1 1 d . . . . .
Si3 Si 0.72966(3) 0.52757(4) 0.64824(3) 0.01190(11) Uani 1 1 d . . . . .
Si4 Si 0.77189(3) 0.68549(4) 0.76070(2) 0.01250(11) Uani 1 1 d . . . . .
N1 N 0.72542(10) 0.40813(11) 0.87251(7) 0.0112(3) Uani 1 1 d . . . . .
N2 N 0.73965(10) 0.56816(12) 0.72343(7) 0.0120(3) Uani 1 1 d . . . . .
C1 C 0.74563(12) 0.26103(14) 0.78241(9) 0.0145(4) Uani 1 1 d . . . . .
H1 H 0.758814 0.325032 0.762918 0.017 Uiso 1 1 calc R . . . .
C2 C 0.64618(13) 0.23619(15) 0.74894(9) 0.0180(4) Uani 1 1 d . . . . .
H2A H 0.630924 0.172217 0.765538 0.027 Uiso 1 1 calc GR . . . .
H2B H 0.635315 0.229056 0.703770 0.027 Uiso 1 1 calc GR . . . .
H2C H 0.609107 0.291512 0.756241 0.027 Uiso 1 1 calc GR . . . .
C3 C 0.80250(14) 0.17599(15) 0.76718(10) 0.0208(4) Uani 1 1 d . . . . .
H3A H 0.865938 0.193768 0.784854 0.031 Uiso 1 1 calc GR . . . .
H3B H 0.786260 0.168556 0.721559 0.031 Uiso 1 1 calc GR . . . .
H3C H 0.791496 0.111537 0.785450 0.031 Uiso 1 1 calc GR . . . .
C4 C 0.89812(12) 0.29561(15) 0.90937(9) 0.0160(4) Uani 1 1 d . . . . .
H4 H 0.907346 0.338413 0.947703 0.019 Uiso 1 1 calc R . . . .
C5 C 0.94956(13) 0.19643(16) 0.93367(11) 0.0244(5) Uani 1 1 d . . . . .
H5A H 0.924233 0.162915 0.962914 0.037 Uiso 1 1 calc GR . . . .
H5B H 1.012621 0.212290 0.955365 0.037 Uiso 1 1 calc GR . . . .
H5C H 0.944621 0.150833 0.898238 0.037 Uiso 1 1 calc GR . . . .
C6 C 0.94303(13) 0.35573(16) 0.86921(10) 0.0190(4) Uani 1 1 d . . . . .
H6A H 0.948775 0.311896 0.835508 0.029 Uiso 1 1 calc GR . . . .
H6B H 1.002445 0.378227 0.895598 0.029 Uiso 1 1 calc GR . . . .
H6C H 0.906473 0.415384 0.850924 0.029 Uiso 1 1 calc GR . . . .
C7 C 0.72511(12) 0.18091(14) 0.90761(9) 0.0155(4) Uani 1 1 d . . . . .
H7 H 0.754759 0.187498 0.953983 0.019 Uiso 1 1 calc R . . . .
C8 C 0.74701(14) 0.07205(15) 0.89053(10) 0.0216(4) Uani 1 1 d . . . . .
H8A H 0.712282 0.057466 0.846695 0.032 Uiso 1 1 calc GR . . . .
H8B H 0.731704 0.022468 0.917939 0.032 Uiso 1 1 calc GR . . . .
H8C H 0.810926 0.067232 0.896130 0.032 Uiso 1 1 calc GR . . . .
C9 C 0.62387(13) 0.18530(15) 0.89667(10) 0.0192(4) Uani 1 1 d . . . . .
H9A H 0.607515 0.254185 0.905885 0.029 Uiso 1 1 calc GR . . . .
H9B H 0.608593 0.136189 0.924351 0.029 Uiso 1 1 calc GR . . . .
H9C H 0.591109 0.168325 0.852833 0.029 Uiso 1 1 calc GR . . . .
C10 C 0.59197(13) 0.52850(14) 0.90354(10) 0.0157(4) Uani 1 1 d . . . . .
H10 H 0.587112 0.551841 0.860314 0.019 Uiso 1 1 calc R . . . .
C11 C 0.51817(13) 0.44682(16) 0.89310(10) 0.0195(4) Uani 1 1 d . . . . .
H11A H 0.529135 0.391340 0.867388 0.029 Uiso 1 1 calc GR . . . .
H11B H 0.459805 0.477676 0.871538 0.029 Uiso 1 1 calc GR . . . .
H11C H 0.518759 0.419643 0.933737 0.029 Uiso 1 1 calc GR . . . .
C12 C 0.56734(13) 0.62247(16) 0.93461(10) 0.0224(5) Uani 1 1 d . . . . .
H12A H 0.568530 0.604987 0.977153 0.034 Uiso 1 1 calc GR . . . .
H12B H 0.507265 0.645520 0.909901 0.034 Uiso 1 1 calc GR . . . .
H12C H 0.610452 0.677128 0.936693 0.034 Uiso 1 1 calc GR . . . .
C13 C 0.79365(12) 0.58137(14) 0.96072(9) 0.0140(4) Uani 1 1 d . . . . .
H13 H 0.776918 0.629863 0.924483 0.017 Uiso 1 1 calc R . . . .
C14 C 0.89116(12) 0.55081(15) 0.97045(9) 0.0154(4) Uani 1 1 d . . . . .
H14A H 0.913430 0.508001 1.007988 0.023 Uiso 1 1 calc GR . . . .
H14B H 0.928073 0.612331 0.975768 0.023 Uiso 1 1 calc GR . . . .
H14C H 0.894055 0.512635 0.933769 0.023 Uiso 1 1 calc GR . . . .
C15 C 0.79252(13) 0.64466(16) 1.01770(10) 0.0201(4) Uani 1 1 d . . . . .
H15A H 0.730717 0.662200 1.013678 0.030 Uiso 1 1 calc GR . . . .
H15B H 0.827097 0.707342 1.019721 0.030 Uiso 1 1 calc GR . . . .
H15C H 0.819026 0.604889 1.056118 0.030 Uiso 1 1 calc GR . . . .
C16 C 0.71824(12) 0.38982(15) 1.00803(9) 0.0164(4) Uani 1 1 d . . . . .
H16 H 0.684930 0.325220 0.992158 0.020 Uiso 1 1 calc R . . . .
C17 C 0.81395(13) 0.35939(16) 1.04769(10) 0.0205(4) Uani 1 1 d . . . . .
H17A H 0.843559 0.326498 1.020742 0.031 Uiso 1 1 calc GR . . . .
H17B H 0.811728 0.311824 1.080696 0.031 Uiso 1 1 calc GR . . . .
H17C H 0.847480 0.420491 1.066882 0.031 Uiso 1 1 calc GR . . . .
C18 C 0.67304(14) 0.44053(16) 1.05192(10) 0.0209(4) Uani 1 1 d . . . . .
H18A H 0.700896 0.506926 1.065893 0.031 Uiso 1 1 calc GR . . . .
H18B H 0.680340 0.396691 1.088484 0.031 Uiso 1 1 calc GR . . . .
H18C H 0.609246 0.450095 1.029191 0.031 Uiso 1 1 calc GR . . . .
C19 C 0.63964(13) 0.42198(15) 0.62802(9) 0.0154(4) Uani 1 1 d . . . . .
H19 H 0.642366 0.390070 0.668909 0.019 Uiso 1 1 calc R . . . .
C20 C 0.65318(15) 0.33440(16) 0.58649(10) 0.0240(5) Uani 1 1 d . . . . .
H20A H 0.654652 0.362107 0.546450 0.036 Uiso 1 1 calc GR . . . .
H20B H 0.603768 0.285713 0.578679 0.036 Uiso 1 1 calc GR . . . .
H20C H 0.709752 0.299641 0.607900 0.036 Uiso 1 1 calc GR . . . .
C21 C 0.54383(13) 0.46210(15) 0.59898(10) 0.0198(4) Uani 1 1 d . . . . .
H21A H 0.534621 0.520160 0.623578 0.030 Uiso 1 1 calc GR . . . .
H21B H 0.501343 0.407799 0.599118 0.030 Uiso 1 1 calc GR . . . .
H21C H 0.534365 0.483962 0.555705 0.030 Uiso 1 1 calc GR . . . .
C22 C 0.83386(14) 0.46491(15) 0.63917(10) 0.0188(4) Uani 1 1 d . . . . .
H22 H 0.813002 0.429754 0.597522 0.023 Uiso 1 1 calc R . . . .
C23 C 0.87337(13) 0.38081(16) 0.68720(10) 0.0229(5) Uani 1 1 d . . . . .
H23A H 0.895575 0.410623 0.729341 0.034 Uiso 1 1 calc GR . . . .
H23B H 0.922780 0.347666 0.677481 0.034 Uiso 1 1 calc GR . . . .
H23C H 0.827084 0.330226 0.685580 0.034 Uiso 1 1 calc GR . . . .
C24 C 0.90847(14) 0.53704(16) 0.63614(12) 0.0257(5) Uani 1 1 d . . . . .
H24A H 0.883118 0.591044 0.605419 0.039 Uiso 1 1 calc GR . . . .
H24B H 0.952946 0.498643 0.623529 0.039 Uiso 1 1 calc GR . . . .
H24C H 0.937088 0.567571 0.677549 0.039 Uiso 1 1 calc GR . . . .
C25 C 0.69692(13) 0.62983(14) 0.58480(9) 0.0154(4) Uani 1 1 d . . . . .
H25 H 0.746762 0.680641 0.596639 0.019 Uiso 1 1 calc R . . . .
C26 C 0.69371(14) 0.58770(16) 0.52021(9) 0.0209(4) Uani 1 1 d . . . . .
H26A H 0.751519 0.557042 0.523491 0.031 Uiso 1 1 calc GR . . . .
H26B H 0.680821 0.643432 0.489570 0.031 Uiso 1 1 calc GR . . . .
H26C H 0.646741 0.535833 0.506535 0.031 Uiso 1 1 calc GR . . . .
C27 C 0.61085(13) 0.69170(15) 0.57694(10) 0.0197(4) Uani 1 1 d . . . . .
H27A H 0.558994 0.653349 0.550639 0.030 Uiso 1 1 calc GR . . . .
H27B H 0.614314 0.757263 0.556963 0.030 Uiso 1 1 calc GR . . . .
H27C H 0.604649 0.703723 0.618240 0.030 Uiso 1 1 calc GR . . . .
C28 C 0.67876(12) 0.71044(14) 0.79596(9) 0.0154(4) Uani 1 1 d . . . . .
H28 H 0.671892 0.644750 0.816481 0.018 Uiso 1 1 calc R . . . .
C29 C 0.58889(13) 0.72686(16) 0.74418(10) 0.0204(4) Uani 1 1 d . . . . .
H29A H 0.588340 0.794165 0.725128 0.031 Uiso 1 1 calc GR . . . .
H29B H 0.540482 0.722948 0.762291 0.031 Uiso 1 1 calc GR . . . .
H29C H 0.580367 0.673968 0.712026 0.031 Uiso 1 1 calc GR . . . .
C30 C 0.68980(14) 0.79204(15) 0.84668(10) 0.0213(4) Uani 1 1 d . . . . .
H30A H 0.741184 0.774945 0.883514 0.032 Uiso 1 1 calc GR . . . .
H30B H 0.635657 0.794707 0.858677 0.032 Uiso 1 1 calc GR . . . .
H30C H 0.699632 0.858625 0.830262 0.032 Uiso 1 1 calc GR . . . .
C31 C 0.88097(13) 0.66866(16) 0.82758(9) 0.0189(4) Uani 1 1 d . . . . .
H31 H 0.866722 0.620068 0.857188 0.023 Uiso 1 1 calc R . . . .
C32 C 0.95563(13) 0.61663(17) 0.80914(10) 0.0238(5) Uani 1 1 d . . . . .
H32A H 0.931479 0.556698 0.783147 0.036 Uiso 1 1 calc GR . . . .
H32B H 1.003425 0.595331 0.847123 0.036 Uiso 1 1 calc GR . . . .
H32C H 0.979676 0.664629 0.785387 0.036 Uiso 1 1 calc GR . . . .
C33 C 0.91914(14) 0.76376(18) 0.86731(10) 0.0274(5) Uani 1 1 d . . . . .
H33A H 0.934432 0.815260 0.840968 0.041 Uiso 1 1 calc GR . . . .
H33B H 0.972906 0.744945 0.901910 0.041 Uiso 1 1 calc GR . . . .
H33C H 0.874387 0.791653 0.884338 0.041 Uiso 1 1 calc GR . . . .
C34 C 0.77942(13) 0.79773(14) 0.70869(9) 0.0183(4) Uani 1 1 d . . . . .
H34 H 0.731039 0.787859 0.667540 0.022 Uiso 1 1 calc R . . . .
C35 C 0.86810(14) 0.80161(17) 0.69461(10) 0.0251(5) Uani 1 1 d . . . . .
H35A H 0.917143 0.816182 0.733396 0.038 Uiso 1 1 calc GR . . . .
H35B H 0.865075 0.855403 0.663788 0.038 Uiso 1 1 calc GR . . . .
H35C H 0.878598 0.735724 0.677686 0.038 Uiso 1 1 calc GR . . . .
C36 C 0.76341(16) 0.90250(15) 0.73366(11) 0.0270(5) Uani 1 1 d . . . . .
H36A H 0.702448 0.905492 0.735470 0.040 Uiso 1 1 calc GR . . . .
H36B H 0.771341 0.956090 0.705613 0.040 Uiso 1 1 calc GR . . . .
H36C H 0.806244 0.912772 0.775822 0.040 Uiso 1 1 calc GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Tm1 0.00877(5) 0.01288(5) 0.01144(6) 0.00041(3) 0.00242(4) -0.00145(3)
Cl1 0.0107(2) 0.0215(2) 0.0174(2) 0.00029(18) 0.00330(19) -0.00106(17)
Si1 0.0100(2) 0.0114(2) 0.0131(3) -0.00013(19) 0.0030(2) 0.00018(19)
Si2 0.0087(2) 0.0131(3) 0.0118(3) -0.00162(19) 0.0029(2) -0.00035(19)
Si3 0.0111(2) 0.0123(3) 0.0125(3) -0.00005(19) 0.0041(2) 0.00033(19)
Si4 0.0113(2) 0.0122(2) 0.0133(3) -0.0011(2) 0.0031(2) -0.0024(2)
N1 0.0091(7) 0.0118(8) 0.0126(8) -0.0024(6) 0.0032(6) -0.0008(6)
N2 0.0097(7) 0.0137(8) 0.0118(8) -0.0011(6) 0.0022(6) -0.0007(6)
C1 0.0176(9) 0.0107(9) 0.0164(10) -0.0011(7) 0.0071(8) -0.0002(7)
C2 0.0191(10) 0.0155(10) 0.0169(10) -0.0008(8) 0.0024(8) -0.0022(8)
C3 0.0267(11) 0.0168(10) 0.0207(11) -0.0034(8) 0.0103(9) 0.0028(9)
C4 0.0131(9) 0.0162(10) 0.0183(10) -0.0020(8) 0.0045(8) 0.0013(8)
C5 0.0158(10) 0.0245(11) 0.0289(12) 0.0012(9) 0.0018(9) 0.0059(9)
C6 0.0126(9) 0.0250(11) 0.0206(11) -0.0045(9) 0.0070(8) -0.0024(8)
C7 0.0166(9) 0.0138(9) 0.0148(10) 0.0005(8) 0.0033(8) -0.0020(8)
C8 0.0273(11) 0.0146(10) 0.0225(11) 0.0031(8) 0.0074(9) 0.0004(9)
C9 0.0186(10) 0.0196(10) 0.0198(11) -0.0006(8) 0.0068(8) -0.0062(8)
C10 0.0112(9) 0.0175(10) 0.0189(11) -0.0022(8) 0.0056(8) -0.0001(7)
C11 0.0104(9) 0.0243(11) 0.0233(11) -0.0037(9) 0.0047(9) -0.0024(8)
C12 0.0155(10) 0.0232(11) 0.0283(12) -0.0054(9) 0.0067(9) 0.0021(8)
C13 0.0114(9) 0.0155(10) 0.0144(10) -0.0020(8) 0.0032(8) -0.0004(7)
C14 0.0122(9) 0.0176(10) 0.0157(10) 0.0001(8) 0.0034(8) -0.0015(8)
C15 0.0149(9) 0.0212(10) 0.0237(11) -0.0081(9) 0.0058(8) -0.0040(8)
C16 0.0161(9) 0.0189(10) 0.0143(10) -0.0014(8) 0.0051(8) -0.0021(8)
C17 0.0181(10) 0.0260(11) 0.0162(10) 0.0056(8) 0.0038(8) 0.0008(8)
C18 0.0240(11) 0.0239(10) 0.0176(11) -0.0008(9) 0.0106(9) -0.0024(9)
C19 0.0173(9) 0.0162(10) 0.0125(10) 0.0001(8) 0.0045(8) -0.0015(8)
C20 0.0283(11) 0.0185(11) 0.0270(12) -0.0081(9) 0.0114(10) -0.0054(9)
C21 0.0145(10) 0.0263(12) 0.0164(11) -0.0002(8) 0.0021(8) -0.0042(8)
C22 0.0166(10) 0.0244(11) 0.0182(11) 0.0003(8) 0.0097(9) 0.0032(8)
C23 0.0190(10) 0.0260(11) 0.0266(12) 0.0040(9) 0.0114(9) 0.0078(9)
C24 0.0187(11) 0.0326(13) 0.0299(13) 0.0028(9) 0.0135(10) 0.0011(9)
C25 0.0171(9) 0.0142(9) 0.0144(10) 0.0010(8) 0.0044(8) -0.0024(8)
C26 0.0255(10) 0.0219(11) 0.0144(10) 0.0010(8) 0.0051(9) -0.0003(9)
C27 0.0197(10) 0.0188(10) 0.0189(11) 0.0036(8) 0.0039(8) 0.0002(8)
C28 0.0172(9) 0.0119(9) 0.0183(10) 0.0001(8) 0.0074(8) -0.0002(7)
C29 0.0160(10) 0.0201(10) 0.0246(11) -0.0006(9) 0.0060(9) 0.0045(8)
C30 0.0289(11) 0.0154(10) 0.0217(11) -0.0019(8) 0.0112(9) 0.0012(8)
C31 0.0149(9) 0.0229(11) 0.0169(10) 0.0017(8) 0.0025(8) -0.0059(8)
C32 0.0139(9) 0.0308(12) 0.0230(11) 0.0033(9) 0.0008(9) -0.0019(9)
C33 0.0214(11) 0.0384(13) 0.0204(11) -0.0073(10) 0.0040(9) -0.0119(10)
C34 0.0229(10) 0.0141(10) 0.0162(10) 0.0003(8) 0.0039(8) -0.0054(8)
C35 0.0271(11) 0.0280(12) 0.0201(11) 0.0025(9) 0.0076(9) -0.0113(9)
C36 0.0417(13) 0.0136(10) 0.0257(12) 0.0018(9) 0.0110(10) -0.0041(9)
_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
Tm1 Cl1 2.4832(5) . ?
Tm1 N1 2.2191(15) . ?
Tm1 N2 2.2377(15) . ?
Tm1 C1 2.8744(18) . ?
Si1 N1 1.7330(15) . ?
Si1 C1 1.934(2) . ?
Si1 C4 1.9018(19) . ?
Si1 C7 1.9087(19) . ?
Si2 N1 1.7522(16) . ?
Si2 C10 1.915(2) . ?
Si2 C13 1.9073(19) . ?
Si2 C16 1.911(2) . ?
Si3 N2 1.7336(16) . ?
Si3 C19 1.931(2) . ?
Si3 C22 1.913(2) . ?
Si3 C25 1.904(2) . ?
Si4 N2 1.7468(16) . ?
Si4 C28 1.9176(19) . ?
Si4 C31 1.899(2) . ?
Si4 C34 1.909(2) . ?
C1 C2 1.542(3) . ?
C1 C3 1.540(3) . ?
C4 C5 1.537(3) . ?
C4 C6 1.538(3) . ?
C7 C8 1.546(3) . ?
C7 C9 1.541(3) . ?
C10 C11 1.545(3) . ?
C10 C12 1.529(3) . ?
C13 C14 1.540(2) . ?
C13 C15 1.534(3) . ?
C16 C17 1.539(3) . ?
C16 C18 1.547(3) . ?
C19 C20 1.540(3) . ?
C19 C21 1.536(3) . ?
C22 C23 1.529(3) . ?
C22 C24 1.532(3) . ?
C25 C26 1.542(3) . ?
C25 C27 1.545(3) . ?
C28 C29 1.533(3) . ?
C28 C30 1.533(3) . ?
C31 C32 1.535(3) . ?
C31 C33 1.539(3) . ?
C34 C35 1.538(3) . ?
C34 C36 1.536(3) . ?
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
Cl1 Tm1 C1 115.53(4) . . ?
N1 Tm1 Cl1 110.37(4) . . ?
N1 Tm1 N2 129.39(5) . . ?
N1 Tm1 C1 67.81(5) . . ?
N2 Tm1 Cl1 114.05(4) . . ?
N2 Tm1 C1 111.10(5) . . ?
N1 Si1 C1 104.02(8) . . ?
N1 Si1 C4 109.84(8) . . ?
N1 Si1 C7 115.54(8) . . ?
C4 Si1 C1 108.69(8) . . ?
C4 Si1 C7 109.58(9) . . ?
C7 Si1 C1 108.86(8) . . ?
N1 Si2 C10 104.39(8) . . ?
N1 Si2 C13 108.92(8) . . ?
N1 Si2 C16 115.70(8) . . ?
C13 Si2 C10 108.71(8) . . ?
C13 Si2 C16 109.28(9) . . ?
C16 Si2 C10 109.58(9) . . ?
N2 Si3 C19 105.99(8) . . ?
N2 Si3 C22 115.44(9) . . ?
N2 Si3 C25 115.70(8) . . ?
C22 Si3 C19 105.23(9) . . ?
C25 Si3 C19 109.16(9) . . ?
C25 Si3 C22 104.78(9) . . ?
N2 Si4 C28 101.88(8) . . ?
N2 Si4 C31 109.07(8) . . ?
N2 Si4 C34 116.76(8) . . ?
C31 Si4 C28 108.30(9) . . ?
C31 Si4 C34 110.75(9) . . ?
C34 Si4 C28 109.48(9) . . ?
Si1 N1 Tm1 107.23(7) . . ?
Si1 N1 Si2 128.67(9) . . ?
Si2 N1 Tm1 123.87(8) . . ?
Si3 N2 Tm1 113.82(8) . . ?
Si3 N2 Si4 131.25(10) . . ?
Si4 N2 Tm1 113.63(8) . . ?
Si1 C1 Tm1 80.70(6) . . ?
C2 C1 Tm1 81.27(10) . . ?
C2 C1 Si1 112.75(13) . . ?
C3 C1 Tm1 154.41(13) . . ?
C3 C1 Si1 114.92(13) . . ?
C3 C1 C2 108.41(16) . . ?
C5 C4 Si1 118.62(14) . . ?
C5 C4 C6 110.50(16) . . ?
C6 C4 Si1 111.90(13) . . ?
C8 C7 Si1 115.21(13) . . ?
C9 C7 Si1 115.74(13) . . ?
C9 C7 C8 107.49(16) . . ?
C11 C10 Si2 112.60(13) . . ?
C12 C10 Si2 119.68(14) . . ?
C12 C10 C11 109.57(16) . . ?
C14 C13 Si2 114.67(13) . . ?
C15 C13 Si2 116.72(13) . . ?
C15 C13 C14 107.85(15) . . ?
C17 C16 Si2 114.94(13) . . ?
C17 C16 C18 108.24(16) . . ?
C18 C16 Si2 112.22(14) . . ?
C20 C19 Si3 116.06(13) . . ?
C21 C19 Si3 113.91(13) . . ?
C21 C19 C20 108.08(16) . . ?
C23 C22 Si3 113.70(14) . . ?
C23 C22 C24 109.47(18) . . ?
C24 C22 Si3 116.37(14) . . ?
C26 C25 Si3 111.94(13) . . ?
C26 C25 C27 108.88(16) . . ?
C27 C25 Si3 117.98(13) . . ?
C29 C28 Si4 110.90(14) . . ?
C29 C28 C30 108.75(16) . . ?
C30 C28 Si4 120.79(13) . . ?
C32 C31 Si4 114.71(14) . . ?
C32 C31 C33 109.07(16) . . ?
C33 C31 Si4 116.78(15) . . ?
C35 C34 Si4 113.35(14) . . ?
C36 C34 Si4 114.41(14) . . ?
C36 C34 C35 108.47(17) . . ?
_shelx_res_file
;
TITL rdpm43 in P21/c #14
rdpm43.res
created by SHELXL-2016/6 at 17:52:51 on 23-Jul-2017
REM reset to P21/c #14
CELL 0.71073 15.830862 13.107736 22.537878 90 109.0428 90
ZERR 4 0.000385 0.000291 0.000615 0 0.0029 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl N Si Tm
UNIT 144 336 4 8 16 4
L.S. 4
PLAN 50
TEMP -173.15(2)
CONN 20 Tm1
FREE Tm1 Si1
FREE Tm1 Si3
FREE Tm1 Si4
BOND
fmap 2
acta
SHEL 100 0.83
REM
REM
REM
WGHT 0.025900 2.075200
FVAR 1.05280
TM1 6 0.674480 0.464232 0.774314 11.00000 0.00877 0.01288 =
0.01144 0.00041 0.00242 -0.00145
CL1 3 0.508920 0.476531 0.738405 11.00000 0.01072 0.02147 =
0.01739 0.00029 0.00330 -0.00106
SI1 5 0.771997 0.288940 0.870869 11.00000 0.01000 0.01145 =
0.01310 -0.00013 0.00299 0.00018
SI2 5 0.709748 0.472197 0.936348 11.00000 0.00868 0.01314 =
0.01182 -0.00162 0.00285 -0.00035
SI3 5 0.729662 0.527573 0.648237 11.00000 0.01107 0.01228 =
0.01252 -0.00005 0.00408 0.00033
SI4 5 0.771892 0.685494 0.760697 11.00000 0.01126 0.01225 =
0.01335 -0.00111 0.00314 -0.00237
N1 4 0.725423 0.408125 0.872508 11.00000 0.00911 0.01176 =
0.01256 -0.00235 0.00322 -0.00078
N2 4 0.739650 0.568164 0.723434 11.00000 0.00965 0.01369 =
0.01182 -0.00110 0.00216 -0.00065
C1 1 0.745630 0.261033 0.782406 11.00000 0.01759 0.01073 =
0.01638 -0.00109 0.00709 -0.00017
AFIX 13
H1 2 0.758814 0.325032 0.762918 11.00000 -1.20000
AFIX 0
C2 1 0.646179 0.236190 0.748938 11.00000 0.01913 0.01546 =
0.01691 -0.00075 0.00243 -0.00220
AFIX 137
H2A 2 0.630924 0.172217 0.765538 11.00000 -1.50000
H2B 2 0.635315 0.229056 0.703770 11.00000 -1.50000
H2C 2 0.609107 0.291512 0.756241 11.00000 -1.50000
AFIX 0
C3 1 0.802503 0.175990 0.767183 11.00000 0.02667 0.01684 =
0.02072 -0.00338 0.01026 0.00284
AFIX 137
H3A 2 0.865938 0.193768 0.784854 11.00000 -1.50000
H3B 2 0.786260 0.168556 0.721559 11.00000 -1.50000
H3C 2 0.791496 0.111537 0.785450 11.00000 -1.50000
AFIX 0
C4 1 0.898120 0.295611 0.909374 11.00000 0.01306 0.01623 =
0.01829 -0.00197 0.00446 0.00125
AFIX 13
H4 2 0.907346 0.338413 0.947703 11.00000 -1.20000
AFIX 0
C5 1 0.949559 0.196427 0.933674 11.00000 0.01575 0.02452 =
0.02894 0.00121 0.00183 0.00589
AFIX 137
H5A 2 0.924233 0.162915 0.962914 11.00000 -1.50000
H5B 2 1.012621 0.212290 0.955365 11.00000 -1.50000
H5C 2 0.944621 0.150833 0.898238 11.00000 -1.50000
AFIX 0
C6 1 0.943027 0.355734 0.869207 11.00000 0.01256 0.02501 =
0.02064 -0.00454 0.00700 -0.00236
AFIX 137
H6A 2 0.948775 0.311896 0.835508 11.00000 -1.50000
H6B 2 1.002445 0.378227 0.895598 11.00000 -1.50000
H6C 2 0.906473 0.415384 0.850924 11.00000 -1.50000
AFIX 0
C7 1 0.725108 0.180908 0.907610 11.00000 0.01658 0.01377 =
0.01480 0.00054 0.00333 -0.00199
AFIX 13
H7 2 0.754759 0.187498 0.953983 11.00000 -1.20000
AFIX 0
C8 1 0.747011 0.072050 0.890529 11.00000 0.02728 0.01458 =
0.02245 0.00310 0.00743 0.00043
AFIX 137
H8A 2 0.712282 0.057466 0.846695 11.00000 -1.50000
H8B 2 0.731704 0.022468 0.917939 11.00000 -1.50000
H8C 2 0.810926 0.067232 0.896130 11.00000 -1.50000
AFIX 0
C9 1 0.623865 0.185302 0.896674 11.00000 0.01859 0.01960 =
0.01978 -0.00062 0.00683 -0.00620
AFIX 137
H9A 2 0.607515 0.254185 0.905885 11.00000 -1.50000
H9B 2 0.608593 0.136189 0.924351 11.00000 -1.50000
H9C 2 0.591109 0.168325 0.852833 11.00000 -1.50000
AFIX 0
C10 1 0.591966 0.528495 0.903545 11.00000 0.01118 0.01752 =
0.01891 -0.00216 0.00559 -0.00010
AFIX 13
H10 2 0.587112 0.551841 0.860314 11.00000 -1.20000
AFIX 0
C11 1 0.518170 0.446822 0.893097 11.00000 0.01036 0.02428 =
0.02329 -0.00368 0.00473 -0.00239
AFIX 137
H11A 2 0.529135 0.391340 0.867388 11.00000 -1.50000
H11B 2 0.459805 0.477676 0.871538 11.00000 -1.50000
H11C 2 0.518759 0.419643 0.933737 11.00000 -1.50000
AFIX 0
C12 1 0.567343 0.622467 0.934611 11.00000 0.01550 0.02319 =
0.02833 -0.00544 0.00672 0.00214
AFIX 137
H12A 2 0.568530 0.604987 0.977153 11.00000 -1.50000
H12B 2 0.507265 0.645520 0.909901 11.00000 -1.50000
H12C 2 0.610452 0.677128 0.936693 11.00000 -1.50000
AFIX 0
C13 1 0.793648 0.581372 0.960720 11.00000 0.01144 0.01549 =
0.01444 -0.00202 0.00319 -0.00043
AFIX 13
H13 2 0.776918 0.629863 0.924483 11.00000 -1.20000
AFIX 0
C14 1 0.891165 0.550807 0.970445 11.00000 0.01222 0.01756 =
0.01569 0.00012 0.00344 -0.00153
AFIX 137
H14A 2 0.913430 0.508001 1.007988 11.00000 -1.50000
H14B 2 0.928073 0.612331 0.975768 11.00000 -1.50000
H14C 2 0.894055 0.512635 0.933769 11.00000 -1.50000
AFIX 0
C15 1 0.792520 0.644665 1.017704 11.00000 0.01493 0.02120 =
0.02369 -0.00812 0.00576 -0.00396
AFIX 137
H15A 2 0.730717 0.662200 1.013678 11.00000 -1.50000
H15B 2 0.827097 0.707342 1.019721 11.00000 -1.50000
H15C 2 0.819026 0.604889 1.056118 11.00000 -1.50000
AFIX 0
C16 1 0.718241 0.389821 1.008031 11.00000 0.01611 0.01891 =
0.01425 -0.00136 0.00509 -0.00207
AFIX 13
H16 2 0.684930 0.325220 0.992158 11.00000 -1.20000
AFIX 0
C17 1 0.813947 0.359394 1.047691 11.00000 0.01810 0.02602 =
0.01616 0.00561 0.00383 0.00081
AFIX 137
H17A 2 0.843559 0.326498 1.020742 11.00000 -1.50000
H17B 2 0.811728 0.311824 1.080696 11.00000 -1.50000
H17C 2 0.847480 0.420491 1.066882 11.00000 -1.50000
AFIX 0
C18 1 0.673037 0.440532 1.051923 11.00000 0.02395 0.02386 =
0.01765 -0.00076 0.01061 -0.00237
AFIX 137
H18A 2 0.700896 0.506926 1.065893 11.00000 -1.50000
H18B 2 0.680340 0.396691 1.088484 11.00000 -1.50000
H18C 2 0.609246 0.450095 1.029191 11.00000 -1.50000
AFIX 0
C19 1 0.639641 0.421979 0.628023 11.00000 0.01734 0.01623 =
0.01248 0.00005 0.00452 -0.00150
AFIX 13
H19 2 0.642366 0.390070 0.668909 11.00000 -1.20000
AFIX 0
C20 1 0.653184 0.334400 0.586488 11.00000 0.02835 0.01848 =
0.02699 -0.00808 0.01144 -0.00544
AFIX 137
H20A 2 0.654652 0.362107 0.546450 11.00000 -1.50000
H20B 2 0.603768 0.285713 0.578679 11.00000 -1.50000
H20C 2 0.709752 0.299641 0.607900 11.00000 -1.50000
AFIX 0
C21 1 0.543826 0.462104 0.598979 11.00000 0.01447 0.02632 =
0.01636 -0.00021 0.00208 -0.00423
AFIX 137
H21A 2 0.534621 0.520160 0.623578 11.00000 -1.50000
H21B 2 0.501343 0.407799 0.599118 11.00000 -1.50000
H21C 2 0.534365 0.483962 0.555705 11.00000 -1.50000
AFIX 0
C22 1 0.833864 0.464906 0.639166 11.00000 0.01660 0.02441 =
0.01823 0.00028 0.00970 0.00317
AFIX 13
H22 2 0.813002 0.429754 0.597522 11.00000 -1.20000
AFIX 0
C23 1 0.873370 0.380810 0.687201 11.00000 0.01902 0.02600 =
0.02664 0.00401 0.01142 0.00780
AFIX 137
H23A 2 0.895575 0.410623 0.729341 11.00000 -1.50000
H23B 2 0.922780 0.347666 0.677481 11.00000 -1.50000
H23C 2 0.827084 0.330226 0.685580 11.00000 -1.50000
AFIX 0
C24 1 0.908472 0.537036 0.636143 11.00000 0.01872 0.03264 =
0.02992 0.00282 0.01351 0.00109
AFIX 137
H24A 2 0.883118 0.591044 0.605419 11.00000 -1.50000
H24B 2 0.952946 0.498643 0.623529 11.00000 -1.50000
H24C 2 0.937088 0.567571 0.677549 11.00000 -1.50000
AFIX 0
C25 1 0.696917 0.629834 0.584796 11.00000 0.01710 0.01417 =
0.01444 0.00097 0.00437 -0.00242
AFIX 13
H25 2 0.746762 0.680641 0.596639 11.00000 -1.20000
AFIX 0
C26 1 0.693707 0.587695 0.520213 11.00000 0.02551 0.02189 =
0.01438 0.00099 0.00511 -0.00031
AFIX 137
H26A 2 0.751519 0.557042 0.523491 11.00000 -1.50000
H26B 2 0.680821 0.643432 0.489570 11.00000 -1.50000
H26C 2 0.646741 0.535833 0.506535 11.00000 -1.50000
AFIX 0
C27 1 0.610846 0.691701 0.576941 11.00000 0.01967 0.01877 =
0.01890 0.00356 0.00388 0.00018
AFIX 137
H27A 2 0.558994 0.653349 0.550639 11.00000 -1.50000
H27B 2 0.614314 0.757263 0.556963 11.00000 -1.50000
H27C 2 0.604649 0.703723 0.618240 11.00000 -1.50000
AFIX 0
C28 1 0.678756 0.710445 0.795961 11.00000 0.01724 0.01191 =
0.01826 0.00012 0.00745 -0.00016
AFIX 13
H28 2 0.671892 0.644750 0.816481 11.00000 -1.20000
AFIX 0
C29 1 0.588885 0.726861 0.744185 11.00000 0.01600 0.02012 =
0.02459 -0.00064 0.00599 0.00448
AFIX 137
H29A 2 0.588340 0.794165 0.725128 11.00000 -1.50000
H29B 2 0.540482 0.722948 0.762291 11.00000 -1.50000
H29C 2 0.580367 0.673968 0.712026 11.00000 -1.50000
AFIX 0
C30 1 0.689804 0.792041 0.846679 11.00000 0.02885 0.01537 =
0.02172 -0.00190 0.01118 0.00123
AFIX 137
H30A 2 0.741184 0.774945 0.883514 11.00000 -1.50000
H30B 2 0.635657 0.794707 0.858677 11.00000 -1.50000
H30C 2 0.699632 0.858625 0.830262 11.00000 -1.50000
AFIX 0
C31 1 0.880975 0.668658 0.827583 11.00000 0.01492 0.02287 =
0.01689 0.00175 0.00249 -0.00588
AFIX 13
H31 2 0.866722 0.620068 0.857188 11.00000 -1.20000
AFIX 0
C32 1 0.955635 0.616627 0.809144 11.00000 0.01386 0.03084 =
0.02301 0.00330 0.00078 -0.00192
AFIX 137
H32A 2 0.931479 0.556698 0.783147 11.00000 -1.50000
H32B 2 1.003425 0.595331 0.847123 11.00000 -1.50000
H32C 2 0.979676 0.664629 0.785387 11.00000 -1.50000
AFIX 0
C33 1 0.919139 0.763762 0.867306 11.00000 0.02137 0.03836 =
0.02042 -0.00727 0.00398 -0.01191
AFIX 137
H33A 2 0.934432 0.815260 0.840968 11.00000 -1.50000
H33B 2 0.972906 0.744945 0.901910 11.00000 -1.50000
H33C 2 0.874387 0.791653 0.884338 11.00000 -1.50000
AFIX 0
C34 1 0.779419 0.797729 0.708692 11.00000 0.02288 0.01409 =
0.01619 0.00035 0.00390 -0.00545
AFIX 13
H34 2 0.731039 0.787859 0.667540 11.00000 -1.20000
AFIX 0
C35 1 0.868101 0.801611 0.694614 11.00000 0.02709 0.02802 =
0.02007 0.00252 0.00761 -0.01128
AFIX 137
H35A 2 0.917143 0.816182 0.733396 11.00000 -1.50000
H35B 2 0.865075 0.855403 0.663788 11.00000 -1.50000
H35C 2 0.878598 0.735724 0.677686 11.00000 -1.50000
AFIX 0
C36 1 0.763414 0.902505 0.733659 11.00000 0.04174 0.01357 =
0.02565 0.00179 0.01101 -0.00413
AFIX 137
H36A 2 0.702448 0.905492 0.735470 11.00000 -1.50000
H36B 2 0.771341 0.956090 0.705613 11.00000 -1.50000
H36C 2 0.806244 0.912772 0.775822 11.00000 -1.50000
AFIX 0
HKLF 4
REM rdpm43 in P21/c #14
REM R1 = 0.0185 for 7461 Fo > 4sig(Fo) and 0.0210 for all 8039 data
REM 421 parameters refined using 0 restraints
END
WGHT 0.0259 2.0752
REM Highest difference peak 0.586, deepest hole -0.601, 1-sigma level 0.064
Q1 1 0.6244 0.4656 0.7328 11.00000 0.05 0.59
Q2 1 0.7157 0.4639 0.8148 11.00000 0.05 0.55
Q3 1 0.7152 0.5137 0.7574 11.00000 0.05 0.55
Q4 1 0.6366 0.4228 0.7891 11.00000 0.05 0.53
Q5 1 0.6436 0.5221 0.7878 11.00000 0.05 0.51
Q6 1 0.7150 0.4167 0.7595 11.00000 0.05 0.50
Q7 1 0.7475 0.2270 0.8842 11.00000 0.05 0.46
Q8 1 0.7223 0.6993 0.7788 11.00000 0.05 0.45
Q9 1 0.7449 0.5332 0.7425 11.00000 0.05 0.43
Q10 1 0.7049 0.4685 0.7390 11.00000 0.05 0.41
Q11 1 0.8352 0.6800 0.7944 11.00000 0.05 0.38
Q12 1 0.7822 0.7542 0.7304 11.00000 0.05 0.37
Q13 1 0.7662 0.6175 0.7412 11.00000 0.05 0.35
Q14 1 0.7531 0.3602 0.8671 11.00000 0.05 0.34
Q15 1 0.7334 0.6164 0.7286 11.00000 0.05 0.34
Q16 1 0.7385 0.4263 0.9030 11.00000 0.05 0.34
Q17 1 0.7523 0.5628 0.6957 11.00000 0.05 0.33
Q18 1 0.8408 0.2859 0.8942 11.00000 0.05 0.33
Q19 1 0.7574 0.5368 0.9523 11.00000 0.05 0.32
Q20 1 0.5237 0.4601 0.7044 11.00000 0.05 0.32
Q21 1 0.7587 0.2595 0.8249 11.00000 0.05 0.32
Q22 1 0.7158 0.2422 0.7798 11.00000 0.05 0.31
Q23 1 0.6356 0.7173 0.7676 11.00000 0.05 0.31
Q24 1 0.7334 0.4332 0.8599 11.00000 0.05 0.31
Q25 1 0.7268 0.4271 0.9774 11.00000 0.05 0.30
Q26 1 0.9197 0.3229 0.8931 11.00000 0.05 0.29
Q27 1 0.7046 0.5851 0.6096 11.00000 0.05 0.29
Q28 1 0.5549 0.4915 0.8999 11.00000 0.05 0.29
Q29 1 0.6436 0.5056 0.9156 11.00000 0.05 0.29
Q30 1 0.6854 0.4613 0.6491 11.00000 0.05 0.28
Q31 1 0.6594 0.6597 0.5802 11.00000 0.05 0.28
Q32 1 0.7640 0.3714 1.0223 11.00000 0.05 0.28
Q33 1 0.7636 0.8437 0.7198 11.00000 0.05 0.27
Q34 1 0.8319 0.5759 0.9633 11.00000 0.05 0.26
Q35 1 0.6122 0.3855 0.7383 11.00000 0.05 0.26
Q36 1 0.9088 0.2362 0.9099 11.00000 0.05 0.25
Q37 1 0.7944 0.6063 0.9901 11.00000 0.05 0.25
Q38 1 0.7953 0.4894 0.6479 11.00000 0.05 0.25
Q39 1 0.7343 0.3169 0.7803 11.00000 0.05 0.25
Q40 1 0.7742 0.2234 0.7708 11.00000 0.05 0.24
Q41 1 0.7332 0.5064 0.8615 11.00000 0.05 0.24
Q42 1 0.7390 0.1354 0.8967 11.00000 0.05 0.24
Q43 1 0.6964 0.4212 1.0229 11.00000 0.05 0.24
Q44 1 0.6135 0.4204 0.6897 11.00000 0.05 0.23
Q45 1 0.7484 0.3900 0.7398 11.00000 0.05 0.23
Q46 1 0.7176 0.9153 0.7499 11.00000 0.05 0.23
Q47 1 0.9133 0.6516 0.8190 11.00000 0.05 0.23
Q48 1 0.7519 0.2024 0.9385 11.00000 0.05 0.22
Q49 1 0.8297 0.7874 0.6991 11.00000 0.05 0.22
Q50 1 0.8930 0.7199 0.8411 11.00000 0.05 0.21
;
_shelx_res_checksum 81991
_olex2_date_sample_data_collection 2017-07-22
_olex2_date_sample_submission 2017-07-22
_olex2_exptl_crystal_mounting_method 'From fomblin on a microscope slide.'
_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 1.720
_oxdiff_exptl_absorpt_empirical_full_min 0.493
#######################################################################
#
# 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_xdpm75
_database_code_depnum_ccdc_archive 'CCDC 1880944'
loop_
_audit_author_name
_audit_author_address
'Hannah Nicholas'
;The University of Manchester
United Kingdom
;
_audit_update_record
;
2018-11-23 deposited with the CCDC. 2019-09-18 downloaded from the CCDC.
;
_manchester_internal_coll_name xdpm75
_manchester_internal_coll_client HN/SWL/CAPG
_manchester_internal_coll_type custom
_manchester_internal_coll_frame_time 7/12s
_manchester_internal_coll_frame_width 1.0
_manchester_internal_coll_frame_method '\w & \f scans'
_manchester_internal_coll_user CAPG/HN
_manchester_internal_coll_date 02/8/17
_manchester_internal_process_user CAPG
_manchester_internal_process_date 02/8/17
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 03/8/17
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 24/8/17
_manchester_internal_validation_user ?
_manchester_internal_validation_date ?
_manchester_internal_archive_date ?
_refine_special_details
;
Positional disorder is evident at the DCM moiety (C61, Cl1-2) however
attempts to model this as multiple components over different positions
did not lead to an improvement of the model, and it has thus been refined
over an average position with an occupancy of 1, and restraints were applied
to reduce the oblate nature of C61.
;
_audit_creation_date 2017-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H84 N2 Si4 Yb, B C24 F20, C H2 Cl2'
_chemical_formula_sum 'C61 H86 B Cl2 F20 N2 Si4 Yb'
_chemical_formula_weight 1594.42
_chemical_melting_point ?
_chemical_oxdiff_formula Yb(N(SiC9H21)2)2B(C6F5)4CH2Cl2
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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -7.2108 4.4329 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 16.0620(3)
_cell_length_b 25.9262(6)
_cell_length_c 16.7464(3)
_cell_angle_alpha 90
_cell_angle_beta 92.749(2)
_cell_angle_gamma 90
_cell_volume 6965.6(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 10054
_cell_measurement_temperature 150.0(2)
_cell_measurement_theta_max 74.6820
_cell_measurement_theta_min 3.1160
_shelx_estimated_absorpt_T_max 0.653
_shelx_estimated_absorpt_T_min 0.335
_exptl_absorpt_coefficient_mu 4.666
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.58628
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear violet'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary violet
_exptl_crystal_density_diffrn 1.520
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 3244
_exptl_crystal_preparation ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0732
_diffrn_reflns_av_unetI/netI 0.1021
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 31
_diffrn_reflns_limit_k_min -31
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 28972
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 68.247
_diffrn_reflns_theta_min 3.144
_diffrn_ambient_temperature 150.0(2)
_diffrn_detector 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.980
_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 83.90 269.84 1.00 12.00 -- 112.68 73.87-175.79 186
2 \w 83.90 268.90 1.00 12.00 -- 112.68 73.87 -55.79 185
3 \w -68.18 116.82 1.00 7.00 -- -39.39 73.87-160.79 185
4 \w 67.90 254.90 1.00 12.00 -- 97.68 73.87 64.21 187
5 \w 3.12 188.12 1.00 7.00 -- 31.90 73.87 76.21 185
;
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker SMART APEX2 area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0344668000
_diffrn_orient_matrix_UB_12 -0.0172842000
_diffrn_orient_matrix_UB_13 -0.0799338000
_diffrn_orient_matrix_UB_21 0.0345447000
_diffrn_orient_matrix_UB_22 0.0546178000
_diffrn_orient_matrix_UB_23 -0.0128027000
_diffrn_orient_matrix_UB_31 0.0827665000
_diffrn_orient_matrix_UB_32 -0.0156570000
_diffrn_orient_matrix_UB_33 0.0439255000
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_diffrn_special_details ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 8206
_reflns_number_total 12492
_reflns_odcompleteness_completeness 98.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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 ?
_refine_diff_density_max 0.791
_refine_diff_density_min -0.780
_refine_diff_density_rms 0.108
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.007
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 844
_refine_ls_number_reflns 12492
_refine_ls_number_restraints 30
_refine_ls_R_factor_all 0.1003
_refine_ls_R_factor_gt 0.0560
_refine_ls_restrained_S_all 1.015
_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^)+(0.0520P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1146
_refine_ls_wR_factor_ref 0.1337
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
Cl2-C61 = Cl1-C61
1.753 with sigma of 0.02
3. Rigid bond restraints
C61, Cl1, Cl2, H61A, H61B
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C61 \\sim Cl1 \\sim Cl2 \\sim H61A \\sim H61B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
5.a Ternary CH refined with riding coordinates:
C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16), C19(H19), C22(H22),
C25(H25), C28(H28), C31(H31), C34(H34)
5.b Secondary CH2 refined with riding coordinates:
C61(H61A,H61B)
5.c Idealised Me refined as rotating group:
C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,
H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C),
C36(H36A,H36B,H36C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.33640(2) 0.35236(2) 0.71553(2) 0.02562(9) Uani 1 1 d . . . . .
Si1 Si 0.47662(10) 0.31529(6) 0.60050(11) 0.0265(4) Uani 1 1 d . . . . .
Si2 Si 0.36125(10) 0.23242(6) 0.68689(11) 0.0266(4) Uani 1 1 d . . . . .
Si3 Si 0.23368(11) 0.40968(7) 0.83682(11) 0.0294(4) Uani 1 1 d . . . . .
Si4 Si 0.39956(11) 0.36733(7) 0.92054(11) 0.0320(4) Uani 1 1 d . . . . .
N1 N 0.4103(3) 0.29071(18) 0.6701(3) 0.0253(11) Uani 1 1 d . . . . .
N2 N 0.3299(3) 0.37714(18) 0.8372(3) 0.0250(11) Uani 1 1 d . . . . .
C1 C 0.4460(4) 0.3874(2) 0.5971(4) 0.0311(14) Uani 1 1 d . . . . .
H1 H 0.384379 0.388513 0.585463 0.037 Uiso 1 1 calc R . . . .
C2 C 0.4633(4) 0.4202(2) 0.6734(4) 0.0348(16) Uani 1 1 d . . . . .
H2A H 0.448072 0.400384 0.720401 0.052 Uiso 1 1 calc GR . . . .
H2B H 0.430224 0.451889 0.669764 0.052 Uiso 1 1 calc GR . . . .
H2C H 0.522710 0.428939 0.678395 0.052 Uiso 1 1 calc GR . . . .
C3 C 0.4859(4) 0.4175(2) 0.5289(4) 0.0350(16) Uani 1 1 d . . . . .
H3A H 0.546727 0.415526 0.535771 0.052 Uiso 1 1 calc GR . . . .
H3B H 0.468330 0.453678 0.530523 0.052 Uiso 1 1 calc GR . . . .
H3C H 0.467817 0.402384 0.477340 0.052 Uiso 1 1 calc GR . . . .
C4 C 0.4558(4) 0.2888(2) 0.4967(4) 0.0296(14) Uani 1 1 d . . . . .
H4 H 0.454869 0.250458 0.502869 0.036 Uiso 1 1 calc R . . . .
C5 C 0.3690(4) 0.3036(3) 0.4601(4) 0.0374(16) Uani 1 1 d . . . . .
H5A H 0.326375 0.295354 0.498084 0.056 Uiso 1 1 calc GR . . . .
H5B H 0.357878 0.284190 0.410524 0.056 Uiso 1 1 calc GR . . . .
H5C H 0.367630 0.340645 0.448468 0.056 Uiso 1 1 calc GR . . . .
C6 C 0.5224(4) 0.3002(3) 0.4346(4) 0.0385(16) Uani 1 1 d . . . . .
H6A H 0.526897 0.337500 0.426776 0.058 Uiso 1 1 calc GR . . . .
H6B H 0.505774 0.283688 0.383588 0.058 Uiso 1 1 calc GR . . . .
H6C H 0.576412 0.286431 0.454177 0.058 Uiso 1 1 calc GR . . . .
C7 C 0.5924(4) 0.3087(3) 0.6245(4) 0.0354(16) Uani 1 1 d . . . . .
H7 H 0.619989 0.329222 0.582676 0.043 Uiso 1 1 calc R . . . .
C8 C 0.6260(4) 0.3305(3) 0.7045(5) 0.050(2) Uani 1 1 d . . . . .
H8A H 0.613365 0.367435 0.707029 0.075 Uiso 1 1 calc GR . . . .
H8B H 0.686504 0.325466 0.709546 0.075 Uiso 1 1 calc GR . . . .
H8C H 0.599733 0.312593 0.748269 0.075 Uiso 1 1 calc GR . . . .
C9 C 0.6237(4) 0.2531(3) 0.6150(4) 0.0418(18) Uani 1 1 d . . . . .
H9A H 0.598728 0.230900 0.654788 0.063 Uiso 1 1 calc GR . . . .
H9B H 0.684535 0.252326 0.623039 0.063 Uiso 1 1 calc GR . . . .
H9C H 0.607810 0.240559 0.561222 0.063 Uiso 1 1 calc GR . . . .
C10 C 0.2507(4) 0.2552(2) 0.7100(4) 0.0313(15) Uani 1 1 d . . . . .
H10 H 0.258516 0.283593 0.750003 0.038 Uiso 1 1 calc R . . . .
C11 C 0.2044(4) 0.2798(3) 0.6359(4) 0.0345(15) Uani 1 1 d . . . . .
H11A H 0.237240 0.308714 0.616639 0.052 Uiso 1 1 calc GR . . . .
H11B H 0.149728 0.292334 0.650824 0.052 Uiso 1 1 calc GR . . . .
H11C H 0.197063 0.253911 0.593526 0.052 Uiso 1 1 calc GR . . . .
C12 C 0.1928(4) 0.2159(3) 0.7477(4) 0.0392(17) Uani 1 1 d . . . . .
H12A H 0.218870 0.203243 0.797988 0.059 Uiso 1 1 calc GR . . . .
H12B H 0.182842 0.186945 0.710865 0.059 Uiso 1 1 calc GR . . . .
H12C H 0.139595 0.232543 0.758194 0.059 Uiso 1 1 calc GR . . . .
C13 C 0.3555(4) 0.1881(2) 0.5975(4) 0.0353(15) Uani 1 1 d . . . . .
H13 H 0.350144 0.211111 0.549545 0.042 Uiso 1 1 calc R . . . .
C14 C 0.4377(4) 0.1580(3) 0.5896(5) 0.0450(19) Uani 1 1 d . . . . .
H14A H 0.484698 0.182137 0.591947 0.068 Uiso 1 1 calc GR . . . .
H14B H 0.436100 0.139605 0.538437 0.068 Uiso 1 1 calc GR . . . .
H14C H 0.444470 0.133107 0.633515 0.068 Uiso 1 1 calc GR . . . .
C15 C 0.2813(4) 0.1510(3) 0.5901(5) 0.0465(18) Uani 1 1 d . . . . .
H15A H 0.278460 0.130854 0.639408 0.070 Uiso 1 1 calc GR . . . .
H15B H 0.288244 0.127616 0.544888 0.070 Uiso 1 1 calc GR . . . .
H15C H 0.229612 0.170729 0.581203 0.070 Uiso 1 1 calc GR . . . .
C16 C 0.4032(4) 0.2004(2) 0.7818(4) 0.0310(14) Uani 1 1 d . . . . .
H16 H 0.379191 0.220455 0.826278 0.037 Uiso 1 1 calc R . . . .
C17 C 0.4983(4) 0.2044(3) 0.7961(5) 0.050(2) Uani 1 1 d . . . . .
H17A H 0.525656 0.180711 0.759978 0.075 Uiso 1 1 calc GR . . . .
H17B H 0.513616 0.195106 0.851633 0.075 Uiso 1 1 calc GR . . . .
H17C H 0.516288 0.239770 0.785845 0.075 Uiso 1 1 calc GR . . . .
C18 C 0.3762(4) 0.1442(3) 0.7949(5) 0.0448(18) Uani 1 1 d . . . . .
H18A H 0.390138 0.134190 0.850352 0.067 Uiso 1 1 calc GR . . . .
H18B H 0.405317 0.121563 0.758646 0.067 Uiso 1 1 calc GR . . . .
H18C H 0.315879 0.141148 0.784046 0.067 Uiso 1 1 calc GR . . . .
C19 C 0.1888(4) 0.4006(2) 0.7284(4) 0.0313(15) Uani 1 1 d . . . . .
H19 H 0.195227 0.363097 0.716388 0.038 Uiso 1 1 calc R . . . .
C20 C 0.2316(4) 0.4297(3) 0.6595(4) 0.0402(17) Uani 1 1 d . . . . .
H20A H 0.292164 0.429156 0.669599 0.060 Uiso 1 1 calc GR . . . .
H20B H 0.212090 0.465554 0.657429 0.060 Uiso 1 1 calc GR . . . .
H20C H 0.217203 0.412735 0.608457 0.060 Uiso 1 1 calc GR . . . .
C21 C 0.0940(4) 0.4121(3) 0.7161(5) 0.0436(19) Uani 1 1 d . . . . .
H21A H 0.073744 0.399214 0.663690 0.065 Uiso 1 1 calc GR . . . .
H21B H 0.084685 0.449444 0.718737 0.065 Uiso 1 1 calc GR . . . .
H21C H 0.063783 0.394995 0.758092 0.065 Uiso 1 1 calc GR . . . .
C22 C 0.2440(4) 0.4815(2) 0.8580(4) 0.0383(17) Uani 1 1 d . . . . .
H22 H 0.248789 0.485015 0.917538 0.046 Uiso 1 1 calc R . . . .
C23 C 0.1664(4) 0.5122(3) 0.8302(5) 0.051(2) Uani 1 1 d . . . . .
H23A H 0.167776 0.518716 0.772602 0.076 Uiso 1 1 calc GR . . . .
H23B H 0.165694 0.545156 0.858835 0.076 Uiso 1 1 calc GR . . . .
H23C H 0.116298 0.492447 0.841270 0.076 Uiso 1 1 calc GR . . . .
C24 C 0.3219(4) 0.5068(3) 0.8265(5) 0.050(2) Uani 1 1 d . . . . .
H24A H 0.318507 0.506324 0.767961 0.075 Uiso 1 1 calc GR . . . .
H24B H 0.371439 0.487654 0.846061 0.075 Uiso 1 1 calc GR . . . .
H24C H 0.325678 0.542493 0.845423 0.075 Uiso 1 1 calc GR . . . .
C25 C 0.1596(4) 0.3774(3) 0.9069(4) 0.0397(17) Uani 1 1 d . . . . .
H25 H 0.195946 0.366266 0.953932 0.048 Uiso 1 1 calc R . . . .
C26 C 0.0928(5) 0.4107(3) 0.9423(5) 0.060(3) Uani 1 1 d . . . . .
H26A H 0.067507 0.391977 0.985781 0.090 Uiso 1 1 calc GR . . . .
H26B H 0.049881 0.419007 0.900733 0.090 Uiso 1 1 calc GR . . . .
H26C H 0.118024 0.442717 0.963222 0.090 Uiso 1 1 calc GR . . . .
C27 C 0.1197(4) 0.3272(3) 0.8741(5) 0.0429(18) Uani 1 1 d . . . . .
H27A H 0.162854 0.305354 0.852077 0.064 Uiso 1 1 calc GR . . . .
H27B H 0.077475 0.335492 0.831885 0.064 Uiso 1 1 calc GR . . . .
H27C H 0.093525 0.308778 0.917390 0.064 Uiso 1 1 calc GR . . . .
C28 C 0.5076(4) 0.3725(3) 0.8789(4) 0.0391(16) Uani 1 1 d . . . . .
H28 H 0.501041 0.357095 0.824138 0.047 Uiso 1 1 calc R . . . .
C29 C 0.5346(4) 0.4287(3) 0.8644(5) 0.050(2) Uani 1 1 d . . . . .
H29A H 0.555006 0.444119 0.915116 0.075 Uiso 1 1 calc GR . . . .
H29B H 0.486908 0.448588 0.842499 0.075 Uiso 1 1 calc GR . . . .
H29C H 0.579215 0.429214 0.826443 0.075 Uiso 1 1 calc GR . . . .
C30 C 0.5794(4) 0.3422(3) 0.9199(5) 0.052(2) Uani 1 1 d . . . . .
H30A H 0.628575 0.344455 0.887628 0.078 Uiso 1 1 calc GR . . . .
H30B H 0.563058 0.306017 0.925251 0.078 Uiso 1 1 calc GR . . . .
H30C H 0.592438 0.356845 0.972947 0.078 Uiso 1 1 calc GR . . . .
C31 C 0.3912(4) 0.2978(3) 0.9567(4) 0.0411(17) Uani 1 1 d . . . . .
H31 H 0.422082 0.276848 0.917764 0.049 Uiso 1 1 calc R . . . .
C32 C 0.3048(5) 0.2747(3) 0.9559(5) 0.0477(19) Uani 1 1 d . . . . .
H32A H 0.309065 0.237465 0.965361 0.072 Uiso 1 1 calc GR . . . .
H32B H 0.276245 0.280967 0.903787 0.072 Uiso 1 1 calc GR . . . .
H32C H 0.273188 0.290636 0.997984 0.072 Uiso 1 1 calc GR . . . .
C33 C 0.4355(5) 0.2865(3) 1.0401(5) 0.055(2) Uani 1 1 d . . . . .
H33A H 0.491612 0.301453 1.041996 0.083 Uiso 1 1 calc GR . . . .
H33B H 0.439382 0.249165 1.048282 0.083 Uiso 1 1 calc GR . . . .
H33C H 0.403252 0.301891 1.082270 0.083 Uiso 1 1 calc GR . . . .
C34 C 0.3918(5) 0.4172(3) 1.0029(4) 0.0449(18) Uani 1 1 d . . . . .
H34 H 0.388681 0.451525 0.975532 0.054 Uiso 1 1 calc R . . . .
C35 C 0.3146(5) 0.4142(3) 1.0542(5) 0.058(2) Uani 1 1 d . . . . .
H35A H 0.264379 0.422235 1.020940 0.088 Uiso 1 1 calc GR . . . .
H35B H 0.320395 0.439092 1.098157 0.088 Uiso 1 1 calc GR . . . .
H35C H 0.309880 0.379312 1.076102 0.088 Uiso 1 1 calc GR . . . .
C36 C 0.4698(5) 0.4194(3) 1.0608(5) 0.058(2) Uani 1 1 d . . . . .
H36A H 0.519226 0.426582 1.030470 0.086 Uiso 1 1 calc GR . . . .
H36B H 0.476801 0.386213 1.088303 0.086 Uiso 1 1 calc GR . . . .
H36C H 0.462875 0.446792 1.100257 0.086 Uiso 1 1 calc GR . . . .
F1 F 0.0429(2) 0.51282(13) 0.3648(2) 0.0353(9) Uani 1 1 d . . . . .
F2 F -0.0828(2) 0.47052(15) 0.4402(3) 0.0415(10) Uani 1 1 d . . . . .
F3 F -0.0605(2) 0.37835(16) 0.5179(3) 0.0481(11) Uani 1 1 d . . . . .
F4 F 0.0872(2) 0.32914(16) 0.5124(3) 0.0457(11) Uani 1 1 d . . . . .
F5 F 0.2115(2) 0.36849(14) 0.4357(2) 0.0379(9) Uani 1 1 d . . . . .
F6 F 0.3957(2) 0.49051(14) 0.3671(2) 0.0345(9) Uani 1 1 d . . . . .
F7 F 0.5133(2) 0.43057(17) 0.3127(2) 0.0463(11) Uani 1 1 d . . . . .
F8 F 0.4746(2) 0.34048(17) 0.2373(2) 0.0486(11) Uani 1 1 d . . . . .
F9 F 0.3109(2) 0.31210(15) 0.2160(3) 0.0459(10) Uani 1 1 d . . . . .
F10 F 0.1907(2) 0.37221(14) 0.2662(2) 0.0361(9) Uani 1 1 d . . . . .
F11 F 0.0500(2) 0.44088(14) 0.2383(2) 0.0355(9) Uani 1 1 d . . . . .
F12 F 0.0167(2) 0.47171(15) 0.0906(2) 0.0369(9) Uani 1 1 d . . . . .
F13 F 0.1194(2) 0.53942(16) 0.0177(2) 0.0411(10) Uani 1 1 d . . . . .
F14 F 0.2601(2) 0.57245(15) 0.0972(2) 0.0414(10) Uani 1 1 d . . . . .
F15 F 0.2969(2) 0.54190(14) 0.2472(2) 0.0330(8) Uani 1 1 d . . . . .
F16 F 0.1708(2) 0.58821(14) 0.3294(2) 0.0372(9) Uani 1 1 d . . . . .
F17 F 0.2151(2) 0.65832(13) 0.4374(3) 0.0429(10) Uani 1 1 d . . . . .
F18 F 0.2967(2) 0.63120(16) 0.5781(3) 0.0511(11) Uani 1 1 d . . . . .
F19 F 0.3365(3) 0.53023(18) 0.6045(2) 0.0481(11) Uani 1 1 d . . . . .
F20 F 0.2962(2) 0.45899(14) 0.4955(2) 0.0323(8) Uani 1 1 d . . . . .
C37 C 0.1327(3) 0.4423(2) 0.3922(4) 0.0252(13) Uani 1 1 d . . . . .
C38 C 0.0558(4) 0.4662(2) 0.3988(4) 0.0279(13) Uani 1 1 d . . . . .
C39 C -0.0089(4) 0.4456(3) 0.4397(4) 0.0294(14) Uani 1 1 d . . . . .
C40 C 0.0011(3) 0.3999(3) 0.4786(4) 0.0303(14) Uani 1 1 d . . . . .
C41 C 0.0763(4) 0.3747(3) 0.4754(4) 0.0320(15) Uani 1 1 d . . . . .
C42 C 0.1396(3) 0.3965(2) 0.4334(4) 0.0276(13) Uani 1 1 d . . . . .
C43 C 0.2856(3) 0.4341(2) 0.3218(3) 0.0229(12) Uani 1 1 d . . . . .
C44 C 0.3704(4) 0.4467(2) 0.3305(4) 0.0281(14) Uani 1 1 d . . . . .
C45 C 0.4328(4) 0.4154(3) 0.3017(4) 0.0342(15) Uani 1 1 d . . . . .
C46 C 0.4139(4) 0.3703(3) 0.2645(4) 0.0361(16) Uani 1 1 d . . . . .
C47 C 0.3319(4) 0.3566(3) 0.2537(4) 0.0314(14) Uani 1 1 d . . . . .
C48 C 0.2707(4) 0.3880(2) 0.2816(4) 0.0282(13) Uani 1 1 d . . . . .
C49 C 0.1744(4) 0.4909(2) 0.2530(4) 0.0251(13) Uani 1 1 d . . . . .
C50 C 0.1046(3) 0.4747(2) 0.2081(4) 0.0253(13) Uani 1 1 d . . . . .
C51 C 0.0855(4) 0.4898(3) 0.1308(4) 0.0305(14) Uani 1 1 d . . . . .
C52 C 0.1372(4) 0.5234(2) 0.0931(4) 0.0307(14) Uani 1 1 d . . . . .
C53 C 0.2085(4) 0.5404(2) 0.1329(4) 0.0300(14) Uani 1 1 d . . . . .
C54 C 0.2253(3) 0.5239(2) 0.2107(4) 0.0288(14) Uani 1 1 d . . . . .
C55 C 0.2337(3) 0.5195(2) 0.4054(4) 0.0282(14) Uani 1 1 d . . . . .
C56 C 0.2141(4) 0.5714(3) 0.3956(4) 0.0329(15) Uani 1 1 d . . . . .
C57 C 0.2353(4) 0.6093(2) 0.4519(5) 0.0340(16) Uani 1 1 d . . . . .
C58 C 0.2762(4) 0.5951(3) 0.5215(4) 0.0359(16) Uani 1 1 d . . . . .
C59 C 0.2957(4) 0.5445(3) 0.5356(4) 0.0372(17) Uani 1 1 d . . . . .
C60 C 0.2744(4) 0.5084(3) 0.4781(4) 0.0307(14) Uani 1 1 d . . . . .
B1 B 0.2058(4) 0.4719(3) 0.3432(4) 0.0251(15) Uani 1 1 d . . . . .
Cl1 Cl -0.11901(19) 0.33222(12) 0.8611(3) 0.1192(13) Uani 1 1 d D U . . .
Cl2 Cl -0.0451(3) 0.29066(15) 0.7208(2) 0.1323(13) Uani 1 1 d D U . . .
C61 C -0.1360(8) 0.3069(6) 0.7661(8) 0.140(3) Uani 1 1 d D U . . .
H61A H -0.171242 0.275692 0.769352 0.168 Uiso 1 1 calc R U . . .
H61B H -0.166943 0.332411 0.732259 0.168 Uiso 1 1 calc R U . . .
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
Yb1 0.02729(15) 0.02361(15) 0.02657(15) 0.00198(17) 0.00751(12) 0.00425(14)
Si1 0.0261(8) 0.0247(8) 0.0290(8) 0.0028(8) 0.0067(7) 0.0033(7)
Si2 0.0284(8) 0.0216(8) 0.0300(8) 0.0019(8) 0.0027(7) 0.0038(7)
Si3 0.0328(9) 0.0240(8) 0.0325(9) 0.0005(8) 0.0146(8) 0.0027(7)
Si4 0.0375(9) 0.0318(9) 0.0267(8) 0.0008(8) 0.0017(8) 0.0006(7)
N1 0.025(2) 0.018(2) 0.033(3) -0.006(2) 0.009(2) 0.0035(19)
N2 0.033(3) 0.023(2) 0.020(2) 0.004(2) 0.009(2) 0.002(2)
C1 0.030(3) 0.030(3) 0.035(4) 0.002(3) 0.007(3) 0.002(3)
C2 0.034(3) 0.032(3) 0.040(4) -0.002(3) 0.011(3) -0.002(3)
C3 0.035(3) 0.032(3) 0.039(4) 0.007(3) 0.013(3) 0.000(3)
C4 0.031(3) 0.027(3) 0.031(3) -0.001(3) 0.002(3) 0.005(3)
C5 0.044(4) 0.041(4) 0.028(3) 0.001(3) 0.005(3) 0.002(3)
C6 0.042(4) 0.045(4) 0.029(3) 0.002(3) 0.012(3) 0.006(3)
C7 0.030(3) 0.038(4) 0.039(4) 0.006(4) 0.011(3) -0.001(3)
C8 0.029(3) 0.059(5) 0.061(5) -0.002(5) -0.001(4) 0.002(3)
C9 0.032(3) 0.046(4) 0.047(4) 0.003(4) 0.008(3) 0.012(3)
C10 0.031(3) 0.026(3) 0.037(4) 0.003(3) 0.009(3) 0.003(3)
C11 0.028(3) 0.035(4) 0.040(4) 0.002(3) 0.003(3) 0.003(3)
C12 0.032(3) 0.039(4) 0.047(4) 0.004(4) 0.014(3) -0.004(3)
C13 0.038(4) 0.026(3) 0.042(4) -0.005(3) 0.002(3) 0.000(3)
C14 0.041(4) 0.033(4) 0.062(5) -0.005(4) 0.009(4) 0.007(3)
C15 0.057(4) 0.031(4) 0.051(4) -0.010(4) 0.003(4) -0.003(4)
C16 0.034(3) 0.026(3) 0.033(3) 0.008(3) 0.002(3) 0.002(3)
C17 0.047(4) 0.046(4) 0.056(5) 0.010(4) -0.008(4) 0.003(4)
C18 0.053(4) 0.030(4) 0.051(4) 0.014(4) 0.000(4) 0.003(3)
C19 0.025(3) 0.026(3) 0.043(4) 0.006(3) 0.009(3) 0.005(2)
C20 0.044(4) 0.033(4) 0.044(4) 0.011(4) 0.013(4) 0.005(3)
C21 0.035(4) 0.043(4) 0.053(5) 0.012(4) 0.009(4) 0.012(3)
C22 0.052(4) 0.025(3) 0.039(4) 0.002(3) 0.016(4) 0.004(3)
C23 0.047(4) 0.030(4) 0.078(6) -0.004(4) 0.025(4) 0.008(3)
C24 0.047(4) 0.030(4) 0.075(6) 0.004(4) 0.018(4) -0.004(3)
C25 0.045(4) 0.035(4) 0.042(4) 0.009(4) 0.024(3) 0.001(3)
C26 0.069(5) 0.038(4) 0.078(6) 0.002(5) 0.051(5) 0.002(4)
C27 0.044(4) 0.038(4) 0.048(4) 0.011(4) 0.014(4) -0.001(3)
C28 0.033(3) 0.044(4) 0.039(4) -0.004(4) -0.001(3) 0.002(3)
C29 0.040(4) 0.067(5) 0.043(4) -0.003(4) 0.002(4) -0.015(4)
C30 0.041(4) 0.057(5) 0.056(5) 0.010(4) -0.014(4) 0.008(4)
C31 0.051(4) 0.043(4) 0.030(4) 0.001(4) 0.004(3) 0.000(3)
C32 0.064(5) 0.034(4) 0.047(4) 0.014(4) 0.015(4) -0.002(4)
C33 0.079(6) 0.049(5) 0.037(4) 0.001(4) -0.003(4) 0.006(4)
C34 0.056(5) 0.045(4) 0.034(4) 0.000(4) 0.003(4) -0.002(4)
C35 0.083(6) 0.047(5) 0.046(5) -0.008(4) 0.009(5) 0.010(4)
C36 0.073(6) 0.058(5) 0.041(4) -0.013(4) -0.007(4) -0.008(4)
F1 0.0311(18) 0.0308(19) 0.044(2) -0.0018(19) 0.0007(17) 0.0035(15)
F2 0.0270(18) 0.048(2) 0.050(2) -0.009(2) 0.0080(18) 0.0043(17)
F3 0.031(2) 0.058(3) 0.056(3) 0.012(2) 0.014(2) -0.0086(19)
F4 0.035(2) 0.051(2) 0.051(3) 0.023(2) 0.005(2) -0.0045(18)
F5 0.0256(17) 0.041(2) 0.048(2) 0.014(2) 0.0054(17) 0.0042(15)
F6 0.0264(17) 0.039(2) 0.038(2) -0.0068(19) 0.0012(16) -0.0071(15)
F7 0.0208(17) 0.070(3) 0.048(2) 0.000(2) 0.0048(18) 0.0027(18)
F8 0.043(2) 0.064(3) 0.040(2) -0.006(2) 0.0089(19) 0.021(2)
F9 0.052(2) 0.039(2) 0.046(2) -0.014(2) 0.004(2) 0.0066(18)
F10 0.0305(18) 0.0334(19) 0.044(2) -0.0085(19) 0.0012(17) -0.0040(15)
F11 0.0300(18) 0.041(2) 0.036(2) -0.0009(19) 0.0017(17) -0.0122(16)
F12 0.0284(18) 0.050(2) 0.0313(19) -0.001(2) -0.0040(17) -0.0038(17)
F13 0.041(2) 0.051(2) 0.031(2) 0.008(2) -0.0036(18) -0.0009(18)
F14 0.040(2) 0.049(2) 0.034(2) 0.014(2) -0.0045(18) -0.0112(18)
F15 0.0287(18) 0.038(2) 0.0316(19) 0.0055(18) -0.0024(16) -0.0117(15)
F16 0.041(2) 0.032(2) 0.039(2) -0.0017(19) -0.0006(19) 0.0042(16)
F17 0.036(2) 0.029(2) 0.064(3) -0.011(2) 0.013(2) -0.0038(16)
F18 0.049(2) 0.056(3) 0.049(3) -0.026(2) 0.012(2) -0.020(2)
F19 0.051(2) 0.066(3) 0.027(2) -0.003(2) -0.0036(19) -0.017(2)
F20 0.0320(18) 0.038(2) 0.0273(18) 0.0034(18) 0.0004(16) -0.0015(16)
C37 0.024(3) 0.028(3) 0.023(3) -0.003(3) 0.000(3) -0.005(2)
C38 0.028(3) 0.025(3) 0.030(3) 0.000(3) 0.000(3) 0.000(3)
C39 0.023(3) 0.037(4) 0.028(3) -0.006(3) 0.004(3) 0.002(3)
C40 0.018(3) 0.040(4) 0.033(3) 0.002(3) 0.006(3) -0.009(3)
C41 0.028(3) 0.036(3) 0.031(3) 0.005(3) -0.001(3) -0.009(3)
C42 0.022(3) 0.035(3) 0.026(3) -0.001(3) 0.000(3) 0.002(3)
C43 0.026(3) 0.025(3) 0.018(3) 0.001(3) 0.001(2) -0.006(2)
C44 0.028(3) 0.033(3) 0.023(3) 0.003(3) 0.004(3) -0.003(3)
C45 0.025(3) 0.051(4) 0.026(3) 0.002(3) 0.003(3) -0.002(3)
C46 0.034(3) 0.045(4) 0.030(3) 0.002(3) 0.004(3) 0.016(3)
C47 0.035(3) 0.030(3) 0.029(3) -0.003(3) 0.006(3) 0.000(3)
C48 0.027(3) 0.028(3) 0.030(3) 0.004(3) 0.002(3) 0.001(3)
C49 0.031(3) 0.023(3) 0.021(3) 0.003(3) 0.000(3) 0.006(2)
C50 0.020(3) 0.027(3) 0.028(3) -0.001(3) 0.003(3) 0.000(2)
C51 0.024(3) 0.035(4) 0.032(3) -0.003(3) -0.001(3) -0.001(3)
C52 0.033(3) 0.033(3) 0.026(3) 0.009(3) 0.000(3) 0.012(3)
C53 0.029(3) 0.030(3) 0.030(3) 0.010(3) 0.004(3) -0.003(3)
C54 0.020(3) 0.031(3) 0.035(3) -0.003(3) 0.000(3) -0.001(2)
C55 0.022(3) 0.033(3) 0.030(3) -0.004(3) 0.005(3) -0.007(3)
C56 0.028(3) 0.034(4) 0.036(4) -0.002(3) 0.003(3) -0.005(3)
C57 0.027(3) 0.028(3) 0.048(4) -0.011(4) 0.013(3) -0.003(3)
C58 0.034(3) 0.040(4) 0.036(4) -0.018(4) 0.014(3) -0.017(3)
C59 0.035(4) 0.051(4) 0.026(3) -0.004(4) 0.008(3) -0.016(3)
C60 0.028(3) 0.034(3) 0.031(3) 0.001(3) 0.009(3) -0.003(3)
B1 0.027(3) 0.022(3) 0.025(3) 0.001(3) -0.004(3) -0.003(3)
Cl1 0.093(2) 0.0776(18) 0.189(4) -0.019(2) 0.024(2) 0.0149(16)
Cl2 0.180(3) 0.123(3) 0.091(2) -0.037(2) -0.025(2) -0.039(3)
C61 0.141(5) 0.119(5) 0.158(5) 0.000(5) -0.014(5) -0.012(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
Yb1 N1 2.152(4) . ?
Yb1 N2 2.144(5) . ?
Yb1 C1 2.862(6) . ?
Yb1 C2 2.808(6) . ?
Yb1 C10 2.871(6) . ?
Yb1 C11 3.089(7) . ?
Yb1 C19 2.698(6) . ?
Yb1 C20 2.755(7) . ?
Si1 N1 1.737(5) . ?
Si1 C1 1.933(6) . ?
Si1 C4 1.883(7) . ?
Si1 C7 1.891(7) . ?
Si2 N1 1.734(5) . ?
Si2 C10 1.928(6) . ?
Si2 C13 1.886(7) . ?
Si2 C16 1.888(7) . ?
Si3 N2 1.761(5) . ?
Si3 C19 1.936(7) . ?
Si3 C22 1.900(7) . ?
Si3 C25 1.905(6) . ?
Si4 N2 1.764(5) . ?
Si4 C28 1.905(7) . ?
Si4 C31 1.908(7) . ?
Si4 C34 1.900(7) . ?
C1 H1 1.0000 . ?
C1 C2 1.549(9) . ?
C1 C3 1.547(8) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4 1.0000 . ?
C4 C5 1.544(8) . ?
C4 C6 1.556(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7 1.0000 . ?
C7 C8 1.529(10) . ?
C7 C9 1.539(9) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.553(9) . ?
C10 C12 1.534(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13 1.0000 . ?
C13 C14 1.546(8) . ?
C13 C15 1.533(9) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16 1.0000 . ?
C16 C17 1.539(9) . ?
C16 C18 1.539(8) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19 1.0000 . ?
C19 C20 1.563(8) . ?
C19 C21 1.557(8) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22 1.0000 . ?
C22 C23 1.532(9) . ?
C22 C24 1.529(9) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25 1.0000 . ?
C25 C26 1.519(9) . ?
C25 C27 1.541(9) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28 1.0000 . ?
C28 C29 1.545(10) . ?
C28 C30 1.530(9) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31 1.0000 . ?
C31 C32 1.511(9) . ?
C31 C33 1.564(9) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34 1.0000 . ?
C34 C35 1.545(10) . ?
C34 C36 1.548(10) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
F1 C38 1.347(7) . ?
F2 C39 1.353(7) . ?
F3 C40 1.336(6) . ?
F4 C41 1.341(7) . ?
F5 C42 1.362(6) . ?
F6 C44 1.345(7) . ?
F7 C45 1.355(7) . ?
F8 C46 1.341(7) . ?
F9 C47 1.351(7) . ?
F10 C48 1.362(7) . ?
F11 C50 1.355(7) . ?
F12 C51 1.350(7) . ?
F13 C52 1.346(7) . ?
F14 C53 1.335(7) . ?
F15 C54 1.359(7) . ?
F16 C56 1.351(7) . ?
F17 C57 1.331(7) . ?
F18 C58 1.360(7) . ?
F19 C59 1.350(8) . ?
F20 C60 1.357(7) . ?
C37 C38 1.391(8) . ?
C37 C42 1.376(8) . ?
C37 B1 1.653(9) . ?
C38 C39 1.379(8) . ?
C39 C40 1.358(9) . ?
C40 C41 1.377(9) . ?
C41 C42 1.385(8) . ?
C43 C44 1.400(8) . ?
C43 C48 1.386(8) . ?
C43 B1 1.667(9) . ?
C44 C45 1.395(9) . ?
C45 C46 1.352(9) . ?
C46 C47 1.368(9) . ?
C47 C48 1.374(8) . ?
C49 C50 1.386(8) . ?
C49 C54 1.400(8) . ?
C49 B1 1.644(9) . ?
C50 C51 1.373(9) . ?
C51 C52 1.376(9) . ?
C52 C53 1.371(9) . ?
C53 C54 1.385(9) . ?
C55 C56 1.392(9) . ?
C55 C60 1.383(9) . ?
C55 B1 1.662(9) . ?
C56 C57 1.392(9) . ?
C57 C58 1.362(10) . ?
C58 C59 1.368(10) . ?
C59 C60 1.374(9) . ?
Cl1 C61 1.732(12) . ?
Cl2 C61 1.728(11) . ?
C61 H61A 0.9900 . ?
C61 H61B 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
N1 Yb1 C1 67.83(18) . . ?
N1 Yb1 C2 87.51(18) . . ?
N1 Yb1 C10 66.96(17) . . ?
N1 Yb1 C11 76.94(17) . . ?
N1 Yb1 C19 151.0(2) . . ?
N1 Yb1 C20 139.4(2) . . ?
N2 Yb1 N1 127.67(19) . . ?
N2 Yb1 C1 128.53(19) . . ?
N2 Yb1 C2 96.89(19) . . ?
N2 Yb1 C10 104.41(18) . . ?
N2 Yb1 C11 121.96(18) . . ?
N2 Yb1 C19 72.7(2) . . ?
N2 Yb1 C20 92.8(2) . . ?
C1 Yb1 C10 124.48(18) . . ?
C1 Yb1 C11 109.05(18) . . ?
C2 Yb1 C1 31.69(17) . . ?
C2 Yb1 C10 153.43(18) . . ?
C2 Yb1 C11 139.87(18) . . ?
C10 Yb1 C11 29.92(17) . . ?
C19 Yb1 C1 118.68(18) . . ?
C19 Yb1 C2 112.39(19) . . ?
C19 Yb1 C10 89.31(18) . . ?
C19 Yb1 C11 74.31(18) . . ?
C19 Yb1 C20 33.30(18) . . ?
C20 Yb1 C1 85.37(18) . . ?
C20 Yb1 C2 84.15(19) . . ?
C20 Yb1 C10 110.1(2) . . ?
C20 Yb1 C11 84.31(19) . . ?
N1 Si1 C1 102.2(2) . . ?
N1 Si1 C4 113.5(3) . . ?
N1 Si1 C7 116.9(3) . . ?
C4 Si1 C1 107.0(3) . . ?
C4 Si1 C7 107.0(3) . . ?
C7 Si1 C1 109.8(3) . . ?
N1 Si2 C10 101.3(2) . . ?
N1 Si2 C13 114.1(3) . . ?
N1 Si2 C16 111.9(3) . . ?
C13 Si2 C10 109.6(3) . . ?
C13 Si2 C16 113.8(3) . . ?
C16 Si2 C10 105.1(3) . . ?
N2 Si3 C19 103.5(2) . . ?
N2 Si3 C22 113.6(3) . . ?
N2 Si3 C25 111.2(3) . . ?
C22 Si3 C19 108.6(3) . . ?
C22 Si3 C25 111.5(3) . . ?
C25 Si3 C19 108.0(3) . . ?
N2 Si4 C28 104.7(3) . . ?
N2 Si4 C31 109.6(3) . . ?
N2 Si4 C34 114.5(3) . . ?
C28 Si4 C31 105.2(3) . . ?
C34 Si4 C28 108.1(3) . . ?
C34 Si4 C31 113.9(3) . . ?
Si1 N1 Yb1 109.3(2) . . ?
Si2 N1 Yb1 109.1(2) . . ?
Si2 N1 Si1 136.6(3) . . ?
Si3 N2 Yb1 102.9(2) . . ?
Si3 N2 Si4 126.5(3) . . ?
Si4 N2 Yb1 130.6(3) . . ?
Yb1 C1 H1 60.6 . . ?
Si1 C1 Yb1 80.6(2) . . ?
Si1 C1 H1 106.4 . . ?
C2 C1 Yb1 72.2(3) . . ?
C2 C1 Si1 118.1(5) . . ?
C2 C1 H1 106.4 . . ?
C3 C1 Yb1 164.1(4) . . ?
C3 C1 Si1 113.3(4) . . ?
C3 C1 H1 106.4 . . ?
C3 C1 C2 105.5(5) . . ?
Yb1 C2 H2A 42.1 . . ?
Yb1 C2 H2B 98.2 . . ?
Yb1 C2 H2C 147.1 . . ?
C1 C2 Yb1 76.1(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4 105.7 . . ?
C5 C4 Si1 113.2(4) . . ?
C5 C4 H4 105.7 . . ?
C5 C4 C6 108.9(5) . . ?
C6 C4 Si1 116.8(4) . . ?
C6 C4 H4 105.7 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7 105.5 . . ?
C8 C7 Si1 117.1(5) . . ?
C8 C7 H7 105.5 . . ?
C8 C7 C9 109.5(6) . . ?
C9 C7 Si1 112.7(5) . . ?
C9 C7 H7 105.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Yb1 C10 H10 44.5 . . ?
Si2 C10 Yb1 80.2(2) . . ?
Si2 C10 H10 105.8 . . ?
C11 C10 Yb1 82.8(3) . . ?
C11 C10 Si2 112.1(4) . . ?
C11 C10 H10 105.8 . . ?
C12 C10 Yb1 150.2(5) . . ?
C12 C10 Si2 117.5(4) . . ?
C12 C10 H10 105.8 . . ?
C12 C10 C11 109.0(5) . . ?
Yb1 C11 H11A 46.2 . . ?
Yb1 C11 H11B 107.0 . . ?
Yb1 C11 H11C 141.8 . . ?
C10 C11 Yb1 67.3(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si2 C13 H13 105.9 . . ?
C14 C13 Si2 111.4(5) . . ?
C14 C13 H13 105.9 . . ?
C15 C13 Si2 117.1(5) . . ?
C15 C13 H13 105.9 . . ?
C15 C13 C14 109.9(5) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si2 C16 H16 105.3 . . ?
C17 C16 Si2 114.4(5) . . ?
C17 C16 H16 105.3 . . ?
C18 C16 Si2 116.4(5) . . ?
C18 C16 H16 105.3 . . ?
C18 C16 C17 109.0(5) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Yb1 C19 H19 55.5 . . ?
Si3 C19 Yb1 80.9(2) . . ?
Si3 C19 H19 105.6 . . ?
C20 C19 Yb1 75.3(3) . . ?
C20 C19 Si3 118.5(5) . . ?
C20 C19 H19 105.6 . . ?
C21 C19 Yb1 159.5(5) . . ?
C21 C19 Si3 114.7(5) . . ?
C21 C19 H19 105.6 . . ?
C21 C19 C20 105.8(5) . . ?
Yb1 C20 H20A 49.0 . . ?
Yb1 C20 H20B 153.0 . . ?
Yb1 C20 H20C 94.8 . . ?
C19 C20 Yb1 71.4(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si3 C22 H22 106.2 . . ?
C23 C22 Si3 113.0(5) . . ?
C23 C22 H22 106.2 . . ?
C24 C22 Si3 114.9(5) . . ?
C24 C22 H22 106.2 . . ?
C24 C22 C23 109.8(6) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si3 C25 H25 104.7 . . ?
C26 C25 Si3 117.7(5) . . ?
C26 C25 H25 104.7 . . ?
C26 C25 C27 109.3(6) . . ?
C27 C25 Si3 114.4(5) . . ?
C27 C25 H25 104.7 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si4 C28 H28 104.5 . . ?
C29 C28 Si4 113.0(5) . . ?
C29 C28 H28 104.5 . . ?
C30 C28 Si4 118.7(5) . . ?
C30 C28 H28 104.5 . . ?
C30 C28 C29 110.0(6) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si4 C31 H31 105.2 . . ?
C32 C31 Si4 116.8(5) . . ?
C32 C31 H31 105.2 . . ?
C32 C31 C33 108.2(6) . . ?
C33 C31 Si4 115.1(5) . . ?
C33 C31 H31 105.2 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Si4 C34 H34 106.0 . . ?
C35 C34 Si4 116.8(5) . . ?
C35 C34 H34 106.0 . . ?
C35 C34 C36 107.5(7) . . ?
C36 C34 Si4 113.6(5) . . ?
C36 C34 H34 106.0 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 B1 119.2(5) . . ?
C42 C37 C38 113.3(5) . . ?
C42 C37 B1 127.4(5) . . ?
F1 C38 C37 119.1(5) . . ?
F1 C38 C39 116.9(5) . . ?
C39 C38 C37 124.0(6) . . ?
F2 C39 C38 120.0(6) . . ?
F2 C39 C40 119.8(5) . . ?
C40 C39 C38 120.2(6) . . ?
F3 C40 C39 121.9(5) . . ?
F3 C40 C41 119.5(6) . . ?
C39 C40 C41 118.6(5) . . ?
F4 C41 C40 119.7(5) . . ?
F4 C41 C42 120.8(6) . . ?
C40 C41 C42 119.5(6) . . ?
F5 C42 C37 121.5(5) . . ?
F5 C42 C41 114.2(5) . . ?
C37 C42 C41 124.3(6) . . ?
C44 C43 B1 126.5(5) . . ?
C48 C43 C44 113.3(5) . . ?
C48 C43 B1 119.6(5) . . ?
F6 C44 C43 121.0(5) . . ?
F6 C44 C45 116.3(5) . . ?
C45 C44 C43 122.7(6) . . ?
F7 C45 C44 118.7(6) . . ?
C46 C45 F7 120.4(6) . . ?
C46 C45 C44 120.9(6) . . ?
F8 C46 C45 120.2(6) . . ?
F8 C46 C47 121.2(6) . . ?
C45 C46 C47 118.6(6) . . ?
F9 C47 C46 120.0(6) . . ?
F9 C47 C48 119.9(5) . . ?
C46 C47 C48 120.1(6) . . ?
F10 C48 C43 119.4(5) . . ?
F10 C48 C47 116.2(6) . . ?
C47 C48 C43 124.4(6) . . ?
C50 C49 C54 112.8(6) . . ?
C50 C49 B1 127.8(5) . . ?
C54 C49 B1 119.2(5) . . ?
F11 C50 C49 121.0(6) . . ?
F11 C50 C51 114.7(5) . . ?
C51 C50 C49 124.3(6) . . ?
F12 C51 C50 120.7(6) . . ?
F12 C51 C52 119.2(6) . . ?
C50 C51 C52 120.1(6) . . ?
F13 C52 C51 121.3(6) . . ?
F13 C52 C53 119.5(6) . . ?
C53 C52 C51 119.2(6) . . ?
F14 C53 C52 120.3(6) . . ?
F14 C53 C54 121.1(6) . . ?
C52 C53 C54 118.6(6) . . ?
F15 C54 C49 118.9(6) . . ?
F15 C54 C53 116.1(5) . . ?
C53 C54 C49 125.0(6) . . ?
C56 C55 B1 126.3(6) . . ?
C60 C55 C56 113.6(6) . . ?
C60 C55 B1 120.0(6) . . ?
F16 C56 C55 120.9(6) . . ?
F16 C56 C57 115.3(6) . . ?
C55 C56 C57 123.8(7) . . ?
F17 C57 C56 120.1(7) . . ?
F17 C57 C58 121.1(6) . . ?
C58 C57 C56 118.8(6) . . ?
F18 C58 C57 120.1(7) . . ?
F18 C58 C59 119.6(7) . . ?
C57 C58 C59 120.2(6) . . ?
F19 C59 C58 120.5(7) . . ?
F19 C59 C60 120.5(7) . . ?
C58 C59 C60 119.0(7) . . ?
F20 C60 C55 119.4(6) . . ?
F20 C60 C59 116.0(6) . . ?
C59 C60 C55 124.6(7) . . ?
C37 B1 C43 114.0(5) . . ?
C37 B1 C55 102.1(5) . . ?
C49 B1 C37 113.6(5) . . ?
C49 B1 C43 100.6(5) . . ?
C49 B1 C55 114.5(5) . . ?
C55 B1 C43 112.6(5) . . ?
Cl1 C61 H61A 108.9 . . ?
Cl1 C61 H61B 108.9 . . ?
Cl2 C61 Cl1 113.4(7) . . ?
Cl2 C61 H61A 108.9 . . ?
Cl2 C61 H61B 108.9 . . ?
H61A C61 H61B 107.7 . . ?
_shelx_res_file
;
TITL xdpm75.res in P2(1)/n
xdpm75.res
created by SHELXL-2017/1 at 12:46:19 on 24-Aug-2017
CELL 1.54184 16.062029 25.926177 16.746444 90 92.7492 90
ZERR 4 0.000328 0.000562 0.000327 0 0.0021 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H B Cl F N Si Yb
UNIT 244 344 4 8 80 8 16 4
DFIX 1.753 Cl2 C61 Cl1 C61
DELU C61 Cl1 Cl2 H61a H61b
SIMU 0.01 0.01 2 C61 Cl1 Cl2 H61a H61b
L.S. 4
PLAN 20
SIZE 0.3 0.1 0.1
TEMP -123.1(2)
CONN 20 Yb1
FREE Yb1 Si2
FREE Yb1 Si1
FREE Yb1 Si4
FREE Yb1 Si3
BOND $H
list 4
fmap 2
acta
SHEL 100 0.83
OMIT 0 3 4
REM
REM
REM
WGHT 0.052000
FVAR 0.41341
YB1 8 0.336400 0.352357 0.715532 11.00000 0.02729 0.02361 =
0.02657 0.00198 0.00751 0.00425
SI1 7 0.476625 0.315286 0.600500 11.00000 0.02614 0.02471 =
0.02904 0.00283 0.00672 0.00326
SI2 7 0.361245 0.232419 0.686889 11.00000 0.02838 0.02160 =
0.03003 0.00186 0.00272 0.00384
SI3 7 0.233681 0.409680 0.836823 11.00000 0.03279 0.02402 =
0.03252 0.00050 0.01460 0.00267
SI4 7 0.399561 0.367331 0.920542 11.00000 0.03753 0.03178 =
0.02672 0.00078 0.00169 0.00058
N1 6 0.410335 0.290709 0.670135 11.00000 0.02549 0.01819 =
0.03290 -0.00581 0.00912 0.00347
N2 6 0.329937 0.377142 0.837231 11.00000 0.03278 0.02329 =
0.01951 0.00443 0.00872 0.00162
C1 1 0.445999 0.387385 0.597114 11.00000 0.02964 0.02951 =
0.03473 0.00175 0.00682 0.00191
AFIX 13
H1 2 0.384379 0.388513 0.585463 11.00000 -1.20000
AFIX 0
C2 1 0.463344 0.420158 0.673424 11.00000 0.03407 0.03171 =
0.03957 -0.00221 0.01099 -0.00217
AFIX 137
H2A 2 0.448072 0.400384 0.720401 11.00000 -1.50000
H2B 2 0.430224 0.451889 0.669764 11.00000 -1.50000
H2C 2 0.522710 0.428939 0.678395 11.00000 -1.50000
AFIX 0
C3 1 0.485872 0.417503 0.528940 11.00000 0.03518 0.03226 =
0.03854 0.00655 0.01314 0.00035
AFIX 137
H3A 2 0.546727 0.415526 0.535771 11.00000 -1.50000
H3B 2 0.468330 0.453678 0.530523 11.00000 -1.50000
H3C 2 0.467817 0.402384 0.477340 11.00000 -1.50000
AFIX 0
C4 1 0.455771 0.288818 0.496736 11.00000 0.03104 0.02728 =
0.03051 -0.00137 0.00173 0.00508
AFIX 13
H4 2 0.454869 0.250458 0.502869 11.00000 -1.20000
AFIX 0
C5 1 0.368988 0.303602 0.460108 11.00000 0.04387 0.04104 =
0.02752 0.00112 0.00525 0.00177
AFIX 137
H5A 2 0.326375 0.295354 0.498084 11.00000 -1.50000
H5B 2 0.357878 0.284190 0.410524 11.00000 -1.50000
H5C 2 0.367630 0.340645 0.448468 11.00000 -1.50000
AFIX 0
C6 1 0.522380 0.300159 0.434564 11.00000 0.04248 0.04517 =
0.02897 0.00190 0.01232 0.00620
AFIX 137
H6A 2 0.526897 0.337500 0.426776 11.00000 -1.50000
H6B 2 0.505774 0.283688 0.383588 11.00000 -1.50000
H6C 2 0.576412 0.286431 0.454177 11.00000 -1.50000
AFIX 0
C7 1 0.592375 0.308722 0.624517 11.00000 0.02983 0.03807 =
0.03931 0.00597 0.01066 -0.00077
AFIX 13
H7 2 0.619989 0.329222 0.582676 11.00000 -1.20000
AFIX 0
C8 1 0.626012 0.330508 0.704517 11.00000 0.02881 0.05878 =
0.06117 -0.00178 -0.00080 0.00176
AFIX 137
H8A 2 0.613365 0.367435 0.707029 11.00000 -1.50000
H8B 2 0.686504 0.325466 0.709546 11.00000 -1.50000
H8C 2 0.599733 0.312593 0.748269 11.00000 -1.50000
AFIX 0
C9 1 0.623706 0.253076 0.615030 11.00000 0.03236 0.04642 =
0.04733 0.00253 0.00827 0.01241
AFIX 137
H9A 2 0.598728 0.230900 0.654788 11.00000 -1.50000
H9B 2 0.684535 0.252326 0.623039 11.00000 -1.50000
H9C 2 0.607810 0.240559 0.561222 11.00000 -1.50000
AFIX 0
C10 1 0.250678 0.255168 0.709984 11.00000 0.03134 0.02589 =
0.03740 0.00313 0.00875 0.00286
AFIX 13
H10 2 0.258516 0.283593 0.750003 11.00000 -1.20000
AFIX 0
C11 1 0.204412 0.279803 0.635915 11.00000 0.02845 0.03510 =
0.04016 0.00240 0.00273 0.00274
AFIX 137
H11A 2 0.237240 0.308714 0.616639 11.00000 -1.50000
H11B 2 0.149728 0.292334 0.650824 11.00000 -1.50000
H11C 2 0.197063 0.253911 0.593526 11.00000 -1.50000
AFIX 0
C12 1 0.192765 0.215930 0.747661 11.00000 0.03221 0.03906 =
0.04743 0.00445 0.01350 -0.00408
AFIX 137
H12A 2 0.218870 0.203243 0.797988 11.00000 -1.50000
H12B 2 0.182842 0.186945 0.710865 11.00000 -1.50000
H12C 2 0.139595 0.232543 0.758194 11.00000 -1.50000
AFIX 0
C13 1 0.355460 0.188124 0.597471 11.00000 0.03801 0.02639 =
0.04160 -0.00516 0.00181 0.00045
AFIX 13
H13 2 0.350144 0.211111 0.549545 11.00000 -1.20000
AFIX 0
C14 1 0.437709 0.157985 0.589624 11.00000 0.04077 0.03328 =
0.06166 -0.00471 0.00885 0.00698
AFIX 137
H14A 2 0.484698 0.182137 0.591947 11.00000 -1.50000
H14B 2 0.436100 0.139605 0.538437 11.00000 -1.50000
H14C 2 0.444470 0.133107 0.633515 11.00000 -1.50000
AFIX 0
C15 1 0.281255 0.150983 0.590076 11.00000 0.05734 0.03127 =
0.05108 -0.01030 0.00313 -0.00342
AFIX 137
H15A 2 0.278460 0.130854 0.639408 11.00000 -1.50000
H15B 2 0.288244 0.127616 0.544888 11.00000 -1.50000
H15C 2 0.229612 0.170729 0.581203 11.00000 -1.50000
AFIX 0
C16 1 0.403153 0.200425 0.781804 11.00000 0.03384 0.02580 =
0.03342 0.00775 0.00183 0.00182
AFIX 13
H16 2 0.379191 0.220455 0.826278 11.00000 -1.20000
AFIX 0
C17 1 0.498323 0.204360 0.796115 11.00000 0.04659 0.04622 =
0.05642 0.01033 -0.00783 0.00302
AFIX 137
H17A 2 0.525656 0.180711 0.759978 11.00000 -1.50000
H17B 2 0.513616 0.195106 0.851633 11.00000 -1.50000
H17C 2 0.516288 0.239770 0.785845 11.00000 -1.50000
AFIX 0
C18 1 0.376172 0.144230 0.794901 11.00000 0.05346 0.02967 =
0.05088 0.01363 -0.00004 0.00296
AFIX 137
H18A 2 0.390138 0.134190 0.850352 11.00000 -1.50000
H18B 2 0.405317 0.121563 0.758646 11.00000 -1.50000
H18C 2 0.315879 0.141148 0.784046 11.00000 -1.50000
AFIX 0
C19 1 0.188847 0.400638 0.728365 11.00000 0.02511 0.02648 =
0.04318 0.00558 0.00937 0.00475
AFIX 13
H19 2 0.195227 0.363097 0.716388 11.00000 -1.20000
AFIX 0
C20 1 0.231560 0.429735 0.659543 11.00000 0.04407 0.03344 =
0.04406 0.01079 0.01265 0.00452
AFIX 137
H20A 2 0.292164 0.429156 0.669599 11.00000 -1.50000
H20B 2 0.212090 0.465554 0.657429 11.00000 -1.50000
H20C 2 0.217203 0.412735 0.608457 11.00000 -1.50000
AFIX 0
C21 1 0.093980 0.412137 0.716084 11.00000 0.03477 0.04323 =
0.05340 0.01233 0.00886 0.01165
AFIX 137
H21A 2 0.073744 0.399214 0.663690 11.00000 -1.50000
H21B 2 0.084685 0.449444 0.718737 11.00000 -1.50000
H21C 2 0.063783 0.394995 0.758092 11.00000 -1.50000
AFIX 0
C22 1 0.243960 0.481459 0.858036 11.00000 0.05231 0.02452 =
0.03944 0.00247 0.01597 0.00432
AFIX 13
H22 2 0.248789 0.485015 0.917538 11.00000 -1.20000
AFIX 0
C23 1 0.166448 0.512216 0.830175 11.00000 0.04724 0.03031 =
0.07755 -0.00357 0.02539 0.00751
AFIX 137
H23A 2 0.167776 0.518716 0.772602 11.00000 -1.50000
H23B 2 0.165694 0.545156 0.858835 11.00000 -1.50000
H23C 2 0.116298 0.492447 0.841270 11.00000 -1.50000
AFIX 0
C24 1 0.321894 0.506753 0.826542 11.00000 0.04738 0.02968 =
0.07517 0.00384 0.01753 -0.00391
AFIX 137
H24A 2 0.318507 0.506324 0.767961 11.00000 -1.50000
H24B 2 0.371439 0.487654 0.846061 11.00000 -1.50000
H24C 2 0.325678 0.542493 0.845423 11.00000 -1.50000
AFIX 0
C25 1 0.159597 0.377413 0.906924 11.00000 0.04464 0.03501 =
0.04163 0.00896 0.02373 0.00130
AFIX 13
H25 2 0.195946 0.366266 0.953932 11.00000 -1.20000
AFIX 0
C26 1 0.092826 0.410736 0.942305 11.00000 0.06864 0.03846 =
0.07817 0.00226 0.05124 0.00227
AFIX 137
H26A 2 0.067507 0.391977 0.985781 11.00000 -1.50000
H26B 2 0.049881 0.419007 0.900733 11.00000 -1.50000
H26C 2 0.118024 0.442717 0.963222 11.00000 -1.50000
AFIX 0
C27 1 0.119736 0.327189 0.874081 11.00000 0.04413 0.03815 =
0.04754 0.01065 0.01418 -0.00128
AFIX 137
H27A 2 0.162854 0.305354 0.852077 11.00000 -1.50000
H27B 2 0.077475 0.335492 0.831885 11.00000 -1.50000
H27C 2 0.093525 0.308778 0.917390 11.00000 -1.50000
AFIX 0
C28 1 0.507562 0.372461 0.878851 11.00000 0.03329 0.04441 =
0.03934 -0.00383 -0.00111 0.00208
AFIX 13
H28 2 0.501041 0.357095 0.824138 11.00000 -1.20000
AFIX 0
C29 1 0.534649 0.428741 0.864407 11.00000 0.04011 0.06725 =
0.04334 -0.00331 0.00166 -0.01540
AFIX 137
H29A 2 0.555006 0.444119 0.915116 11.00000 -1.50000
H29B 2 0.486908 0.448588 0.842499 11.00000 -1.50000
H29C 2 0.579215 0.429214 0.826443 11.00000 -1.50000
AFIX 0
C30 1 0.579357 0.342229 0.919852 11.00000 0.04101 0.05721 =
0.05626 0.00985 -0.01401 0.00802
AFIX 137
H30A 2 0.628575 0.344455 0.887628 11.00000 -1.50000
H30B 2 0.563058 0.306017 0.925251 11.00000 -1.50000
H30C 2 0.592438 0.356845 0.972947 11.00000 -1.50000
AFIX 0
C31 1 0.391180 0.297844 0.956749 11.00000 0.05071 0.04306 =
0.02970 0.00142 0.00389 0.00007
AFIX 13
H31 2 0.422082 0.276848 0.917764 11.00000 -1.20000
AFIX 0
C32 1 0.304838 0.274696 0.955895 11.00000 0.06358 0.03387 =
0.04686 0.01420 0.01468 -0.00217
AFIX 137
H32A 2 0.309065 0.237465 0.965361 11.00000 -1.50000
H32B 2 0.276245 0.280967 0.903787 11.00000 -1.50000
H32C 2 0.273188 0.290636 0.997984 11.00000 -1.50000
AFIX 0
C33 1 0.435493 0.286532 1.040105 11.00000 0.07928 0.04864 =
0.03716 0.00113 -0.00288 0.00601
AFIX 137
H33A 2 0.491612 0.301453 1.041996 11.00000 -1.50000
H33B 2 0.439382 0.249165 1.048282 11.00000 -1.50000
H33C 2 0.403252 0.301891 1.082270 11.00000 -1.50000
AFIX 0
C34 1 0.391816 0.417249 1.002896 11.00000 0.05612 0.04468 =
0.03393 0.00025 0.00274 -0.00242
AFIX 13
H34 2 0.388681 0.451525 0.975532 11.00000 -1.20000
AFIX 0
C35 1 0.314553 0.414192 1.054216 11.00000 0.08281 0.04725 =
0.04578 -0.00786 0.00904 0.01010
AFIX 137
H35A 2 0.264379 0.422235 1.020940 11.00000 -1.50000
H35B 2 0.320395 0.439092 1.098157 11.00000 -1.50000
H35C 2 0.309880 0.379312 1.076102 11.00000 -1.50000
AFIX 0
C36 1 0.469839 0.419407 1.060794 11.00000 0.07279 0.05759 =
0.04120 -0.01332 -0.00722 -0.00758
AFIX 137
H36A 2 0.519226 0.426582 1.030470 11.00000 -1.50000
H36B 2 0.476801 0.386213 1.088303 11.00000 -1.50000
H36C 2 0.462875 0.446792 1.100257 11.00000 -1.50000
AFIX 0
F1 5 0.042875 0.512816 0.364776 11.00000 0.03109 0.03083 =
0.04389 -0.00178 0.00066 0.00355
F2 5 -0.082846 0.470517 0.440151 11.00000 0.02696 0.04794 =
0.05008 -0.00878 0.00802 0.00433
F3 5 -0.060490 0.378351 0.517898 11.00000 0.03136 0.05845 =
0.05559 0.01248 0.01363 -0.00861
F4 5 0.087181 0.329139 0.512351 11.00000 0.03529 0.05095 =
0.05120 0.02275 0.00523 -0.00455
F5 5 0.211471 0.368491 0.435665 11.00000 0.02557 0.04060 =
0.04774 0.01390 0.00537 0.00415
F6 5 0.395732 0.490506 0.367072 11.00000 0.02644 0.03947 =
0.03770 -0.00676 0.00120 -0.00713
F7 5 0.513275 0.430566 0.312651 11.00000 0.02076 0.07007 =
0.04837 -0.00029 0.00480 0.00272
F8 5 0.474648 0.340484 0.237316 11.00000 0.04280 0.06385 =
0.03967 -0.00552 0.00886 0.02070
F9 5 0.310944 0.312099 0.215979 11.00000 0.05229 0.03944 =
0.04611 -0.01408 0.00445 0.00656
F10 5 0.190732 0.372212 0.266182 11.00000 0.03051 0.03340 =
0.04426 -0.00855 0.00124 -0.00399
F11 5 0.049960 0.440884 0.238255 11.00000 0.02995 0.04060 =
0.03590 -0.00095 0.00169 -0.01216
F12 5 0.016743 0.471708 0.090573 11.00000 0.02838 0.05041 =
0.03128 -0.00135 -0.00404 -0.00379
F13 5 0.119373 0.539423 0.017729 11.00000 0.04067 0.05116 =
0.03109 0.00841 -0.00361 -0.00086
F14 5 0.260127 0.572446 0.097151 11.00000 0.04018 0.04887 =
0.03447 0.01356 -0.00454 -0.01124
F15 5 0.296921 0.541899 0.247223 11.00000 0.02870 0.03843 =
0.03158 0.00546 -0.00237 -0.01171
F16 5 0.170847 0.588211 0.329392 11.00000 0.04056 0.03181 =
0.03909 -0.00168 -0.00064 0.00420
F17 5 0.215096 0.658317 0.437431 11.00000 0.03649 0.02919 =
0.06392 -0.01092 0.01260 -0.00375
F18 5 0.296698 0.631203 0.578080 11.00000 0.04890 0.05593 =
0.04936 -0.02565 0.01227 -0.01980
F19 5 0.336456 0.530228 0.604482 11.00000 0.05093 0.06629 =
0.02668 -0.00285 -0.00359 -0.01674
F20 5 0.296219 0.458992 0.495493 11.00000 0.03198 0.03755 =
0.02730 0.00336 0.00037 -0.00146
C37 1 0.132667 0.442327 0.392206 11.00000 0.02435 0.02837 =
0.02274 -0.00322 0.00046 -0.00481
C38 1 0.055810 0.466250 0.398804 11.00000 0.02801 0.02549 =
0.02998 -0.00031 0.00002 0.00004
C39 1 -0.008881 0.445600 0.439651 11.00000 0.02343 0.03681 =
0.02833 -0.00607 0.00412 0.00215
C40 1 0.001076 0.399897 0.478587 11.00000 0.01817 0.04036 =
0.03283 0.00235 0.00603 -0.00912
C41 1 0.076278 0.374672 0.475357 11.00000 0.02831 0.03642 =
0.03118 0.00502 -0.00063 -0.00926
C42 1 0.139619 0.396497 0.433417 11.00000 0.02187 0.03515 =
0.02558 -0.00083 0.00049 0.00171
C43 1 0.285647 0.434091 0.321816 11.00000 0.02563 0.02509 =
0.01807 0.00118 0.00080 -0.00623
C44 1 0.370379 0.446660 0.330523 11.00000 0.02796 0.03350 =
0.02319 0.00271 0.00418 -0.00318
C45 1 0.432842 0.415351 0.301690 11.00000 0.02532 0.05138 =
0.02614 0.00172 0.00280 -0.00189
C46 1 0.413922 0.370265 0.264534 11.00000 0.03403 0.04501 =
0.02958 0.00166 0.00410 0.01613
C47 1 0.331902 0.356633 0.253716 11.00000 0.03543 0.03023 =
0.02904 -0.00287 0.00579 0.00010
C48 1 0.270746 0.388000 0.281650 11.00000 0.02686 0.02780 =
0.02995 0.00413 0.00182 0.00058
C49 1 0.174427 0.490901 0.253043 11.00000 0.03129 0.02295 =
0.02089 0.00285 0.00033 0.00590
C50 1 0.104563 0.474711 0.208116 11.00000 0.02020 0.02748 =
0.02831 -0.00143 0.00313 -0.00010
C51 1 0.085535 0.489813 0.130774 11.00000 0.02448 0.03483 =
0.03196 -0.00321 -0.00104 -0.00075
C52 1 0.137177 0.523390 0.093082 11.00000 0.03265 0.03315 =
0.02617 0.00889 -0.00037 0.01179
C53 1 0.208503 0.540420 0.132920 11.00000 0.02948 0.03028 =
0.03043 0.00977 0.00369 -0.00298
C54 1 0.225327 0.523882 0.210667 11.00000 0.02014 0.03119 =
0.03506 -0.00350 -0.00032 -0.00103
C55 1 0.233696 0.519465 0.405437 11.00000 0.02204 0.03322 =
0.02975 -0.00403 0.00525 -0.00675
C56 1 0.214124 0.571431 0.395559 11.00000 0.02803 0.03443 =
0.03626 -0.00174 0.00297 -0.00517
C57 1 0.235307 0.609280 0.451859 11.00000 0.02674 0.02800 =
0.04830 -0.01135 0.01258 -0.00261
C58 1 0.276249 0.595115 0.521525 11.00000 0.03387 0.03951 =
0.03557 -0.01763 0.01394 -0.01662
C59 1 0.295746 0.544457 0.535612 11.00000 0.03528 0.05089 =
0.02598 -0.00368 0.00813 -0.01645
C60 1 0.274368 0.508416 0.478090 11.00000 0.02761 0.03421 =
0.03101 0.00050 0.00922 -0.00268
B1 3 0.205800 0.471894 0.343220 11.00000 0.02731 0.02214 =
0.02524 0.00090 -0.00424 -0.00261
CL1 4 -0.119008 0.332221 0.861102 11.00000 0.09300 0.07757 =
0.18856 -0.01852 0.02371 0.01490
CL2 4 -0.045099 0.290655 0.720793 11.00000 0.17962 0.12322 =
0.09101 -0.03745 -0.02475 -0.03943
C61 1 -0.135952 0.306855 0.766057 11.00000 0.14100 0.11899 =
0.15820 -0.00045 -0.01399 -0.01198
AFIX 23
H61A 2 -0.171242 0.275692 0.769352 11.00000 -1.20000
H61B 2 -0.166943 0.332411 0.732259 11.00000 -1.20000
AFIX 0
HKLF 4
REM xdpm75.res in P2(1)/n
REM R1 = 0.0560 for 8206 Fo > 4sig(Fo) and 0.1003 for all 12492 data
REM 844 parameters refined using 30 restraints
END
WGHT 0.0520 0.0000
REM Highest difference peak 0.791, deepest hole -0.780, 1-sigma level 0.108
Q1 1 -0.1097 0.2997 0.7347 11.00000 0.05 0.79
Q2 1 0.3424 0.3127 0.7231 11.00000 0.05 0.74
Q3 1 0.3985 0.3593 0.7002 11.00000 0.05 0.71
Q4 1 0.4650 0.3531 0.5935 11.00000 0.05 0.55
Q5 1 0.3176 0.3928 0.7192 11.00000 0.05 0.51
Q6 1 -0.2624 0.2682 0.8734 11.00000 0.05 0.49
Q7 1 0.5489 0.3187 0.6215 11.00000 0.05 0.46
Q8 1 0.3791 0.3165 0.8059 11.00000 0.05 0.46
Q9 1 0.4359 0.2907 0.8317 11.00000 0.05 0.45
Q10 1 0.3232 0.3306 0.8214 11.00000 0.05 0.45
Q11 1 0.2633 0.3564 0.7166 11.00000 0.05 0.44
Q12 1 -0.0276 0.2813 0.7367 11.00000 0.05 0.42
Q13 1 0.0043 0.4287 0.0629 11.00000 0.05 0.42
Q14 1 0.2212 0.3564 0.8396 11.00000 0.05 0.42
Q15 1 0.2288 0.4540 0.8364 11.00000 0.05 0.42
Q16 1 0.3363 0.3281 0.6042 11.00000 0.05 0.41
Q17 1 0.3559 0.3935 0.7303 11.00000 0.05 0.40
Q18 1 0.2921 0.3614 0.8184 11.00000 0.05 0.40
Q19 1 0.3870 0.3288 0.9192 11.00000 0.05 0.38
Q20 1 0.2846 0.4593 0.6632 11.00000 0.05 0.37
;
_shelx_res_checksum 66860
_olex2_date_sample_completion 2017-08-03
_olex2_date_sample_data_collection 2017-08-02
_olex2_date_sample_submission 2017-08-02
_olex2_exptl_crystal_mounting_method 'From fomblin on a microscope slide.'
_olex2_submission_original_sample_id XDPM75
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.840
_oxdiff_exptl_absorpt_empirical_full_min 0.641
#######################################################################
#
# 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_rdpm78
_database_code_depnum_ccdc_archive 'CCDC 1880943'
loop_
_audit_author_name
_audit_author_address
'Hannah Nicholas'
;The University of Manchester
United Kingdom
;
_audit_update_record
;
2018-11-23 deposited with the CCDC. 2019-09-18 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_rdpm78
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 19 Note
RESPONSE: Reduction of beam stop mask did not yield significant
improvement. Most of those missing strong reflections
appeared to be very strong and were treated as overflows.
;
# end Validation Reply Form
_audit_creation_date 2017-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic '[Tm(Ntt)2][BArF]'
_chemical_formula_moiety 'C36 H84 N2 Si4 Tm, C H2 Cl2, B C24 F20'
_chemical_formula_sum 'C61 H86 B Cl2 F20 N2 Si4 Tm'
_chemical_formula_weight 1590.31
_chemical_melting_point ?
_chemical_oxdiff_formula TmN2Si4C90F20B
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 16.3084(3)
_cell_length_b 16.8020(4)
_cell_length_c 25.4751(5)
_cell_angle_alpha 89.3578(18)
_cell_angle_beta 88.4783(16)
_cell_angle_gamma 88.0167(16)
_cell_volume 6973.5(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 30567
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 30.0500
_cell_measurement_theta_min 2.3530
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.510
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.300
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (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 'clear yellowish yellow'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier yellowish
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.515
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 3240
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-17 5 22 0.1804
2 23 -5 0.1829
-4 -23 7 0.1602
7 -22 -7 0.2080
8 -19 15 0.1393
8 3 34 0.1326
-8 19 -15 0.1578
-9 0 -33 0.1404
-16 -15 -13 0.1364
-22 -2 -12 0.1411
-19 13 -7 0.1643
21 6 13 0.1428
19 -11 8 0.1867
19 11 -12 0.2458
-14 -11 -25 0.0919
15 -15 15 0.1489
17 2 25 0.1314
-13 -15 18 0.1691
_exptl_crystal_preparation ?
_exptl_crystal_size_max 0.547
_exptl_crystal_size_mid 0.351
_exptl_crystal_size_min 0.275
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
-16.9643 4.9887 21.9328 -0.3269 0.8419 -0.4231
2.0029 22.9392 -5.0146 0.1227 -0.3313 -0.9159
-3.9986 -22.9389 7.0089 -0.1716 0.4203 0.8919
6.9793 -21.9428 -6.9533 0.0637 -0.1498 0.9906
7.9678 -18.9532 14.9910 0.3993 0.3469 0.8211
7.9651 2.9867 33.9191 0.7518 0.6506 -0.1330
-7.9678 18.9532 -14.9910 -0.3993 -0.3469 -0.8211
-8.9622 0.0055 -32.9256 -0.7616 -0.6281 -0.0026
-15.9567 -14.9551 -12.9590 -0.8385 0.1117 0.4984
-21.9383 -1.9881 -11.9800 -0.9862 0.1607 -0.0968
-18.9444 12.9710 -7.0084 -0.7364 0.1130 -0.6988
20.9415 5.9777 12.9723 0.9813 -0.1456 -0.0800
18.9445 -10.9764 8.0036 0.7590 -0.1032 0.6139
18.9589 10.9675 -11.9749 0.6087 -0.7545 -0.2421
-13.9556 -10.9650 -24.9341 -0.8990 -0.2515 0.3828
14.9507 -14.9655 14.9897 0.6803 0.1776 0.7230
16.9455 1.9881 24.9464 0.9670 0.2576 0.0165
-12.9781 -14.9590 17.9684 -0.3268 0.8109 0.4489
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0300
_diffrn_reflns_av_unetI/netI 0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_number 69827
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.350
_diffrn_reflns_theta_min 2.373
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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 -4.00 33.00 1.00 1.00 -- 5.00 -76.00 -30.00 37
2 \w -82.00 -36.00 1.00 1.00 -- 5.00 -76.00 -30.00 46
3 \w -42.00 45.00 1.00 1.00 -- -7.80 76.00 60.00 87
4 \w -79.00 11.00 1.00 1.00 -- -7.80 -76.00 -90.00 90
5 \w -30.00 77.00 1.00 1.00 -- -7.80 57.00 0.00 107
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0374421000
_diffrn_orient_matrix_UB_12 0.0049065000
_diffrn_orient_matrix_UB_13 0.0129402000
_diffrn_orient_matrix_UB_21 -0.0200604000
_diffrn_orient_matrix_UB_22 -0.0073283000
_diffrn_orient_matrix_UB_23 0.0245366000
_diffrn_orient_matrix_UB_31 0.0095333000
_diffrn_orient_matrix_UB_32 -0.0413120000
_diffrn_orient_matrix_UB_33 -0.0025223000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 22123
_reflns_number_total 25354
_reflns_odcompleteness_completeness 98.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_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 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection 'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction 'CrysAlisPro 1.171.39.30c (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 1.360
_refine_diff_density_min -0.547
_refine_diff_density_rms 0.072
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.049
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 1697
_refine_ls_number_reflns 25354
_refine_ls_number_restraints 1593
_refine_ls_R_factor_all 0.0377
_refine_ls_R_factor_gt 0.0305
_refine_ls_restrained_S_all 1.018
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+10.9488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0678
_refine_ls_wR_factor_ref 0.0697
_refine_special_details ?
_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
Cl4A-C124 \\sim Cl4B-C124 \\sim Cl3-C124 \\sim Cl2-C123 \\sim Cl1-C123
with sigma of 0.01
3. Rigid bond restraints
Cl3, C124, Cl4B, Cl4A
with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.008
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
Sof(H12F)=Sof(H12G)=Sof(Cl4A)=1-FVAR(1)
Sof(H12D)=Sof(H12E)=Sof(Cl4B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16), C19(H19), C22(H22),
C25(H25), C28(H28), C31(H31), C34(H34), C37(H37), C40(H40), C43(H43), C46(H46),
C49(H49), C52(H52), C55(H55), C60(H60), C61(H61), C64(H64), C67(H67), C70(H70)
6.b Secondary CH2 refined with riding coordinates:
C123(H12H,H12I), C124(H12D,H12E), C124(H12F,H12G)
6.c Idealised Me refined as rotating group:
C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,
H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C),
C36(H36A,H36B,H36C), C04F(H04A,H04B,H04C), C38(H38A,H38B,H38C), C39(H39A,H39B,
H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,
H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C),
C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,
H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C63(H63A,
H63B,H63C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C),
C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C)
;
_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
Tm1 Tm 0.34704(2) 0.27192(2) 0.35870(2) 0.01841(4) Uani 1 1 d . U . . .
Si1 Si 0.49088(5) 0.38420(5) 0.32165(3) 0.02012(18) Uani 1 1 d . U . . .
Si2 Si 0.37491(5) 0.30480(5) 0.23732(3) 0.02029(18) Uani 1 1 d . U . . .
Si3 Si 0.24319(5) 0.14688(5) 0.41512(3) 0.02327(19) Uani 1 1 d . U . . .
Si4 Si 0.40496(5) 0.06529(5) 0.36795(3) 0.02186(18) Uani 1 1 d . U . . .
N1 N 0.42432(14) 0.31728(14) 0.29603(10) 0.0186(5) Uani 1 1 d . U . . .
N2 N 0.33759(14) 0.14824(14) 0.38064(10) 0.0194(5) Uani 1 1 d . U . . .
C1 C 0.45864(18) 0.38432(17) 0.39545(12) 0.0202(6) Uani 1 1 d . U . . .
H1 H 0.399132 0.394759 0.396869 0.024 Uiso 1 1 calc R . . . .
C2 C 0.4963(2) 0.45118(19) 0.42706(13) 0.0276(7) Uani 1 1 d . U . . .
H2A H 0.555092 0.446036 0.424553 0.041 Uiso 1 1 calc GR . . . .
H2B H 0.478650 0.447054 0.463203 0.041 Uiso 1 1 calc GR . . . .
H2C H 0.478626 0.502025 0.413072 0.041 Uiso 1 1 calc GR . . . .
C3 C 0.4743(2) 0.30679(19) 0.42715(13) 0.0267(7) Uani 1 1 d . U . . .
H3A H 0.459029 0.262098 0.406869 0.040 Uiso 1 1 calc GR . . . .
H3B H 0.442233 0.308618 0.459277 0.040 Uiso 1 1 calc GR . . . .
H3C H 0.531507 0.301401 0.435031 0.040 Uiso 1 1 calc GR . . . .
C4 C 0.4725(2) 0.48949(18) 0.29659(13) 0.0264(7) Uani 1 1 d . U . . .
H4 H 0.472423 0.486156 0.258207 0.032 Uiso 1 1 calc R . . . .
C5 C 0.3881(2) 0.52440(19) 0.31329(14) 0.0301(8) Uani 1 1 d . U . . .
H5A H 0.346644 0.487861 0.304737 0.045 Uiso 1 1 calc GR . . . .
H5B H 0.378165 0.574042 0.295150 0.045 Uiso 1 1 calc GR . . . .
H5C H 0.386587 0.533229 0.350474 0.045 Uiso 1 1 calc GR . . . .
C6 C 0.5390(2) 0.5491(2) 0.30954(15) 0.0339(8) Uani 1 1 d . U . . .
H6A H 0.542814 0.553140 0.346945 0.051 Uiso 1 1 calc GR . . . .
H6B H 0.524490 0.600390 0.294913 0.051 Uiso 1 1 calc GR . . . .
H6C H 0.590915 0.530676 0.294804 0.051 Uiso 1 1 calc GR . . . .
C7 C 0.60454(18) 0.3600(2) 0.31388(14) 0.0287(7) Uani 1 1 d . U . . .
H7 H 0.631814 0.399169 0.334983 0.034 Uiso 1 1 calc R . . . .
C8 C 0.6364(2) 0.3723(2) 0.25734(16) 0.0395(9) Uani 1 1 d . U . . .
H8A H 0.616607 0.331287 0.235515 0.059 Uiso 1 1 calc GR . . . .
H8B H 0.695348 0.369858 0.256533 0.059 Uiso 1 1 calc GR . . . .
H8C H 0.617309 0.423399 0.244541 0.059 Uiso 1 1 calc GR . . . .
C9 C 0.6356(2) 0.2783(2) 0.33347(16) 0.0393(9) Uani 1 1 d . U . . .
H9A H 0.621412 0.272328 0.370076 0.059 Uiso 1 1 calc GR . . . .
H9B H 0.694184 0.273943 0.328658 0.059 Uiso 1 1 calc GR . . . .
H9C H 0.610781 0.237386 0.313958 0.059 Uiso 1 1 calc GR . . . .
C10 C 0.3720(2) 0.39587(19) 0.19306(13) 0.0302(7) Uani 1 1 d . U . . .
H10 H 0.367601 0.442174 0.216148 0.036 Uiso 1 1 calc R . . . .
C11 C 0.3001(2) 0.4041(2) 0.15539(15) 0.0403(9) Uani 1 1 d . U . . .
H11A H 0.299181 0.357658 0.133860 0.060 Uiso 1 1 calc GR . . . .
H11B H 0.306713 0.450427 0.133456 0.060 Uiso 1 1 calc GR . . . .
H11C H 0.249425 0.409488 0.175303 0.060 Uiso 1 1 calc GR . . . .
C12 C 0.4534(2) 0.4023(2) 0.16172(15) 0.0410(9) Uani 1 1 d . U . . .
H12A H 0.498227 0.399931 0.185427 0.062 Uiso 1 1 calc GR . . . .
H12B H 0.453489 0.451972 0.142713 0.062 Uiso 1 1 calc GR . . . .
H12C H 0.459323 0.359063 0.137456 0.062 Uiso 1 1 calc GR . . . .
C13 C 0.26458(18) 0.28415(18) 0.26222(13) 0.0228(7) Uani 1 1 d . U . . .
H13 H 0.270253 0.243713 0.290032 0.027 Uiso 1 1 calc R . . . .
C14 C 0.2228(2) 0.35748(19) 0.28843(14) 0.0305(8) Uani 1 1 d . U . . .
H14A H 0.256106 0.374952 0.316326 0.046 Uiso 1 1 calc GR . . . .
H14B H 0.169906 0.343762 0.302437 0.046 Uiso 1 1 calc GR . . . .
H14C H 0.216474 0.399529 0.262882 0.046 Uiso 1 1 calc GR . . . .
C15 C 0.2068(2) 0.2493(2) 0.22176(14) 0.0327(8) Uani 1 1 d . U . . .
H15A H 0.201032 0.285698 0.192657 0.049 Uiso 1 1 calc GR . . . .
H15B H 0.153890 0.241431 0.238103 0.049 Uiso 1 1 calc GR . . . .
H15C H 0.229472 0.199256 0.209451 0.049 Uiso 1 1 calc GR . . . .
C16 C 0.4130(2) 0.21069(18) 0.20306(13) 0.0253(7) Uani 1 1 d . U . . .
H16 H 0.388490 0.166983 0.223103 0.030 Uiso 1 1 calc R . . . .
C17 C 0.3861(2) 0.2000(2) 0.14639(14) 0.0356(8) Uani 1 1 d . U . . .
H17A H 0.328799 0.214380 0.143956 0.053 Uiso 1 1 calc GR . . . .
H17B H 0.395192 0.145452 0.136422 0.053 Uiso 1 1 calc GR . . . .
H17C H 0.417410 0.233634 0.123318 0.053 Uiso 1 1 calc GR . . . .
C18 C 0.5059(2) 0.1957(2) 0.20630(15) 0.0377(9) Uani 1 1 d . U . . .
H18A H 0.533634 0.232441 0.183413 0.056 Uiso 1 1 calc GR . . . .
H18B H 0.519922 0.142191 0.195776 0.056 Uiso 1 1 calc GR . . . .
H18C H 0.522451 0.203240 0.241744 0.056 Uiso 1 1 calc GR . . . .
C19 C 0.19975(19) 0.25567(19) 0.41051(14) 0.0281(7) Uani 1 1 d . U . . .
H19 H 0.205260 0.270946 0.373377 0.034 Uiso 1 1 calc R . . . .
C20 C 0.2429(2) 0.3204(2) 0.44104(16) 0.0374(9) Uani 1 1 d . U . . .
H20A H 0.301280 0.313669 0.435951 0.056 Uiso 1 1 calc GR . . . .
H20B H 0.228979 0.315653 0.477768 0.056 Uiso 1 1 calc GR . . . .
H20C H 0.225356 0.372077 0.428395 0.056 Uiso 1 1 calc GR . . . .
C21 C 0.1059(2) 0.2665(3) 0.42505(19) 0.0501(11) Uani 1 1 d . U . . .
H21A H 0.076046 0.226488 0.407836 0.075 Uiso 1 1 calc GR . . . .
H21B H 0.086404 0.318328 0.413820 0.075 Uiso 1 1 calc GR . . . .
H21C H 0.097860 0.261270 0.462379 0.075 Uiso 1 1 calc GR . . . .
C22 C 0.2543(2) 0.1188(2) 0.48675(14) 0.0371(8) Uani 1 1 d . U . . .
H22 H 0.259359 0.060554 0.488086 0.045 Uiso 1 1 calc R . . . .
C23 C 0.3317(2) 0.1492(3) 0.51217(15) 0.0430(9) Uani 1 1 d . U . . .
H23A H 0.379347 0.133104 0.491446 0.064 Uiso 1 1 calc GR . . . .
H23B H 0.336056 0.127253 0.546971 0.064 Uiso 1 1 calc GR . . . .
H23C H 0.328118 0.206292 0.513933 0.064 Uiso 1 1 calc GR . . . .
C24 C 0.1800(3) 0.1421(3) 0.52229(16) 0.0556(12) Uani 1 1 d . U . . .
H24A H 0.176616 0.198882 0.526033 0.083 Uiso 1 1 calc GR . . . .
H24B H 0.186181 0.117383 0.556189 0.083 Uiso 1 1 calc GR . . . .
H24C H 0.130807 0.124462 0.506872 0.083 Uiso 1 1 calc GR . . . .
C25 C 0.1687(2) 0.0817(2) 0.38069(14) 0.0301(8) Uani 1 1 d . U . . .
H25 H 0.202509 0.036625 0.367354 0.036 Uiso 1 1 calc R . . . .
C26 C 0.1026(3) 0.0440(3) 0.41566(16) 0.0526(12) Uani 1 1 d . U . . .
H26A H 0.127651 0.019022 0.445595 0.079 Uiso 1 1 calc GR . . . .
H26B H 0.075216 0.004748 0.396089 0.079 Uiso 1 1 calc GR . . . .
H26C H 0.063445 0.084435 0.427249 0.079 Uiso 1 1 calc GR . . . .
C27 C 0.1293(2) 0.1193(2) 0.33184(15) 0.0352(8) Uani 1 1 d . U . . .
H27A H 0.085809 0.156071 0.342483 0.053 Uiso 1 1 calc GR . . . .
H27B H 0.107396 0.078222 0.310931 0.053 Uiso 1 1 calc GR . . . .
H27C H 0.169950 0.146957 0.311564 0.053 Uiso 1 1 calc GR . . . .
C28 C 0.51241(19) 0.10477(19) 0.37356(14) 0.0291(7) Uani 1 1 d . U . . .
H28 H 0.508344 0.158929 0.358964 0.035 Uiso 1 1 calc R . . . .
C29 C 0.5403(2) 0.1156(2) 0.42989(15) 0.0364(9) Uani 1 1 d . U . . .
H29A H 0.496289 0.139764 0.450537 0.055 Uiso 1 1 calc GR . . . .
H29B H 0.586752 0.149221 0.429649 0.055 Uiso 1 1 calc GR . . . .
H29C H 0.555427 0.064629 0.444801 0.055 Uiso 1 1 calc GR . . . .
C30 C 0.5827(2) 0.0632(2) 0.34107(18) 0.0431(10) Uani 1 1 d . U . . .
H30A H 0.590802 0.009426 0.353447 0.065 Uiso 1 1 calc GR . . . .
H30B H 0.632313 0.091499 0.344878 0.065 Uiso 1 1 calc GR . . . .
H30C H 0.568590 0.062981 0.304728 0.065 Uiso 1 1 calc GR . . . .
C31 C 0.3968(2) 0.03290(18) 0.29731(13) 0.0261(7) Uani 1 1 d . U . . .
H31 H 0.427788 0.071955 0.276816 0.031 Uiso 1 1 calc R . . . .
C32 C 0.3105(2) 0.0377(2) 0.27462(14) 0.0319(8) Uani 1 1 d . U . . .
H32A H 0.277865 -0.003027 0.290450 0.048 Uiso 1 1 calc GR . . . .
H32B H 0.314403 0.030016 0.237333 0.048 Uiso 1 1 calc GR . . . .
H32C H 0.285348 0.088999 0.281861 0.048 Uiso 1 1 calc GR . . . .
C33 C 0.4375(2) -0.0482(2) 0.28271(15) 0.0385(9) Uani 1 1 d . U . . .
H33A H 0.491691 -0.052092 0.296594 0.058 Uiso 1 1 calc GR . . . .
H33B H 0.440985 -0.052910 0.245190 0.058 Uiso 1 1 calc GR . . . .
H33C H 0.405301 -0.090264 0.297257 0.058 Uiso 1 1 calc GR . . . .
C34 C 0.3928(2) -0.0213(2) 0.41681(14) 0.0344(8) Uani 1 1 d . U . . .
H34 H 0.389685 0.002340 0.451821 0.041 Uiso 1 1 calc R . . . .
C35 C 0.3154(3) -0.0702(2) 0.41223(16) 0.0432(9) Uani 1 1 d . U . . .
H35A H 0.267917 -0.037883 0.422007 0.065 Uiso 1 1 calc GR . . . .
H35B H 0.319213 -0.115852 0.435168 0.065 Uiso 1 1 calc GR . . . .
H35C H 0.310881 -0.087468 0.376663 0.065 Uiso 1 1 calc GR . . . .
C36 C 0.4685(3) -0.0791(2) 0.41624(17) 0.0451(10) Uani 1 1 d . U . . .
H36A H 0.472767 -0.105781 0.383097 0.068 Uiso 1 1 calc GR . . . .
H36B H 0.462656 -0.117751 0.444014 0.068 Uiso 1 1 calc GR . . . .
H36C H 0.517058 -0.049736 0.421242 0.068 Uiso 1 1 calc GR . . . .
Tm2 Tm 0.82042(2) 0.80056(2) 0.15101(2) 0.01801(4) Uani 1 1 d . U . . .
Si5 Si 0.96712(5) 0.91036(5) 0.18338(3) 0.01828(17) Uani 1 1 d . U . . .
Si6 Si 0.85926(5) 0.81864(5) 0.27167(3) 0.01877(17) Uani 1 1 d . U . . .
Si7 Si 0.71065(5) 0.68673(5) 0.09463(3) 0.02043(18) Uani 1 1 d . U . . .
Si8 Si 0.87092(5) 0.59440(5) 0.13118(4) 0.02245(18) Uani 1 1 d . U . . .
N3 N 0.90155(14) 0.84114(14) 0.21060(10) 0.0186(5) Uani 1 1 d . U . . .
N4 N 0.80568(14) 0.68024(14) 0.12479(10) 0.0193(5) Uani 1 1 d . U . . .
C04F C 0.5635(2) 0.5923(2) 0.09647(16) 0.0416(9) Uani 1 1 d . U . . .
H04A H 0.527152 0.636264 0.087400 0.062 Uiso 1 1 calc GR . . . .
H04B H 0.533395 0.553314 0.116069 0.062 Uiso 1 1 calc GR . . . .
H04C H 0.586502 0.568765 0.065010 0.062 Uiso 1 1 calc GR . . . .
C37 C 0.94836(19) 1.01340(17) 0.21212(13) 0.0236(7) Uani 1 1 d . U . . .
H37 H 0.945371 1.005606 0.250296 0.028 Uiso 1 1 calc R . . . .
C38 C 0.8654(2) 1.05187(19) 0.19720(14) 0.0294(7) Uani 1 1 d . U . . .
H38A H 0.822513 1.015476 0.205074 0.044 Uiso 1 1 calc GR . . . .
H38B H 0.866169 1.064372 0.160328 0.044 Uiso 1 1 calc GR . . . .
H38C H 0.855456 1.099816 0.216856 0.044 Uiso 1 1 calc GR . . . .
C39 C 1.0164(2) 1.07357(19) 0.20165(15) 0.0335(8) Uani 1 1 d . U . . .
H39A H 1.019182 1.086673 0.164881 0.050 Uiso 1 1 calc GR . . . .
H39B H 1.068165 1.050458 0.212120 0.050 Uiso 1 1 calc GR . . . .
H39C H 1.004189 1.121014 0.221422 0.050 Uiso 1 1 calc GR . . . .
C40 C 0.93397(18) 0.91687(18) 0.11131(12) 0.0222(6) Uani 1 1 d . U . . .
H40 H 0.875275 0.931560 0.112190 0.027 Uiso 1 1 calc R . . . .
C41 C 0.9772(2) 0.9833(2) 0.08015(14) 0.0311(8) Uani 1 1 d . U . . .
H41A H 1.035529 0.974116 0.081093 0.047 Uiso 1 1 calc GR . . . .
H41B H 0.962760 1.033945 0.095582 0.047 Uiso 1 1 calc GR . . . .
H41C H 0.960079 0.983319 0.044376 0.047 Uiso 1 1 calc GR . . . .
C42 C 0.9442(2) 0.84103(19) 0.07735(13) 0.0274(7) Uani 1 1 d . U . . .
H42A H 0.925534 0.795930 0.097185 0.041 Uiso 1 1 calc GR . . . .
H42B H 1.001040 0.832472 0.067500 0.041 Uiso 1 1 calc GR . . . .
H42C H 0.912425 0.847711 0.046331 0.041 Uiso 1 1 calc GR . . . .
C43 C 1.08073(18) 0.88552(19) 0.18614(13) 0.0246(7) Uani 1 1 d . U . . .
H43 H 1.107941 0.928733 0.167182 0.030 Uiso 1 1 calc R . . . .
C44 C 1.1126(2) 0.8866(2) 0.24227(15) 0.0341(8) Uani 1 1 d . U . . .
H44A H 1.089524 0.843868 0.262392 0.051 Uiso 1 1 calc GR . . . .
H44B H 1.096978 0.936515 0.258306 0.051 Uiso 1 1 calc GR . . . .
H44C H 1.171387 0.880245 0.241223 0.051 Uiso 1 1 calc GR . . . .
C45 C 1.1105(2) 0.8088(2) 0.15912(16) 0.0355(8) Uani 1 1 d . U . . .
H45A H 1.097077 0.811549 0.122666 0.053 Uiso 1 1 calc GR . . . .
H45B H 1.084308 0.764285 0.175490 0.053 Uiso 1 1 calc GR . . . .
H45C H 1.168918 0.802284 0.162197 0.053 Uiso 1 1 calc GR . . . .
C46 C 0.74664(18) 0.80275(18) 0.25424(12) 0.0218(6) Uani 1 1 d . U . . .
H46 H 0.748446 0.762587 0.226594 0.026 Uiso 1 1 calc R . . . .
C47 C 0.70157(19) 0.87684(19) 0.23093(14) 0.0277(7) Uani 1 1 d . U . . .
H47A H 0.731508 0.895209 0.200445 0.042 Uiso 1 1 calc GR . . . .
H47B H 0.697788 0.918223 0.256646 0.042 Uiso 1 1 calc GR . . . .
H47C H 0.647408 0.863131 0.221209 0.042 Uiso 1 1 calc GR . . . .
C48 C 0.6927(2) 0.7688(2) 0.29932(15) 0.0360(8) Uani 1 1 d . U . . .
H48A H 0.692334 0.804148 0.328693 0.054 Uiso 1 1 calc GR . . . .
H48B H 0.714579 0.717439 0.309720 0.054 Uiso 1 1 calc GR . . . .
H48C H 0.637705 0.763822 0.287569 0.054 Uiso 1 1 calc GR . . . .
C49 C 0.8612(2) 0.8907(2) 0.32779(15) 0.0356(8) Uani 1 1 d . U . . .
H49 H 0.837131 0.860137 0.356951 0.043 Uiso 1 1 calc R . . . .
C50 C 0.8113(3) 0.9663(2) 0.32929(17) 0.0482(10) Uani 1 1 d . U . . .
H50A H 0.754105 0.954631 0.329805 0.072 Uiso 1 1 calc GR . . . .
H50B H 0.824189 0.997911 0.298752 0.072 Uiso 1 1 calc GR . . . .
H50C H 0.823459 0.995142 0.360293 0.072 Uiso 1 1 calc GR . . . .
C51 C 0.9480(2) 0.9044(2) 0.34666(15) 0.0387(9) Uani 1 1 d . U . . .
H51A H 0.975205 0.940018 0.322745 0.058 Uiso 1 1 calc GR . . . .
H51B H 0.978343 0.854514 0.348036 0.058 Uiso 1 1 calc GR . . . .
H51C H 0.944746 0.927376 0.381029 0.058 Uiso 1 1 calc GR . . . .
C52 C 0.89869(19) 0.71876(19) 0.29771(13) 0.0266(7) Uani 1 1 d . U . . .
H52 H 0.868262 0.679294 0.278816 0.032 Uiso 1 1 calc R . . . .
C53 C 0.8803(2) 0.7012(2) 0.35613(14) 0.0377(9) Uani 1 1 d . U . . .
H53A H 0.915446 0.731668 0.377235 0.057 Uiso 1 1 calc GR . . . .
H53B H 0.889995 0.645507 0.363167 0.057 Uiso 1 1 calc GR . . . .
H53C H 0.824018 0.715614 0.364452 0.057 Uiso 1 1 calc GR . . . .
C54 C 0.9890(2) 0.6984(2) 0.28473(16) 0.0376(9) Uani 1 1 d . U . . .
H54A H 1.023010 0.729943 0.305936 0.056 Uiso 1 1 calc GR . . . .
H54B H 1.000456 0.709658 0.248278 0.056 Uiso 1 1 calc GR . . . .
H54C H 1.000378 0.642966 0.291809 0.056 Uiso 1 1 calc GR . . . .
C55 C 0.67398(18) 0.79641(18) 0.10502(13) 0.0234(7) Uani 1 1 d . U . . .
H55 H 0.681448 0.807428 0.142248 0.028 Uiso 1 1 calc R . . . .
C56 C 0.7201(2) 0.86139(19) 0.07388(14) 0.0296(8) Uani 1 1 d . U . . .
H56A H 0.777891 0.848266 0.073115 0.044 Uiso 1 1 calc GR . . . .
H56B H 0.710337 0.911898 0.090570 0.044 Uiso 1 1 calc GR . . . .
H56C H 0.700737 0.864321 0.038631 0.044 Uiso 1 1 calc GR . . . .
C57 C 0.5817(2) 0.8109(2) 0.09515(16) 0.0348(8) Uani 1 1 d . U . . .
H57A H 0.550786 0.771758 0.114093 0.052 Uiso 1 1 calc GR . . . .
H57B H 0.572039 0.806797 0.058279 0.052 Uiso 1 1 calc GR . . . .
H57C H 0.564726 0.863132 0.106941 0.052 Uiso 1 1 calc GR . . . .
C58 C 0.6412(2) 0.6951(2) -0.00912(15) 0.0394(9) Uani 1 1 d . U . . .
H58A H 0.641277 0.752168 -0.011637 0.059 Uiso 1 1 calc GR . . . .
H58B H 0.591957 0.679149 0.008907 0.059 Uiso 1 1 calc GR . . . .
H58C H 0.643655 0.673032 -0.043745 0.059 Uiso 1 1 calc GR . . . .
C59 C 0.7948(2) 0.6928(2) -0.00661(14) 0.0384(9) Uani 1 1 d . U . . .
H59A H 0.842200 0.671518 0.010941 0.058 Uiso 1 1 calc GR . . . .
H59B H 0.794925 0.749926 -0.006300 0.058 Uiso 1 1 calc GR . . . .
H59C H 0.795972 0.674766 -0.042255 0.058 Uiso 1 1 calc GR . . . .
C60 C 0.7170(2) 0.6644(2) 0.02176(13) 0.0292(7) Uani 1 1 d . U . . .
H60 H 0.718506 0.606250 0.018895 0.035 Uiso 1 1 calc R . . . .
C61 C 0.6330(2) 0.6224(2) 0.13011(14) 0.0296(7) Uani 1 1 d . U . . .
H61 H 0.664290 0.574205 0.140573 0.036 Uiso 1 1 calc R . . . .
C63 C 0.5964(2) 0.6565(2) 0.18173(15) 0.0388(9) Uani 1 1 d . U . . .
H63A H 0.639011 0.679888 0.201136 0.058 Uiso 1 1 calc GR . . . .
H63B H 0.572618 0.614568 0.202247 0.058 Uiso 1 1 calc GR . . . .
H63C H 0.554870 0.696508 0.174020 0.058 Uiso 1 1 calc GR . . . .
C64 C 0.9794(2) 0.6322(2) 0.12113(15) 0.0317(8) Uani 1 1 d . U . . .
H64 H 0.977781 0.684611 0.137668 0.038 Uiso 1 1 calc R . . . .
C65 C 1.0045(2) 0.6483(2) 0.06366(16) 0.0391(9) Uani 1 1 d . U . . .
H65A H 0.962026 0.679697 0.047090 0.059 Uiso 1 1 calc GR . . . .
H65B H 1.012605 0.598655 0.045664 0.059 Uiso 1 1 calc GR . . . .
H65C H 1.054624 0.676696 0.062256 0.059 Uiso 1 1 calc GR . . . .
C66 C 1.0488(2) 0.5852(2) 0.14825(18) 0.0465(10) Uani 1 1 d . U . . .
H66A H 1.035967 0.580603 0.185125 0.070 Uiso 1 1 calc GR . . . .
H66B H 1.099202 0.612547 0.143231 0.070 Uiso 1 1 calc GR . . . .
H66C H 1.054803 0.533009 0.133365 0.070 Uiso 1 1 calc GR . . . .
C67 C 0.8644(2) 0.55559(19) 0.20109(13) 0.0287(7) Uani 1 1 d . U . . .
H67 H 0.896805 0.592229 0.221071 0.034 Uiso 1 1 calc R . . . .
C68 C 0.7793(2) 0.5597(2) 0.22768(14) 0.0349(8) Uani 1 1 d . U . . .
H68A H 0.745339 0.521037 0.212429 0.052 Uiso 1 1 calc GR . . . .
H68B H 0.754884 0.612009 0.222764 0.052 Uiso 1 1 calc GR . . . .
H68C H 0.784096 0.548715 0.264551 0.052 Uiso 1 1 calc GR . . . .
C69 C 0.9037(3) 0.4728(2) 0.21216(16) 0.0455(10) Uani 1 1 d . U . . .
H69A H 0.957632 0.469265 0.196137 0.068 Uiso 1 1 calc GR . . . .
H69B H 0.870456 0.432679 0.197874 0.068 Uiso 1 1 calc GR . . . .
H69C H 0.907523 0.464682 0.249394 0.068 Uiso 1 1 calc GR . . . .
C70 C 0.8528(2) 0.51309(19) 0.08122(14) 0.0327(8) Uani 1 1 d . U . . .
H70 H 0.846867 0.539790 0.047066 0.039 Uiso 1 1 calc R . . . .
C71 C 0.9265(3) 0.4534(2) 0.07551(17) 0.0446(10) Uani 1 1 d . U . . .
H71A H 0.933966 0.425197 0.108119 0.067 Uiso 1 1 calc GR . . . .
H71B H 0.975138 0.481633 0.066504 0.067 Uiso 1 1 calc GR . . . .
H71C H 0.916201 0.416123 0.048345 0.067 Uiso 1 1 calc GR . . . .
C72 C 0.7748(2) 0.4649(2) 0.09095(16) 0.0413(9) Uani 1 1 d . U . . .
H72A H 0.774601 0.421753 0.066551 0.062 Uiso 1 1 calc GR . . . .
H72B H 0.727081 0.498951 0.086187 0.062 Uiso 1 1 calc GR . . . .
H72C H 0.774334 0.443916 0.126169 0.062 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.77873(7) 0.38190(10) 0.76363(5) 0.0749(4) Uani 1 1 d D U . . .
Cl2 Cl 0.62580(7) 0.37555(8) 0.82409(5) 0.0649(3) Uani 1 1 d D U . . .
C123 C 0.7221(2) 0.3297(3) 0.81065(16) 0.0520(11) Uani 1 1 d D U . . .
H12H H 0.752591 0.325736 0.842807 0.062 Uiso 1 1 calc R . . . .
H12I H 0.714585 0.276086 0.798312 0.062 Uiso 1 1 calc R . . . .
Cl3 Cl 0.88998(8) 0.17805(8) 0.33176(6) 0.0761(4) Uani 1 1 d D U . . .
C124 C 0.8960(2) 0.2726(3) 0.30457(19) 0.0638(13) Uani 1 1 d D U . . .
H12D H 0.880354 0.311623 0.331097 0.077 Uiso 0.41(4) 1 calc R . P A 1
H12E H 0.857440 0.278300 0.276338 0.077 Uiso 0.41(4) 1 calc R . P A 1
H12F H 0.871649 0.272571 0.270255 0.077 Uiso 0.59(4) 1 calc R . P A 2
H12G H 0.863485 0.309347 0.326384 0.077 Uiso 0.59(4) 1 calc R . P A 2
Cl4B Cl 0.9937(4) 0.2918(6) 0.2802(3) 0.053(2) Uani 0.41(4) 1 d D U P A 1
Cl4A Cl 0.9933(3) 0.3073(8) 0.2977(11) 0.094(3) Uani 0.59(4) 1 d D U P A 2
F00F F 0.55614(10) 0.27056(10) 0.05963(7) 0.0272(4) Uani 1 1 d . U . . .
F00H F 0.79316(11) 0.01665(10) 0.03224(7) 0.0273(4) Uani 1 1 d . U . . .
F00L F 0.76516(12) 0.42053(11) -0.07395(8) 0.0345(5) Uani 1 1 d . U . . .
F00M F 0.71327(10) 0.07376(11) 0.12861(7) 0.0278(4) Uani 1 1 d . U . . .
F00O F 0.79788(10) 0.26945(10) -0.04785(7) 0.0280(4) Uani 1 1 d . U . . .
F00P F 0.62776(12) 0.49844(10) -0.03485(8) 0.0348(5) Uani 1 1 d . U . . .
F00Q F 0.59197(12) -0.00763(11) 0.16915(8) 0.0350(5) Uani 1 1 d . U . . .
F00S F 0.69687(11) 0.24151(11) 0.12586(7) 0.0299(4) Uani 1 1 d . U . . .
F00T F 0.54822(11) 0.14722(11) -0.01518(7) 0.0294(4) Uani 1 1 d . U . . .
F00U F 0.89393(10) 0.14399(11) 0.00018(8) 0.0289(4) Uani 1 1 d . U . . .
F00Y F 0.42547(11) 0.06563(12) 0.02742(8) 0.0354(5) Uani 1 1 d . U . . .
F00Z F 0.70373(12) 0.08232(12) -0.16662(8) 0.0369(5) Uani 1 1 d . U . . .
F01C F 1.01194(11) 0.19557(13) 0.05827(9) 0.0420(5) Uani 1 1 d . U . . .
F01D F 0.44628(11) -0.01409(11) 0.12060(9) 0.0377(5) Uani 1 1 d . U . . .
F01E F 0.97731(13) 0.26884(12) 0.15160(9) 0.0462(6) Uani 1 1 d . U . . .
F01J F 0.81730(13) 0.28852(12) 0.18472(8) 0.0415(5) Uani 1 1 d . U . . .
F01K F 0.77999(13) -0.06009(12) -0.14322(9) 0.0429(5) Uani 1 1 d . U . . .
F011 F 0.67057(11) 0.18921(11) -0.09408(7) 0.0306(4) Uani 1 1 d . U . . .
F014 F 0.52503(11) 0.42022(10) 0.03252(8) 0.0320(4) Uani 1 1 d . U . . .
F019 F 0.82435(13) -0.09087(11) -0.04217(9) 0.0405(5) Uani 1 1 d . U . . .
C73 C 0.73193(17) 0.11022(17) -0.02648(12) 0.0205(6) Uani 1 1 d . U . . .
C74 C 0.70999(18) 0.12129(18) -0.07803(13) 0.0231(7) Uani 1 1 d . U . . .
C75 C 0.72592(19) 0.0666(2) -0.11727(13) 0.0274(7) Uani 1 1 d . U . . .
C76 C 0.7644(2) -0.00555(19) -0.10562(14) 0.0296(7) Uani 1 1 d . U . . .
C77 C 0.78663(19) -0.02066(18) -0.05491(14) 0.0278(7) Uani 1 1 d . U . . .
C78 C 0.76996(18) 0.03581(18) -0.01729(13) 0.0223(6) Uani 1 1 d . U . . .
C79 C 0.67825(17) 0.26034(17) 0.00608(12) 0.0197(6) Uani 1 1 d . U . . .
C80 C 0.72789(18) 0.30418(18) -0.02723(12) 0.0213(6) Uani 1 1 d . U . . .
C81 C 0.71287(19) 0.38247(18) -0.04152(13) 0.0248(7) Uani 1 1 d . U . . .
C82 C 0.64347(19) 0.42174(18) -0.02178(13) 0.0242(7) Uani 1 1 d . U . . .
C83 C 0.59244(18) 0.38206(18) 0.01181(13) 0.0230(7) Uani 1 1 d . U . . .
C84 C 0.61008(18) 0.30341(18) 0.02547(12) 0.0208(6) Uani 1 1 d . U . . .
C85 C 0.63639(17) 0.11858(17) 0.05506(12) 0.0194(6) Uani 1 1 d . U . . .
C86 C 0.56128(18) 0.11084(18) 0.03138(12) 0.0221(6) Uani 1 1 d . U . . .
C87 C 0.49742(18) 0.06839(18) 0.05229(14) 0.0250(7) Uani 1 1 d . U . . .
C88 C 0.50726(19) 0.02802(18) 0.09885(14) 0.0264(7) Uani 1 1 d . U . . .
C89 C 0.58084(19) 0.03154(18) 0.12340(13) 0.0243(7) Uani 1 1 d . U . . .
C90 C 0.64337(18) 0.07581(17) 0.10119(13) 0.0210(6) Uani 1 1 d . U . . .
C91 C 0.78801(18) 0.18813(17) 0.06039(12) 0.0198(6) Uani 1 1 d . U . . .
C92 C 0.87008(19) 0.17934(18) 0.04578(13) 0.0236(7) Uani 1 1 d . U . . .
C93 C 0.93366(19) 0.20580(19) 0.07542(14) 0.0292(7) Uani 1 1 d . U . . .
C94 C 0.9165(2) 0.24289(19) 0.12229(14) 0.0302(8) Uani 1 1 d . U . . .
C95 C 0.8359(2) 0.25312(18) 0.13877(13) 0.0274(7) Uani 1 1 d . U . . .
C96 C 0.77432(18) 0.22714(17) 0.10783(13) 0.0232(7) Uani 1 1 d . U . . .
B1 B 0.7086(2) 0.1689(2) 0.02361(14) 0.0196(7) Uani 1 1 d . U . . .
F00G F 0.69815(11) 0.49683(10) 0.54782(7) 0.0269(4) Uani 1 1 d . U . . .
F00I F 0.78531(10) 0.44014(11) 0.63839(7) 0.0292(4) Uani 1 1 d . U . . .
F00J F 0.60374(10) 0.36616(11) 0.51945(7) 0.0291(4) Uani 1 1 d . U . . .
F00K F 0.94462(11) 0.24522(10) 0.56320(7) 0.0286(4) Uani 1 1 d . U . . .
F00N F 0.95290(11) 0.36968(11) 0.49024(7) 0.0303(4) Uani 1 1 d . U . . .
F00R F 0.80717(11) 0.27166(11) 0.63640(7) 0.0298(4) Uani 1 1 d . U . . .
F00V F 0.70143(10) 0.25028(10) 0.46476(8) 0.0285(4) Uani 1 1 d . U . . .
F00W F 0.82767(11) 0.33625(11) 0.41573(7) 0.0303(4) Uani 1 1 d . U . . .
F00X F 0.48901(11) 0.31395(12) 0.58429(9) 0.0394(5) Uani 1 1 d . U . . .
F01A F 0.90839(12) 0.51537(12) 0.67761(9) 0.0409(5) Uani 1 1 d . U . . .
F01B F 0.68945(13) 0.22295(12) 0.70235(8) 0.0392(5) Uani 1 1 d . U . . .
F01F F 0.70535(12) 0.58223(12) 0.37251(8) 0.0378(5) Uani 1 1 d . U . . .
F01L F 0.52840(12) 0.24384(12) 0.67779(9) 0.0402(5) Uani 1 1 d . U . . .
F010 F 0.74495(11) 0.10735(11) 0.42661(8) 0.0354(5) Uani 1 1 d . U . . .
F012 F 0.98421(11) 0.10378(11) 0.52494(8) 0.0335(5) Uani 1 1 d . U . . .
F013 F 0.78789(11) 0.44421(12) 0.34492(7) 0.0331(4) Uani 1 1 d . U . . .
F015 F 1.07708(11) 0.44393(12) 0.53183(8) 0.0371(5) Uani 1 1 d . U . . .
F016 F 0.88822(12) 0.03344(11) 0.45462(8) 0.0369(5) Uani 1 1 d . U . . .
F017 F 0.65800(12) 0.60485(11) 0.47479(8) 0.0353(5) Uani 1 1 d . U . . .
F018 F 1.05572(12) 0.51988(13) 0.62539(9) 0.0440(5) Uani 1 1 d . U . . .
C98 C 0.85623(18) 0.43786(18) 0.60966(13) 0.0232(7) Uani 1 1 d . U . . .
C99 C 0.9196(2) 0.47886(18) 0.63094(14) 0.0272(7) Uani 1 1 d . U . . .
C100 C 0.99361(19) 0.48131(19) 0.60473(14) 0.0290(7) Uani 1 1 d . U . . .
C101 C 1.00390(18) 0.44291(19) 0.55759(14) 0.0262(7) Uani 1 1 d . U . . .
C102 C 0.93902(18) 0.40382(17) 0.53765(12) 0.0218(6) Uani 1 1 d . U . . .
C103 C 0.86337(18) 0.39668(17) 0.56288(12) 0.0208(6) Uani 1 1 d . U . . .
C105 C 0.89248(18) 0.21532(18) 0.52847(12) 0.0218(6) Uani 1 1 d . U . . .
C106 C 0.91500(18) 0.14130(19) 0.50935(13) 0.0241(7) Uani 1 1 d . U . . .
C107 C 0.86636(19) 0.10504(18) 0.47434(13) 0.0251(7) Uani 1 1 d . U . . .
C108 C 0.79404(19) 0.14289(19) 0.46017(13) 0.0241(7) Uani 1 1 d . U . . .
C109 C 0.77390(18) 0.21659(18) 0.48030(13) 0.0218(6) Uani 1 1 d . U . . .
C110 C 0.82181(18) 0.25862(18) 0.51396(12) 0.0204(6) Uani 1 1 d . U . . .
C111 C 0.76323(18) 0.40864(18) 0.48619(12) 0.0208(6) Uani 1 1 d . U . . .
C112 C 0.78439(18) 0.40112(18) 0.43357(13) 0.0242(7) Uani 1 1 d . U . . .
C113 C 0.76532(19) 0.4572(2) 0.39538(13) 0.0263(7) Uani 1 1 d . U . . .
C114 C 0.72317(19) 0.52656(19) 0.40912(13) 0.0267(7) Uani 1 1 d . U . . .
C115 C 0.70059(18) 0.53778(18) 0.46053(14) 0.0256(7) Uani 1 1 d . U . . .
C116 C 0.72124(18) 0.48059(18) 0.49747(13) 0.0225(7) Uani 1 1 d . U . . .
C117 C 0.71297(18) 0.32483(17) 0.57505(12) 0.0214(6) Uani 1 1 d . U . . .
C118 C 0.72857(19) 0.28590(18) 0.62235(13) 0.0233(7) Uani 1 1 d . U . . .
C119 C 0.6690(2) 0.25915(18) 0.65715(13) 0.0270(7) Uani 1 1 d . U . . .
C120 C 0.5875(2) 0.26917(18) 0.64461(14) 0.0285(7) Uani 1 1 d . U . . .
C121 C 0.56784(18) 0.30476(18) 0.59791(14) 0.0270(7) Uani 1 1 d . U . . .
C122 C 0.62965(18) 0.33160(18) 0.56458(13) 0.0229(7) Uani 1 1 d . U . . .
B2 B 0.7899(2) 0.3474(2) 0.53468(14) 0.0206(7) Uani 1 1 d . U . . .
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
Tm1 0.01825(7) 0.01756(7) 0.01946(8) -0.00244(5) 0.00245(5) -0.00290(5)
Si1 0.0183(4) 0.0210(4) 0.0213(5) -0.0022(3) 0.0016(3) -0.0042(3)
Si2 0.0249(4) 0.0177(4) 0.0183(4) -0.0009(3) -0.0002(3) -0.0019(3)
Si3 0.0235(4) 0.0263(4) 0.0206(5) -0.0044(4) 0.0034(3) -0.0099(4)
Si4 0.0256(4) 0.0177(4) 0.0224(5) -0.0002(3) -0.0032(4) -0.0010(3)
N1 0.0203(12) 0.0180(12) 0.0176(13) -0.0009(10) 0.0016(10) -0.0031(10)
N2 0.0189(12) 0.0202(12) 0.0193(14) -0.0020(10) 0.0003(10) -0.0036(10)
C1 0.0177(14) 0.0224(15) 0.0209(16) -0.0043(12) -0.0003(12) -0.0029(12)
C2 0.0307(18) 0.0256(17) 0.0272(19) -0.0033(14) -0.0042(14) -0.0066(14)
C3 0.0260(17) 0.0269(16) 0.0277(19) -0.0030(14) -0.0030(14) -0.0053(13)
C4 0.0322(17) 0.0233(16) 0.0239(18) -0.0009(13) 0.0016(14) -0.0075(13)
C5 0.0357(18) 0.0187(16) 0.036(2) -0.0033(14) -0.0053(15) 0.0000(13)
C6 0.041(2) 0.0261(17) 0.035(2) -0.0027(15) 0.0038(16) -0.0122(15)
C7 0.0158(15) 0.0330(18) 0.038(2) -0.0070(15) 0.0027(13) -0.0063(13)
C8 0.0304(19) 0.044(2) 0.044(2) -0.0037(18) 0.0145(16) -0.0053(16)
C9 0.0208(17) 0.052(2) 0.045(2) 0.0033(18) 0.0032(16) 0.0054(16)
C10 0.047(2) 0.0211(16) 0.0228(18) 0.0010(13) -0.0033(15) -0.0059(15)
C11 0.056(2) 0.0326(19) 0.032(2) 0.0076(16) -0.0113(18) 0.0001(17)
C12 0.056(2) 0.034(2) 0.033(2) 0.0073(17) 0.0057(17) -0.0137(18)
C13 0.0223(15) 0.0232(16) 0.0229(17) 0.0001(13) -0.0055(12) 0.0017(12)
C14 0.0259(17) 0.0282(17) 0.037(2) -0.0012(15) -0.0021(15) 0.0042(14)
C15 0.0302(18) 0.0370(19) 0.032(2) 0.0015(16) -0.0101(15) -0.0061(15)
C16 0.0305(17) 0.0223(16) 0.0231(17) -0.0023(13) 0.0013(13) -0.0007(13)
C17 0.044(2) 0.0342(19) 0.028(2) -0.0084(16) 0.0013(16) -0.0027(16)
C18 0.039(2) 0.038(2) 0.036(2) -0.0142(17) 0.0028(16) 0.0058(16)
C19 0.0227(16) 0.0315(17) 0.0299(19) -0.0104(15) 0.0070(14) -0.0027(13)
C20 0.0342(19) 0.0352(19) 0.043(2) -0.0179(17) 0.0124(16) -0.0088(15)
C21 0.0233(18) 0.062(3) 0.064(3) -0.021(2) 0.0104(18) -0.0026(18)
C22 0.047(2) 0.042(2) 0.0231(19) -0.0045(16) 0.0055(15) -0.0171(17)
C23 0.047(2) 0.059(3) 0.023(2) -0.0049(18) -0.0014(16) -0.0106(19)
C24 0.057(3) 0.079(3) 0.032(2) -0.016(2) 0.0200(19) -0.035(2)
C25 0.0319(18) 0.0305(18) 0.0286(19) -0.0053(15) 0.0014(14) -0.0138(14)
C26 0.054(3) 0.066(3) 0.041(2) -0.005(2) 0.0026(19) -0.046(2)
C27 0.0262(18) 0.044(2) 0.037(2) -0.0080(17) -0.0034(15) -0.0086(15)
C28 0.0240(16) 0.0213(16) 0.042(2) -0.0028(15) -0.0048(14) 0.0037(13)
C29 0.0311(19) 0.0311(19) 0.048(2) -0.0023(17) -0.0148(16) 0.0007(15)
C30 0.0259(18) 0.039(2) 0.064(3) -0.0079(19) 0.0001(17) 0.0081(16)
C31 0.0349(18) 0.0189(15) 0.0246(18) -0.0013(13) 0.0003(14) -0.0008(13)
C32 0.0389(19) 0.0320(18) 0.0254(19) -0.0055(15) -0.0043(15) -0.0032(15)
C33 0.053(2) 0.0253(18) 0.037(2) -0.0073(16) -0.0009(18) 0.0035(16)
C34 0.055(2) 0.0227(17) 0.0260(19) 0.0033(14) -0.0070(16) -0.0028(15)
C35 0.062(3) 0.0277(19) 0.040(2) 0.0107(17) 0.0018(19) -0.0094(17)
C36 0.064(3) 0.0271(19) 0.045(2) 0.0066(17) -0.018(2) 0.0025(17)
Tm2 0.01827(7) 0.01603(7) 0.02000(8) 0.00012(5) -0.00414(5) -0.00183(5)
Si5 0.0166(4) 0.0176(4) 0.0208(4) 0.0000(3) -0.0016(3) -0.0013(3)
Si6 0.0200(4) 0.0197(4) 0.0168(4) -0.0018(3) -0.0012(3) -0.0018(3)
Si7 0.0227(4) 0.0189(4) 0.0202(5) 0.0017(3) -0.0052(3) -0.0053(3)
Si8 0.0260(4) 0.0170(4) 0.0245(5) -0.0021(3) -0.0038(4) 0.0012(3)
N3 0.0186(12) 0.0175(12) 0.0198(14) -0.0013(10) -0.0030(10) 0.0002(10)
N4 0.0198(12) 0.0165(12) 0.0217(14) 0.0012(10) -0.0014(10) -0.0014(10)
C04F 0.040(2) 0.045(2) 0.042(2) -0.0023(18) -0.0038(17) -0.0233(18)
C37 0.0264(16) 0.0192(15) 0.0254(18) -0.0016(13) -0.0033(13) -0.0003(12)
C38 0.0310(18) 0.0220(16) 0.035(2) -0.0013(14) -0.0047(15) 0.0013(13)
C39 0.0349(19) 0.0230(17) 0.043(2) -0.0023(15) -0.0079(16) -0.0050(14)
C40 0.0200(15) 0.0247(16) 0.0219(17) 0.0028(13) -0.0011(12) -0.0023(12)
C41 0.0347(19) 0.0294(18) 0.030(2) 0.0073(15) -0.0006(15) -0.0087(15)
C42 0.0282(17) 0.0294(17) 0.0247(18) -0.0028(14) 0.0068(14) -0.0069(14)
C43 0.0171(15) 0.0264(16) 0.0304(19) 0.0038(14) 0.0000(13) -0.0037(12)
C44 0.0226(17) 0.040(2) 0.040(2) 0.0000(17) -0.0067(15) -0.0013(15)
C45 0.0220(17) 0.0347(19) 0.050(2) -0.0053(17) -0.0018(16) 0.0059(14)
C46 0.0191(15) 0.0258(16) 0.0207(17) -0.0036(13) -0.0005(12) -0.0017(12)
C47 0.0219(16) 0.0329(18) 0.0282(19) -0.0044(14) -0.0021(13) 0.0043(13)
C48 0.0251(18) 0.045(2) 0.037(2) 0.0061(17) 0.0050(15) -0.0051(15)
C49 0.0308(18) 0.044(2) 0.032(2) -0.0158(17) 0.0071(15) -0.0095(15)
C50 0.054(3) 0.048(2) 0.042(3) -0.0160(19) -0.0043(19) 0.0060(19)
C51 0.044(2) 0.044(2) 0.029(2) -0.0138(17) -0.0018(16) -0.0135(17)
C52 0.0268(16) 0.0260(16) 0.0274(18) 0.0040(14) -0.0077(13) -0.0022(13)
C53 0.041(2) 0.043(2) 0.030(2) 0.0116(17) -0.0071(16) -0.0062(17)
C54 0.0301(18) 0.039(2) 0.043(2) 0.0145(17) -0.0066(16) 0.0065(15)
C55 0.0245(16) 0.0229(15) 0.0231(17) 0.0012(13) -0.0077(13) -0.0009(12)
C56 0.0316(18) 0.0216(16) 0.036(2) 0.0044(14) -0.0101(15) -0.0017(13)
C57 0.0269(17) 0.0310(18) 0.047(2) -0.0008(17) -0.0116(16) -0.0029(14)
C58 0.046(2) 0.045(2) 0.029(2) 0.0039(17) -0.0168(17) -0.0117(17)
C59 0.048(2) 0.044(2) 0.024(2) -0.0023(16) 0.0003(16) -0.0090(17)
C60 0.0391(19) 0.0288(17) 0.0205(17) -0.0007(14) -0.0068(14) -0.0078(14)
C61 0.0285(17) 0.0298(17) 0.0314(19) 0.0052(15) -0.0041(14) -0.0115(14)
C63 0.0325(19) 0.051(2) 0.034(2) 0.0053(17) 0.0012(15) -0.0152(17)
C64 0.0264(17) 0.0277(17) 0.041(2) -0.0090(15) -0.0016(15) 0.0034(14)
C65 0.034(2) 0.036(2) 0.047(2) -0.0107(17) 0.0096(17) -0.0011(16)
C66 0.030(2) 0.047(2) 0.063(3) -0.010(2) -0.0073(18) 0.0109(17)
C67 0.0356(18) 0.0231(16) 0.0277(19) 0.0005(14) -0.0095(14) -0.0005(14)
C68 0.045(2) 0.0318(19) 0.028(2) 0.0083(15) -0.0054(16) -0.0048(16)
C69 0.068(3) 0.0274(19) 0.041(2) 0.0061(17) -0.014(2) 0.0103(18)
C70 0.049(2) 0.0221(16) 0.0274(19) -0.0052(14) -0.0067(16) 0.0022(15)
C71 0.055(2) 0.0264(19) 0.052(3) -0.0139(18) 0.000(2) 0.0071(17)
C72 0.057(2) 0.0263(18) 0.042(2) -0.0089(17) -0.0149(19) -0.0059(17)
Cl1 0.0386(6) 0.1324(12) 0.0532(8) 0.0136(8) -0.0059(5) 0.0052(7)
Cl2 0.0410(6) 0.0694(8) 0.0824(9) 0.0170(7) 0.0036(6) 0.0146(5)
C123 0.047(2) 0.062(3) 0.046(3) -0.001(2) -0.0089(19) 0.024(2)
Cl3 0.0715(8) 0.0760(8) 0.0806(10) -0.0037(7) 0.0212(7) -0.0171(7)
C124 0.051(2) 0.088(3) 0.050(3) 0.005(3) 0.007(2) 0.023(2)
Cl4B 0.055(2) 0.041(3) 0.061(5) 0.0028(18) 0.006(3) 0.0087(18)
Cl4A 0.0537(19) 0.050(3) 0.179(9) 0.026(5) -0.032(3) -0.0047(16)
F00F 0.0243(9) 0.0229(9) 0.0335(11) 0.0026(8) 0.0094(8) 0.0033(7)
F00H 0.0294(10) 0.0216(9) 0.0306(11) 0.0040(8) -0.0006(8) 0.0039(7)
F00L 0.0377(11) 0.0276(10) 0.0373(12) 0.0092(9) 0.0102(9) -0.0009(8)
F00M 0.0217(9) 0.0342(10) 0.0277(11) 0.0084(8) -0.0056(7) -0.0012(8)
F00O 0.0237(9) 0.0253(9) 0.0342(11) 0.0019(8) 0.0090(8) 0.0030(7)
F00P 0.0387(11) 0.0185(9) 0.0465(13) 0.0063(9) 0.0014(9) 0.0051(8)
F00Q 0.0342(11) 0.0336(11) 0.0366(12) 0.0172(9) 0.0009(9) -0.0021(8)
F00S 0.0281(10) 0.0336(10) 0.0276(11) -0.0082(8) 0.0032(8) 0.0034(8)
F00T 0.0250(9) 0.0374(11) 0.0260(10) 0.0054(8) -0.0076(8) -0.0006(8)
F00U 0.0193(9) 0.0339(10) 0.0333(11) -0.0053(8) 0.0050(8) -0.0008(8)
F00Y 0.0192(9) 0.0388(11) 0.0488(13) -0.0025(10) -0.0088(8) -0.0044(8)
F00Z 0.0424(12) 0.0471(12) 0.0219(11) -0.0086(9) -0.0011(9) -0.0090(9)
F01C 0.0171(9) 0.0469(12) 0.0622(15) -0.0021(11) -0.0036(9) -0.0037(9)
F01D 0.0240(10) 0.0342(11) 0.0547(14) 0.0093(10) 0.0080(9) -0.0081(8)
F01E 0.0410(12) 0.0399(12) 0.0596(15) -0.0054(11) -0.0268(11) -0.0086(10)
F01J 0.0553(13) 0.0384(12) 0.0317(12) -0.0132(9) -0.0108(10) -0.0028(10)
F01K 0.0504(13) 0.0353(11) 0.0431(13) -0.0224(10) 0.0098(10) -0.0059(10)
F011 0.0367(11) 0.0299(10) 0.0249(11) 0.0005(8) -0.0067(8) 0.0053(8)
F014 0.0255(10) 0.0246(10) 0.0450(13) -0.0019(9) 0.0051(8) 0.0085(8)
F019 0.0468(12) 0.0207(10) 0.0528(14) -0.0048(9) 0.0068(10) 0.0091(9)
C73 0.0159(14) 0.0211(15) 0.0247(17) -0.0007(12) 0.0009(12) -0.0038(11)
C74 0.0191(15) 0.0216(15) 0.0286(17) -0.0020(13) -0.0006(13) -0.0013(12)
C75 0.0245(16) 0.0334(17) 0.0250(18) -0.0044(14) 0.0016(13) -0.0113(13)
C76 0.0276(17) 0.0272(17) 0.0344(19) -0.0129(14) 0.0075(14) -0.0099(13)
C77 0.0232(16) 0.0182(15) 0.042(2) -0.0039(14) 0.0061(14) -0.0038(12)
C78 0.0166(15) 0.0232(15) 0.0272(17) 0.0009(13) 0.0024(12) -0.0033(12)
C79 0.0188(14) 0.0211(15) 0.0192(16) -0.0012(12) -0.0043(12) 0.0015(11)
C80 0.0201(15) 0.0230(15) 0.0206(17) -0.0024(12) 0.0006(12) 0.0021(12)
C81 0.0274(16) 0.0218(15) 0.0252(18) 0.0000(13) 0.0009(13) -0.0036(12)
C82 0.0268(16) 0.0176(15) 0.0283(18) 0.0025(13) -0.0064(13) 0.0018(12)
C83 0.0205(15) 0.0220(15) 0.0263(18) -0.0038(13) -0.0027(12) 0.0042(12)
C84 0.0190(14) 0.0243(15) 0.0192(16) 0.0001(12) -0.0013(12) -0.0021(12)
C85 0.0182(14) 0.0185(14) 0.0213(16) -0.0022(12) 0.0002(12) 0.0014(11)
C86 0.0204(15) 0.0246(16) 0.0211(17) -0.0009(13) -0.0006(12) 0.0023(12)
C87 0.0175(15) 0.0212(15) 0.0365(19) -0.0066(14) -0.0031(13) 0.0026(12)
C88 0.0201(15) 0.0212(16) 0.038(2) -0.0013(14) 0.0063(13) -0.0031(12)
C89 0.0253(16) 0.0201(15) 0.0267(18) 0.0031(13) 0.0042(13) 0.0039(12)
C90 0.0179(14) 0.0195(15) 0.0255(17) -0.0011(12) -0.0031(12) 0.0027(12)
C91 0.0222(15) 0.0136(14) 0.0239(17) 0.0036(12) -0.0039(12) -0.0021(11)
C92 0.0236(15) 0.0199(15) 0.0272(18) 0.0015(13) -0.0005(13) -0.0020(12)
C93 0.0197(15) 0.0263(17) 0.042(2) 0.0052(15) -0.0045(14) -0.0044(13)
C94 0.0312(17) 0.0200(16) 0.041(2) 0.0017(14) -0.0176(14) -0.0067(13)
C95 0.0377(18) 0.0192(15) 0.0259(18) -0.0023(13) -0.0082(14) -0.0005(13)
C96 0.0237(16) 0.0190(15) 0.0267(17) 0.0024(13) -0.0016(13) 0.0012(12)
B1 0.0182(16) 0.0201(16) 0.0204(18) 0.0014(14) 0.0004(13) 0.0009(13)
F00G 0.0326(10) 0.0229(9) 0.0251(10) -0.0032(8) -0.0005(8) 0.0015(8)
F00I 0.0225(9) 0.0354(10) 0.0299(11) -0.0112(8) 0.0025(8) -0.0030(8)
F00J 0.0232(9) 0.0329(10) 0.0314(11) 0.0001(8) -0.0075(8) -0.0010(8)
F00K 0.0257(9) 0.0284(10) 0.0321(11) -0.0049(8) -0.0120(8) 0.0007(8)
F00N 0.0277(10) 0.0372(11) 0.0262(11) -0.0040(8) 0.0051(8) -0.0053(8)
F00R 0.0246(9) 0.0352(10) 0.0295(11) 0.0064(8) -0.0050(8) -0.0005(8)
F00V 0.0223(9) 0.0278(10) 0.0359(11) -0.0069(8) -0.0107(8) 0.0030(7)
F00W 0.0359(11) 0.0312(10) 0.0232(10) -0.0009(8) 0.0042(8) 0.0045(8)
F00X 0.0185(9) 0.0415(12) 0.0584(15) -0.0012(10) 0.0004(9) -0.0045(8)
F01A 0.0349(11) 0.0452(12) 0.0434(13) -0.0254(10) -0.0045(9) -0.0039(9)
F01B 0.0476(12) 0.0396(12) 0.0304(12) 0.0113(9) 0.0013(9) -0.0067(10)
F01F 0.0385(11) 0.0346(11) 0.0408(13) 0.0163(9) -0.0123(9) -0.0053(9)
F01L 0.0349(11) 0.0324(11) 0.0528(14) 0.0028(10) 0.0187(10) -0.0079(9)
F010 0.0325(11) 0.0348(11) 0.0399(12) -0.0186(9) -0.0106(9) -0.0006(8)
F012 0.0258(10) 0.0324(10) 0.0418(12) -0.0046(9) -0.0061(8) 0.0095(8)
F013 0.0325(10) 0.0445(12) 0.0226(10) 0.0050(9) -0.0023(8) -0.0072(9)
F015 0.0239(10) 0.0448(12) 0.0427(13) 0.0036(10) 0.0041(9) -0.0097(9)
F016 0.0401(11) 0.0283(10) 0.0419(13) -0.0163(9) -0.0050(9) 0.0098(9)
F017 0.0399(11) 0.0219(9) 0.0440(13) -0.0003(9) -0.0089(9) 0.0058(8)
F018 0.0267(10) 0.0478(13) 0.0592(15) -0.0145(11) -0.0083(10) -0.0155(9)
C98 0.0183(15) 0.0233(16) 0.0280(18) -0.0008(13) -0.0004(12) -0.0018(12)
C99 0.0297(17) 0.0217(16) 0.0307(19) -0.0057(14) -0.0058(14) -0.0007(13)
C100 0.0216(16) 0.0247(16) 0.042(2) -0.0007(15) -0.0093(14) -0.0068(13)
C101 0.0189(15) 0.0240(16) 0.0357(19) 0.0067(14) -0.0006(13) -0.0028(12)
C102 0.0241(15) 0.0188(15) 0.0226(17) 0.0011(13) -0.0018(12) -0.0010(12)
C103 0.0206(15) 0.0174(14) 0.0245(17) 0.0026(12) -0.0018(12) -0.0016(12)
C105 0.0186(15) 0.0288(16) 0.0183(16) -0.0012(13) -0.0022(12) -0.0049(12)
C106 0.0197(15) 0.0269(16) 0.0255(18) 0.0018(13) -0.0003(13) 0.0019(12)
C107 0.0290(16) 0.0220(15) 0.0238(18) -0.0047(13) 0.0049(13) 0.0018(13)
C108 0.0235(16) 0.0268(16) 0.0225(17) -0.0049(13) -0.0036(13) -0.0046(12)
C109 0.0183(14) 0.0231(15) 0.0241(17) -0.0001(13) -0.0022(12) -0.0012(12)
C110 0.0202(15) 0.0225(15) 0.0186(16) 0.0027(12) 0.0010(12) -0.0039(12)
C111 0.0177(14) 0.0218(15) 0.0233(16) -0.0002(12) -0.0024(12) -0.0051(12)
C112 0.0210(15) 0.0241(16) 0.0278(17) -0.0023(13) -0.0020(13) -0.0050(12)
C113 0.0209(16) 0.0360(18) 0.0227(17) 0.0026(14) -0.0020(13) -0.0099(13)
C114 0.0242(16) 0.0259(16) 0.0308(18) 0.0108(14) -0.0100(13) -0.0094(13)
C115 0.0208(15) 0.0194(15) 0.0370(19) 0.0010(13) -0.0061(13) -0.0046(12)
C116 0.0210(15) 0.0205(15) 0.0265(17) -0.0021(13) -0.0034(13) -0.0059(12)
C117 0.0240(15) 0.0162(14) 0.0244(17) -0.0048(12) -0.0015(12) -0.0030(12)
C118 0.0240(15) 0.0198(15) 0.0263(17) -0.0031(13) -0.0034(13) -0.0016(12)
C119 0.0341(17) 0.0203(16) 0.0266(18) 0.0004(13) 0.0018(14) -0.0023(13)
C120 0.0293(17) 0.0182(15) 0.038(2) -0.0026(14) 0.0111(14) -0.0053(13)
C121 0.0189(15) 0.0213(16) 0.041(2) -0.0056(14) -0.0006(13) -0.0043(12)
C122 0.0211(15) 0.0193(15) 0.0285(18) -0.0018(13) -0.0033(13) -0.0008(12)
B2 0.0193(16) 0.0199(16) 0.0227(19) 0.0000(14) -0.0040(14) 0.0008(13)
_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
Tm1 N1 2.156(2) . ?
Tm1 N2 2.156(2) . ?
Tm1 C1 2.850(3) . ?
Tm1 C3 2.827(3) . ?
Tm1 C13 2.835(3) . ?
Tm1 C19 2.731(3) . ?
Tm1 C20 2.775(4) . ?
Si1 N1 1.734(2) . ?
Si1 C1 1.939(3) . ?
Si1 C4 1.891(3) . ?
Si1 C7 1.889(3) . ?
Si2 N1 1.736(3) . ?
Si2 C10 1.891(3) . ?
Si2 C13 1.933(3) . ?
Si2 C16 1.892(3) . ?
Si3 N2 1.753(3) . ?
Si3 C19 1.941(3) . ?
Si3 C22 1.891(4) . ?
Si3 C25 1.902(3) . ?
Si4 N2 1.772(3) . ?
Si4 C28 1.904(3) . ?
Si4 C31 1.895(3) . ?
Si4 C34 1.917(3) . ?
C1 C2 1.543(4) . ?
C1 C3 1.542(4) . ?
C4 C5 1.528(5) . ?
C4 C6 1.546(4) . ?
C7 C8 1.533(5) . ?
C7 C9 1.530(5) . ?
C10 C11 1.537(5) . ?
C10 C12 1.537(5) . ?
C13 C14 1.537(4) . ?
C13 C15 1.548(4) . ?
C16 C17 1.534(5) . ?
C16 C18 1.532(5) . ?
C19 C20 1.544(4) . ?
C19 C21 1.570(5) . ?
C22 C23 1.540(5) . ?
C22 C24 1.535(5) . ?
C25 C26 1.530(5) . ?
C25 C27 1.535(5) . ?
C28 C29 1.532(5) . ?
C28 C30 1.547(5) . ?
C31 C32 1.534(5) . ?
C31 C33 1.541(4) . ?
C34 C35 1.536(5) . ?
C34 C36 1.544(5) . ?
Tm2 N3 2.171(2) . ?
Tm2 N4 2.159(2) . ?
Tm2 C40 2.895(3) . ?
Tm2 C42 2.815(3) . ?
Tm2 C46 2.863(3) . ?
Tm2 C55 2.691(3) . ?
Tm2 C56 2.755(3) . ?
Si5 N3 1.734(2) . ?
Si5 C37 1.899(3) . ?
Si5 C40 1.929(3) . ?
Si5 C43 1.888(3) . ?
Si6 N3 1.728(3) . ?
Si6 C46 1.929(3) . ?
Si6 C49 1.886(3) . ?
Si6 C52 1.896(3) . ?
Si7 N4 1.748(2) . ?
Si7 C55 1.936(3) . ?
Si7 C60 1.897(3) . ?
Si7 C61 1.898(3) . ?
Si8 N4 1.771(2) . ?
Si8 C64 1.910(3) . ?
Si8 C67 1.891(3) . ?
Si8 C70 1.913(3) . ?
C04F C61 1.542(5) . ?
C37 C38 1.535(4) . ?
C37 C39 1.543(4) . ?
C40 C41 1.542(4) . ?
C40 C42 1.550(4) . ?
C43 C44 1.535(5) . ?
C43 C45 1.527(5) . ?
C46 C47 1.545(4) . ?
C46 C48 1.544(4) . ?
C49 C50 1.484(5) . ?
C49 C51 1.532(5) . ?
C52 C53 1.537(5) . ?
C52 C54 1.529(5) . ?
C55 C56 1.547(4) . ?
C55 C57 1.544(4) . ?
C58 C60 1.552(5) . ?
C59 C60 1.531(5) . ?
C61 C63 1.538(5) . ?
C64 C65 1.533(5) . ?
C64 C66 1.533(5) . ?
C67 C68 1.529(5) . ?
C67 C69 1.538(5) . ?
C70 C71 1.544(5) . ?
C70 C72 1.544(5) . ?
Cl1 C123 1.741(4) . ?
Cl2 C123 1.752(4) . ?
Cl3 C124 1.731(4) . ?
C124 Cl4B 1.733(6) . ?
C124 Cl4A 1.713(5) . ?
F00F C84 1.348(3) . ?
F00H C78 1.359(4) . ?
F00L C81 1.344(4) . ?
F00M C90 1.352(3) . ?
F00O C80 1.359(3) . ?
F00P C82 1.345(3) . ?
F00Q C89 1.345(4) . ?
F00S C96 1.347(4) . ?
F00T C86 1.347(4) . ?
F00U C92 1.352(4) . ?
F00Y C87 1.351(3) . ?
F00Z C75 1.338(4) . ?
F01C C93 1.344(4) . ?
F01D C88 1.344(4) . ?
F01E C94 1.344(4) . ?
F01J C95 1.342(4) . ?
F01K C76 1.346(4) . ?
F011 C74 1.355(4) . ?
F014 C83 1.351(4) . ?
F019 C77 1.352(4) . ?
C73 C74 1.379(4) . ?
C73 C78 1.396(4) . ?
C73 B1 1.649(5) . ?
C74 C75 1.379(5) . ?
C75 C76 1.379(5) . ?
C76 C77 1.369(5) . ?
C77 C78 1.372(5) . ?
C79 C80 1.382(4) . ?
C79 C84 1.388(4) . ?
C79 B1 1.658(4) . ?
C80 C81 1.376(4) . ?
C81 C82 1.377(5) . ?
C82 C83 1.363(5) . ?
C83 C84 1.385(4) . ?
C85 C86 1.391(4) . ?
C85 C90 1.376(4) . ?
C85 B1 1.657(4) . ?
C86 C87 1.375(4) . ?
C87 C88 1.370(5) . ?
C88 C89 1.371(4) . ?
C89 C90 1.388(4) . ?
C91 C92 1.383(4) . ?
C91 C96 1.390(5) . ?
C91 B1 1.661(4) . ?
C92 C93 1.387(4) . ?
C93 C94 1.371(5) . ?
C94 C95 1.375(5) . ?
C95 C96 1.378(4) . ?
F00G C116 1.355(4) . ?
F00I C98 1.352(4) . ?
F00J C122 1.353(4) . ?
F00K C105 1.356(3) . ?
F00N C102 1.353(4) . ?
F00R C118 1.353(3) . ?
F00V C109 1.359(3) . ?
F00W C112 1.354(4) . ?
F00X C121 1.344(4) . ?
F01A C99 1.349(4) . ?
F01B C119 1.341(4) . ?
F01F C114 1.344(4) . ?
F01L C120 1.342(4) . ?
F010 C108 1.345(3) . ?
F012 C106 1.341(3) . ?
F013 C113 1.346(4) . ?
F015 C101 1.347(4) . ?
F016 C107 1.342(4) . ?
F017 C115 1.351(4) . ?
F018 C100 1.343(4) . ?
C98 C99 1.387(4) . ?
C98 C103 1.385(5) . ?
C99 C100 1.366(5) . ?
C100 C101 1.373(5) . ?
C101 C102 1.376(4) . ?
C102 C103 1.384(4) . ?
C103 B2 1.662(4) . ?
C105 C106 1.375(4) . ?
C105 C110 1.397(4) . ?
C106 C107 1.371(4) . ?
C107 C108 1.375(4) . ?
C108 C109 1.372(4) . ?
C109 C110 1.390(4) . ?
C110 B2 1.651(4) . ?
C111 C112 1.381(5) . ?
C111 C116 1.397(4) . ?
C111 B2 1.656(4) . ?
C112 C113 1.381(5) . ?
C113 C114 1.376(5) . ?
C114 C115 1.364(5) . ?
C115 C116 1.377(4) . ?
C117 C118 1.390(4) . ?
C117 C122 1.392(4) . ?
C117 B2 1.653(5) . ?
C118 C119 1.381(5) . ?
C119 C120 1.380(5) . ?
C120 C121 1.366(5) . ?
C121 C122 1.385(5) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Tm1 C1 68.05(9) . . ?
N1 Tm1 C3 86.86(9) . . ?
N1 Tm1 C13 67.81(9) . . ?
N1 Tm1 C19 153.20(10) . . ?
N1 Tm1 C20 142.26(10) . . ?
N2 Tm1 N1 125.49(9) . . ?
N2 Tm1 C1 128.32(9) . . ?
N2 Tm1 C3 96.86(9) . . ?
N2 Tm1 C13 103.72(9) . . ?
N2 Tm1 C19 72.43(10) . . ?
N2 Tm1 C20 92.08(10) . . ?
C3 Tm1 C1 31.52(9) . . ?
C3 Tm1 C13 153.61(9) . . ?
C13 Tm1 C1 125.03(9) . . ?
C19 Tm1 C1 119.20(9) . . ?
C19 Tm1 C3 112.45(10) . . ?
C19 Tm1 C13 89.66(10) . . ?
C19 Tm1 C20 32.56(9) . . ?
C20 Tm1 C1 86.64(9) . . ?
C20 Tm1 C3 84.87(10) . . ?
C20 Tm1 C13 110.36(10) . . ?
N1 Si1 C1 102.14(12) . . ?
N1 Si1 C4 113.02(13) . . ?
N1 Si1 C7 117.32(14) . . ?
C4 Si1 C1 106.48(14) . . ?
C7 Si1 C1 110.01(14) . . ?
C7 Si1 C4 107.30(15) . . ?
N1 Si2 C10 114.57(13) . . ?
N1 Si2 C13 101.32(13) . . ?
N1 Si2 C16 111.40(13) . . ?
C10 Si2 C13 108.95(15) . . ?
C10 Si2 C16 113.77(15) . . ?
C16 Si2 C13 105.65(14) . . ?
N2 Si3 C19 104.56(13) . . ?
N2 Si3 C22 112.79(15) . . ?
N2 Si3 C25 110.77(14) . . ?
C22 Si3 C19 108.72(17) . . ?
C22 Si3 C25 112.43(15) . . ?
C25 Si3 C19 107.08(15) . . ?
N2 Si4 C28 105.12(13) . . ?
N2 Si4 C31 110.18(13) . . ?
N2 Si4 C34 114.08(15) . . ?
C28 Si4 C34 108.60(16) . . ?
C31 Si4 C28 105.87(15) . . ?
C31 Si4 C34 112.39(15) . . ?
Si1 N1 Tm1 109.07(12) . . ?
Si1 N1 Si2 137.06(15) . . ?
Si2 N1 Tm1 108.01(11) . . ?
Si3 N2 Tm1 102.84(12) . . ?
Si3 N2 Si4 126.45(14) . . ?
Si4 N2 Tm1 130.70(13) . . ?
Si1 C1 Tm1 80.73(10) . . ?
C2 C1 Tm1 162.2(2) . . ?
C2 C1 Si1 114.0(2) . . ?
C3 C1 Tm1 73.42(16) . . ?
C3 C1 Si1 117.5(2) . . ?
C3 C1 C2 106.0(2) . . ?
C1 C3 Tm1 75.06(16) . . ?
C5 C4 Si1 112.7(2) . . ?
C5 C4 C6 109.3(3) . . ?
C6 C4 Si1 115.7(2) . . ?
C8 C7 Si1 112.4(2) . . ?
C9 C7 Si1 117.3(2) . . ?
C9 C7 C8 108.6(3) . . ?
C11 C10 Si2 116.7(2) . . ?
C11 C10 C12 109.4(3) . . ?
C12 C10 Si2 110.5(2) . . ?
Si2 C13 Tm1 80.57(10) . . ?
C14 C13 Tm1 82.80(18) . . ?
C14 C13 Si2 112.0(2) . . ?
C14 C13 C15 109.9(3) . . ?
C15 C13 Tm1 150.3(2) . . ?
C15 C13 Si2 116.3(2) . . ?
C17 C16 Si2 116.7(2) . . ?
C18 C16 Si2 113.3(2) . . ?
C18 C16 C17 109.9(3) . . ?
Si3 C19 Tm1 80.09(11) . . ?
C20 C19 Tm1 75.30(18) . . ?
C20 C19 Si3 118.1(2) . . ?
C20 C19 C21 105.9(3) . . ?
C21 C19 Tm1 160.4(3) . . ?
C21 C19 Si3 114.8(2) . . ?
C19 C20 Tm1 72.13(18) . . ?
C23 C22 Si3 114.8(2) . . ?
C24 C22 Si3 114.8(3) . . ?
C24 C22 C23 108.0(3) . . ?
C26 C25 Si3 116.1(2) . . ?
C26 C25 C27 109.7(3) . . ?
C27 C25 Si3 115.2(2) . . ?
C29 C28 Si4 114.8(2) . . ?
C29 C28 C30 109.1(3) . . ?
C30 C28 Si4 117.7(2) . . ?
C32 C31 Si4 116.2(2) . . ?
C32 C31 C33 108.5(3) . . ?
C33 C31 Si4 116.8(2) . . ?
C35 C34 Si4 116.6(2) . . ?
C35 C34 C36 108.5(3) . . ?
C36 C34 Si4 112.3(3) . . ?
N3 Tm2 C40 67.10(9) . . ?
N3 Tm2 C42 86.45(9) . . ?
N3 Tm2 C46 66.65(9) . . ?
N3 Tm2 C55 152.74(10) . . ?
N3 Tm2 C56 139.89(9) . . ?
N4 Tm2 N3 127.93(9) . . ?
N4 Tm2 C40 128.41(9) . . ?
N4 Tm2 C42 96.99(9) . . ?
N4 Tm2 C46 104.17(9) . . ?
N4 Tm2 C55 72.56(9) . . ?
N4 Tm2 C56 91.70(9) . . ?
C42 Tm2 C40 31.46(9) . . ?
C42 Tm2 C46 152.44(9) . . ?
C46 Tm2 C40 124.36(9) . . ?
C55 Tm2 C40 117.17(9) . . ?
C55 Tm2 C42 110.73(10) . . ?
C55 Tm2 C46 92.55(9) . . ?
C55 Tm2 C56 32.97(9) . . ?
C56 Tm2 C40 84.22(9) . . ?
C56 Tm2 C42 82.20(10) . . ?
C56 Tm2 C46 114.16(10) . . ?
N3 Si5 C37 112.36(13) . . ?
N3 Si5 C40 102.75(12) . . ?
N3 Si5 C43 116.85(13) . . ?
C37 Si5 C40 106.72(14) . . ?
C43 Si5 C37 107.68(14) . . ?
C43 Si5 C40 109.98(14) . . ?
N3 Si6 C46 101.01(13) . . ?
N3 Si6 C49 121.55(15) . . ?
N3 Si6 C52 112.19(14) . . ?
C49 Si6 C46 108.84(15) . . ?
C49 Si6 C52 106.77(17) . . ?
C52 Si6 C46 105.23(14) . . ?
N4 Si7 C55 103.83(12) . . ?
N4 Si7 C60 113.48(14) . . ?
N4 Si7 C61 111.25(14) . . ?
C60 Si7 C55 109.71(15) . . ?
C60 Si7 C61 111.28(15) . . ?
C61 Si7 C55 106.80(15) . . ?
N4 Si8 C64 104.83(13) . . ?
N4 Si8 C67 109.52(14) . . ?
N4 Si8 C70 114.29(14) . . ?
C64 Si8 C70 109.47(16) . . ?
C67 Si8 C64 106.07(15) . . ?
C67 Si8 C70 112.10(15) . . ?
Si5 N3 Tm2 109.67(12) . . ?
Si6 N3 Tm2 108.49(12) . . ?
Si6 N3 Si5 137.75(15) . . ?
Si7 N4 Tm2 102.57(11) . . ?
Si7 N4 Si8 127.07(14) . . ?
Si8 N4 Tm2 130.35(13) . . ?
C38 C37 Si5 113.1(2) . . ?
C38 C37 C39 109.2(3) . . ?
C39 C37 Si5 116.3(2) . . ?
Si5 C40 Tm2 80.48(10) . . ?
C41 C40 Tm2 165.5(2) . . ?
C41 C40 Si5 112.4(2) . . ?
C41 C40 C42 106.1(3) . . ?
C42 C40 Tm2 71.45(16) . . ?
C42 C40 Si5 118.2(2) . . ?
C40 C42 Tm2 77.09(17) . . ?
C44 C43 Si5 112.6(2) . . ?
C45 C43 Si5 116.1(2) . . ?
C45 C43 C44 109.7(3) . . ?
Si6 C46 Tm2 80.42(10) . . ?
C47 C46 Tm2 81.15(18) . . ?
C47 C46 Si6 114.6(2) . . ?
C48 C46 Tm2 153.8(2) . . ?
C48 C46 Si6 114.9(2) . . ?
C48 C46 C47 108.5(3) . . ?
C50 C49 Si6 123.0(3) . . ?
C50 C49 C51 110.2(3) . . ?
C51 C49 Si6 113.1(2) . . ?
C53 C52 Si6 116.3(2) . . ?
C54 C52 Si6 115.1(2) . . ?
C54 C52 C53 109.6(3) . . ?
Si7 C55 Tm2 80.99(10) . . ?
C56 C55 Tm2 75.79(16) . . ?
C56 C55 Si7 117.5(2) . . ?
C57 C55 Tm2 160.5(2) . . ?
C57 C55 Si7 113.0(2) . . ?
C57 C55 C56 107.0(3) . . ?
C55 C56 Tm2 71.24(16) . . ?
C58 C60 Si7 114.2(3) . . ?
C59 C60 Si7 114.6(2) . . ?
C59 C60 C58 108.7(3) . . ?
C04F C61 Si7 115.9(2) . . ?
C63 C61 Si7 115.4(2) . . ?
C63 C61 C04F 109.5(3) . . ?
C65 C64 Si8 114.5(2) . . ?
C66 C64 Si8 117.1(3) . . ?
C66 C64 C65 109.5(3) . . ?
C68 C67 Si8 116.0(2) . . ?
C68 C67 C69 108.2(3) . . ?
C69 C67 Si8 117.3(3) . . ?
C71 C70 Si8 112.5(2) . . ?
C71 C70 C72 107.8(3) . . ?
C72 C70 Si8 115.8(3) . . ?
Cl1 C123 Cl2 112.3(2) . . ?
Cl3 C124 Cl4B 112.4(4) . . ?
Cl4A C124 Cl3 115.0(3) . . ?
C74 C73 C78 112.8(3) . . ?
C74 C73 B1 127.4(3) . . ?
C78 C73 B1 119.3(3) . . ?
F011 C74 C73 121.3(3) . . ?
F011 C74 C75 114.4(3) . . ?
C75 C74 C73 124.4(3) . . ?
F00Z C75 C74 120.8(3) . . ?
F00Z C75 C76 119.4(3) . . ?
C74 C75 C76 119.8(3) . . ?
F01K C76 C75 120.8(3) . . ?
F01K C76 C77 120.6(3) . . ?
C77 C76 C75 118.6(3) . . ?
F019 C77 C76 120.1(3) . . ?
F019 C77 C78 120.5(3) . . ?
C76 C77 C78 119.5(3) . . ?
F00H C78 C73 118.8(3) . . ?
F00H C78 C77 116.3(3) . . ?
C77 C78 C73 124.9(3) . . ?
C80 C79 C84 113.4(3) . . ?
C80 C79 B1 119.4(3) . . ?
C84 C79 B1 126.9(3) . . ?
F00O C80 C79 119.2(3) . . ?
F00O C80 C81 115.7(3) . . ?
C81 C80 C79 125.1(3) . . ?
F00L C81 C80 120.9(3) . . ?
F00L C81 C82 120.2(3) . . ?
C80 C81 C82 119.0(3) . . ?
F00P C82 C81 120.1(3) . . ?
F00P C82 C83 121.1(3) . . ?
C83 C82 C81 118.9(3) . . ?
F014 C83 C82 119.7(3) . . ?
F014 C83 C84 120.0(3) . . ?
C82 C83 C84 120.4(3) . . ?
F00F C84 C79 121.4(3) . . ?
F00F C84 C83 115.3(3) . . ?
C83 C84 C79 123.4(3) . . ?
C86 C85 B1 118.7(3) . . ?
C90 C85 C86 113.5(3) . . ?
C90 C85 B1 127.5(3) . . ?
F00T C86 C85 119.1(3) . . ?
F00T C86 C87 116.3(3) . . ?
C87 C86 C85 124.6(3) . . ?
F00Y C87 C86 120.9(3) . . ?
F00Y C87 C88 119.7(3) . . ?
C88 C87 C86 119.4(3) . . ?
F01D C88 C87 121.2(3) . . ?
F01D C88 C89 120.1(3) . . ?
C87 C88 C89 118.7(3) . . ?
F00Q C89 C88 119.8(3) . . ?
F00Q C89 C90 120.2(3) . . ?
C88 C89 C90 120.0(3) . . ?
F00M C90 C85 121.7(3) . . ?
F00M C90 C89 114.5(3) . . ?
C85 C90 C89 123.8(3) . . ?
C92 C91 C96 113.7(3) . . ?
C92 C91 B1 126.4(3) . . ?
C96 C91 B1 119.3(3) . . ?
F00U C92 C91 121.3(3) . . ?
F00U C92 C93 114.8(3) . . ?
C91 C92 C93 123.9(3) . . ?
F01C C93 C92 120.3(3) . . ?
F01C C93 C94 119.9(3) . . ?
C94 C93 C92 119.8(3) . . ?
F01E C94 C93 120.7(3) . . ?
F01E C94 C95 120.6(3) . . ?
C93 C94 C95 118.7(3) . . ?
F01J C95 C94 120.1(3) . . ?
F01J C95 C96 120.2(3) . . ?
C94 C95 C96 119.8(3) . . ?
F00S C96 C91 119.7(3) . . ?
F00S C96 C95 116.3(3) . . ?
C95 C96 C91 124.0(3) . . ?
C73 B1 C79 113.7(3) . . ?
C73 B1 C85 101.8(2) . . ?
C73 B1 C91 113.9(2) . . ?
C79 B1 C91 100.7(2) . . ?
C85 B1 C79 113.6(2) . . ?
C85 B1 C91 113.7(3) . . ?
F00I C98 C99 114.9(3) . . ?
F00I C98 C103 121.3(3) . . ?
C103 C98 C99 123.8(3) . . ?
F01A C99 C98 120.1(3) . . ?
F01A C99 C100 120.2(3) . . ?
C100 C99 C98 119.7(3) . . ?
F018 C100 C99 120.1(3) . . ?
F018 C100 C101 120.7(3) . . ?
C99 C100 C101 119.2(3) . . ?
F015 C101 C100 119.6(3) . . ?
F015 C101 C102 121.2(3) . . ?
C100 C101 C102 119.1(3) . . ?
F00N C102 C101 115.8(3) . . ?
F00N C102 C103 119.5(3) . . ?
C101 C102 C103 124.7(3) . . ?
C98 C103 B2 126.4(3) . . ?
C102 C103 C98 113.4(3) . . ?
C102 C103 B2 120.1(3) . . ?
F00K C105 C106 115.1(3) . . ?
F00K C105 C110 120.8(3) . . ?
C106 C105 C110 124.1(3) . . ?
F012 C106 C105 120.5(3) . . ?
F012 C106 C107 119.4(3) . . ?
C107 C106 C105 120.1(3) . . ?
F016 C107 C106 120.8(3) . . ?
F016 C107 C108 120.4(3) . . ?
C106 C107 C108 118.8(3) . . ?
F010 C108 C107 119.5(3) . . ?
F010 C108 C109 121.4(3) . . ?
C109 C108 C107 119.1(3) . . ?
F00V C109 C108 115.9(3) . . ?
F00V C109 C110 118.8(3) . . ?
C108 C109 C110 125.3(3) . . ?
C105 C110 B2 127.5(3) . . ?
C109 C110 C105 112.5(3) . . ?
C109 C110 B2 120.0(3) . . ?
C112 C111 C116 112.8(3) . . ?
C112 C111 B2 127.1(3) . . ?
C116 C111 B2 119.8(3) . . ?
F00W C112 C111 121.0(3) . . ?
F00W C112 C113 114.6(3) . . ?
C113 C112 C111 124.5(3) . . ?
F013 C113 C112 120.2(3) . . ?
F013 C113 C114 120.1(3) . . ?
C114 C113 C112 119.7(3) . . ?
F01F C114 C113 120.4(3) . . ?
F01F C114 C115 120.9(3) . . ?
C115 C114 C113 118.7(3) . . ?
F017 C115 C114 119.7(3) . . ?
F017 C115 C116 120.5(3) . . ?
C114 C115 C116 119.7(3) . . ?
F00G C116 C111 119.3(3) . . ?
F00G C116 C115 116.2(3) . . ?
C115 C116 C111 124.5(3) . . ?
C118 C117 C122 112.9(3) . . ?
C118 C117 B2 120.0(3) . . ?
C122 C117 B2 126.7(3) . . ?
F00R C118 C117 119.3(3) . . ?
F00R C118 C119 115.9(3) . . ?
C119 C118 C117 124.8(3) . . ?
F01B C119 C118 120.9(3) . . ?
F01B C119 C120 119.9(3) . . ?
C120 C119 C118 119.2(3) . . ?
F01L C120 C119 120.3(3) . . ?
F01L C120 C121 120.6(3) . . ?
C121 C120 C119 119.1(3) . . ?
F00X C121 C120 120.3(3) . . ?
F00X C121 C122 120.0(3) . . ?
C120 C121 C122 119.7(3) . . ?
F00J C122 C117 120.6(3) . . ?
F00J C122 C121 115.0(3) . . ?
C121 C122 C117 124.4(3) . . ?
C110 B2 C103 112.8(2) . . ?
C110 B2 C111 112.9(3) . . ?
C110 B2 C117 101.7(2) . . ?
C111 B2 C103 102.1(2) . . ?
C117 B2 C103 113.9(3) . . ?
C117 B2 C111 113.8(2) . . ?
_shelx_res_file
;
TITL rdpm78_a.res in P-1
rdpm78.res
created by SHELXL-2017/1 at 14:16:00 on 27-Nov-2017
REM Old TITL rdpm78 in P-1 #2
REM SHELXT solution in P-1
REM R1 0.088, Rweak 0.008, Alpha 0.048, Orientation as input
REM Formula found by SHELXT: C113 B4 N8 F44 Si11 Tm2
CELL 0.71073 16.308356 16.801977 25.475123 89.3578 88.4783 88.0167
ZERR 4 0.000284 0.000365 0.000549 0.0018 0.0016 0.0016
LATT 1
SFAC C H B Cl F N Si Tm
UNIT 244 344 4 8 80 8 16 4
SADI 0.01 Cl4A C124 Cl4B C124 Cl3 C124 Cl2 C123 Cl1 C123
DELU 0.008 0.008 Cl3 > Cl4A
RIGU
L.S. 4
PLAN 20
CONN 20 Tm1
FREE Tm1 Si1
FREE Tm1 Si2
FREE Tm1 Si3
CONN 20 Tm2
FREE Tm2 Si7
FREE Tm2 Si6
FREE Tm2 Si5
list 4
fmap 2 53
acta
SHEL 100 0.83
OMIT 3 -3 1
OMIT -10 3 1
OMIT -12 -4 3
OMIT 3 -3 2
OMIT 9 -1 1
OMIT 1 6 1
OMIT -5 4 1
OMIT -2 5 2
OMIT 1 7 3
OMIT 0 -8 1
OMIT -1 8 1
OMIT 2 -8 1
OMIT 4 -4 1
OMIT -2 4 8
REM
REM
REM
WGHT 0.019100 10.948800
FVAR 1.62370 0.40746
TM1 8 0.347044 0.271920 0.358695 11.00000 0.01825 0.01756 =
0.01946 -0.00244 0.00245 -0.00290
SI1 7 0.490884 0.384200 0.321650 11.00000 0.01825 0.02103 =
0.02125 -0.00221 0.00157 -0.00418
SI2 7 0.374907 0.304796 0.237319 11.00000 0.02493 0.01774 =
0.01828 -0.00090 -0.00025 -0.00187
SI3 7 0.243191 0.146875 0.415121 11.00000 0.02347 0.02627 =
0.02057 -0.00440 0.00336 -0.00990
SI4 7 0.404961 0.065290 0.367949 11.00000 0.02560 0.01772 =
0.02241 -0.00018 -0.00324 -0.00101
N1 6 0.424318 0.317281 0.296027 11.00000 0.02034 0.01795 =
0.01760 -0.00092 0.00161 -0.00314
N2 6 0.337588 0.148238 0.380644 11.00000 0.01887 0.02015 =
0.01928 -0.00196 0.00030 -0.00363
C1 1 0.458640 0.384319 0.395447 11.00000 0.01766 0.02239 =
0.02092 -0.00434 -0.00033 -0.00285
AFIX 13
H1 2 0.399132 0.394759 0.396869 11.00000 -1.20000
AFIX 0
C2 1 0.496312 0.451177 0.427056 11.00000 0.03068 0.02559 =
0.02718 -0.00331 -0.00424 -0.00658
AFIX 137
H2A 2 0.555092 0.446036 0.424553 11.00000 -1.50000
H2B 2 0.478650 0.447054 0.463203 11.00000 -1.50000
H2C 2 0.478626 0.502025 0.413072 11.00000 -1.50000
AFIX 0
C3 1 0.474334 0.306791 0.427148 11.00000 0.02598 0.02686 =
0.02770 -0.00298 -0.00297 -0.00529
AFIX 137
H3A 2 0.459029 0.262098 0.406869 11.00000 -1.50000
H3B 2 0.442233 0.308618 0.459277 11.00000 -1.50000
H3C 2 0.531507 0.301401 0.435031 11.00000 -1.50000
AFIX 0
C4 1 0.472468 0.489486 0.296587 11.00000 0.03220 0.02330 =
0.02391 -0.00095 0.00165 -0.00751
AFIX 13
H4 2 0.472423 0.486156 0.258207 11.00000 -1.20000
AFIX 0
C5 1 0.388125 0.524400 0.313290 11.00000 0.03567 0.01868 =
0.03614 -0.00331 -0.00535 0.00003
AFIX 137
H5A 2 0.346644 0.487861 0.304737 11.00000 -1.50000
H5B 2 0.378165 0.574042 0.295150 11.00000 -1.50000
H5C 2 0.386587 0.533229 0.350474 11.00000 -1.50000
AFIX 0
C6 1 0.538971 0.549066 0.309539 11.00000 0.04116 0.02614 =
0.03499 -0.00274 0.00384 -0.01221
AFIX 137
H6A 2 0.542814 0.553140 0.346945 11.00000 -1.50000
H6B 2 0.524490 0.600390 0.294913 11.00000 -1.50000
H6C 2 0.590915 0.530676 0.294804 11.00000 -1.50000
AFIX 0
C7 1 0.604538 0.360017 0.313885 11.00000 0.01583 0.03299 =
0.03758 -0.00701 0.00272 -0.00633
AFIX 13
H7 2 0.631814 0.399169 0.334983 11.00000 -1.20000
AFIX 0
C8 1 0.636430 0.372287 0.257336 11.00000 0.03037 0.04380 =
0.04400 -0.00373 0.01446 -0.00526
AFIX 137
H8A 2 0.616607 0.331287 0.235515 11.00000 -1.50000
H8B 2 0.695348 0.369858 0.256533 11.00000 -1.50000
H8C 2 0.617309 0.423399 0.244541 11.00000 -1.50000
AFIX 0
C9 1 0.635623 0.278310 0.333468 11.00000 0.02077 0.05163 =
0.04470 0.00334 0.00317 0.00537
AFIX 137
H9A 2 0.621412 0.272328 0.370076 11.00000 -1.50000
H9B 2 0.694184 0.273943 0.328658 11.00000 -1.50000
H9C 2 0.610781 0.237386 0.313958 11.00000 -1.50000
AFIX 0
C10 1 0.371984 0.395874 0.193060 11.00000 0.04707 0.02109 =
0.02281 0.00103 -0.00326 -0.00590
AFIX 13
H10 2 0.367601 0.442174 0.216148 11.00000 -1.20000
AFIX 0
C11 1 0.300081 0.404137 0.155386 11.00000 0.05603 0.03258 =
0.03248 0.00765 -0.01131 0.00013
AFIX 137
H11A 2 0.299181 0.357658 0.133860 11.00000 -1.50000
H11B 2 0.306713 0.450427 0.133456 11.00000 -1.50000
H11C 2 0.249425 0.409488 0.175303 11.00000 -1.50000
AFIX 0
C12 1 0.453400 0.402315 0.161721 11.00000 0.05614 0.03405 =
0.03318 0.00729 0.00565 -0.01374
AFIX 137
H12A 2 0.498227 0.399931 0.185427 11.00000 -1.50000
H12B 2 0.453489 0.451972 0.142713 11.00000 -1.50000
H12C 2 0.459323 0.359063 0.137456 11.00000 -1.50000
AFIX 0
C13 1 0.264585 0.284149 0.262222 11.00000 0.02231 0.02322 =
0.02288 0.00012 -0.00551 0.00166
AFIX 13
H13 2 0.270253 0.243713 0.290032 11.00000 -1.20000
AFIX 0
C14 1 0.222849 0.357483 0.288427 11.00000 0.02593 0.02816 =
0.03729 -0.00115 -0.00215 0.00425
AFIX 137
H14A 2 0.256106 0.374952 0.316326 11.00000 -1.50000
H14B 2 0.169906 0.343762 0.302437 11.00000 -1.50000
H14C 2 0.216474 0.399529 0.262882 11.00000 -1.50000
AFIX 0
C15 1 0.206751 0.249325 0.221765 11.00000 0.03024 0.03700 =
0.03158 0.00148 -0.01008 -0.00610
AFIX 137
H15A 2 0.201032 0.285698 0.192657 11.00000 -1.50000
H15B 2 0.153890 0.241431 0.238103 11.00000 -1.50000
H15C 2 0.229472 0.199256 0.209451 11.00000 -1.50000
AFIX 0
C16 1 0.412975 0.210687 0.203061 11.00000 0.03052 0.02229 =
0.02308 -0.00230 0.00127 -0.00070
AFIX 13
H16 2 0.388490 0.166983 0.223103 11.00000 -1.20000
AFIX 0
C17 1 0.386077 0.200042 0.146387 11.00000 0.04446 0.03423 =
0.02829 -0.00839 0.00126 -0.00269
AFIX 137
H17A 2 0.328799 0.214380 0.143956 11.00000 -1.50000
H17B 2 0.395192 0.145452 0.136422 11.00000 -1.50000
H17C 2 0.417410 0.233634 0.123318 11.00000 -1.50000
AFIX 0
C18 1 0.505923 0.195745 0.206301 11.00000 0.03885 0.03751 =
0.03623 -0.01423 0.00282 0.00584
AFIX 137
H18A 2 0.533634 0.232441 0.183413 11.00000 -1.50000
H18B 2 0.519922 0.142191 0.195776 11.00000 -1.50000
H18C 2 0.522451 0.203240 0.241744 11.00000 -1.50000
AFIX 0
C19 1 0.199751 0.255667 0.410509 11.00000 0.02271 0.03151 =
0.02988 -0.01043 0.00704 -0.00275
AFIX 13
H19 2 0.205260 0.270946 0.373377 11.00000 -1.20000
AFIX 0
C20 1 0.242925 0.320388 0.441044 11.00000 0.03425 0.03516 =
0.04310 -0.01785 0.01241 -0.00876
AFIX 137
H20A 2 0.301280 0.313669 0.435951 11.00000 -1.50000
H20B 2 0.228979 0.315653 0.477768 11.00000 -1.50000
H20C 2 0.225356 0.372077 0.428395 11.00000 -1.50000
AFIX 0
C21 1 0.105898 0.266490 0.425049 11.00000 0.02331 0.06246 =
0.06442 -0.02109 0.01043 -0.00264
AFIX 137
H21A 2 0.076046 0.226488 0.407836 11.00000 -1.50000
H21B 2 0.086404 0.318328 0.413820 11.00000 -1.50000
H21C 2 0.097860 0.261270 0.462379 11.00000 -1.50000
AFIX 0
C22 1 0.254295 0.118826 0.486746 11.00000 0.04694 0.04215 =
0.02305 -0.00454 0.00554 -0.01713
AFIX 13
H22 2 0.259359 0.060554 0.488086 11.00000 -1.20000
AFIX 0
C23 1 0.331746 0.149231 0.512167 11.00000 0.04698 0.05940 =
0.02331 -0.00493 -0.00138 -0.01058
AFIX 137
H23A 2 0.379347 0.133104 0.491446 11.00000 -1.50000
H23B 2 0.336056 0.127253 0.546971 11.00000 -1.50000
H23C 2 0.328118 0.206292 0.513933 11.00000 -1.50000
AFIX 0
C24 1 0.180018 0.142065 0.522289 11.00000 0.05725 0.07904 =
0.03202 -0.01630 0.01997 -0.03484
AFIX 137
H24A 2 0.176616 0.198882 0.526033 11.00000 -1.50000
H24B 2 0.186181 0.117383 0.556189 11.00000 -1.50000
H24C 2 0.130807 0.124462 0.506872 11.00000 -1.50000
AFIX 0
C25 1 0.168660 0.081691 0.380693 11.00000 0.03192 0.03052 =
0.02860 -0.00532 0.00138 -0.01378
AFIX 13
H25 2 0.202509 0.036625 0.367354 11.00000 -1.20000
AFIX 0
C26 1 0.102592 0.043961 0.415663 11.00000 0.05397 0.06627 =
0.04059 -0.00548 0.00258 -0.04572
AFIX 137
H26A 2 0.127651 0.019022 0.445595 11.00000 -1.50000
H26B 2 0.075216 0.004748 0.396089 11.00000 -1.50000
H26C 2 0.063445 0.084435 0.427249 11.00000 -1.50000
AFIX 0
C27 1 0.129264 0.119253 0.331842 11.00000 0.02621 0.04354 =
0.03667 -0.00803 -0.00339 -0.00859
AFIX 137
H27A 2 0.085809 0.156071 0.342483 11.00000 -1.50000
H27B 2 0.107396 0.078222 0.310931 11.00000 -1.50000
H27C 2 0.169950 0.146957 0.311564 11.00000 -1.50000
AFIX 0
C28 1 0.512409 0.104766 0.373561 11.00000 0.02398 0.02135 =
0.04200 -0.00284 -0.00482 0.00370
AFIX 13
H28 2 0.508344 0.158929 0.358964 11.00000 -1.20000
AFIX 0
C29 1 0.540324 0.115607 0.429894 11.00000 0.03111 0.03111 =
0.04761 -0.00234 -0.01480 0.00074
AFIX 137
H29A 2 0.496289 0.139764 0.450537 11.00000 -1.50000
H29B 2 0.586752 0.149221 0.429649 11.00000 -1.50000
H29C 2 0.555427 0.064629 0.444801 11.00000 -1.50000
AFIX 0
C30 1 0.582696 0.063227 0.341072 11.00000 0.02588 0.03908 =
0.06371 -0.00787 0.00008 0.00806
AFIX 137
H30A 2 0.590802 0.009426 0.353447 11.00000 -1.50000
H30B 2 0.632313 0.091499 0.344878 11.00000 -1.50000
H30C 2 0.568590 0.062981 0.304728 11.00000 -1.50000
AFIX 0
C31 1 0.396775 0.032895 0.297312 11.00000 0.03486 0.01895 =
0.02457 -0.00135 0.00029 -0.00080
AFIX 13
H31 2 0.427788 0.071955 0.276816 11.00000 -1.20000
AFIX 0
C32 1 0.310529 0.037667 0.274616 11.00000 0.03888 0.03200 =
0.02538 -0.00553 -0.00433 -0.00321
AFIX 137
H32A 2 0.277865 -0.003027 0.290450 11.00000 -1.50000
H32B 2 0.314403 0.030016 0.237333 11.00000 -1.50000
H32C 2 0.285348 0.088999 0.281861 11.00000 -1.50000
AFIX 0
C33 1 0.437528 -0.048238 0.282713 11.00000 0.05325 0.02531 =
0.03685 -0.00734 -0.00091 0.00352
AFIX 137
H33A 2 0.491691 -0.052092 0.296594 11.00000 -1.50000
H33B 2 0.440985 -0.052910 0.245190 11.00000 -1.50000
H33C 2 0.405301 -0.090264 0.297257 11.00000 -1.50000
AFIX 0
C34 1 0.392782 -0.021335 0.416812 11.00000 0.05467 0.02273 =
0.02603 0.00334 -0.00703 -0.00281
AFIX 13
H34 2 0.389685 0.002340 0.451821 11.00000 -1.20000
AFIX 0
C35 1 0.315444 -0.070220 0.412233 11.00000 0.06233 0.02772 =
0.03973 0.01066 0.00185 -0.00938
AFIX 137
H35A 2 0.267917 -0.037883 0.422007 11.00000 -1.50000
H35B 2 0.319213 -0.115852 0.435168 11.00000 -1.50000
H35C 2 0.310881 -0.087468 0.376663 11.00000 -1.50000
AFIX 0
C36 1 0.468469 -0.079112 0.416237 11.00000 0.06353 0.02715 =
0.04516 0.00665 -0.01803 0.00249
AFIX 137
H36A 2 0.472767 -0.105781 0.383097 11.00000 -1.50000
H36B 2 0.462656 -0.117751 0.444014 11.00000 -1.50000
H36C 2 0.517058 -0.049736 0.421242 11.00000 -1.50000
AFIX 0
TM2 8 0.820416 0.800559 0.151015 11.00000 0.01827 0.01603 =
0.02000 0.00012 -0.00414 -0.00183
SI5 7 0.967121 0.910357 0.183376 11.00000 0.01658 0.01760 =
0.02077 0.00004 -0.00159 -0.00128
SI6 7 0.859261 0.818643 0.271667 11.00000 0.01996 0.01967 =
0.01682 -0.00177 -0.00116 -0.00178
SI7 7 0.710647 0.686731 0.094629 11.00000 0.02269 0.01893 =
0.02019 0.00169 -0.00524 -0.00533
SI8 7 0.870919 0.594397 0.131178 11.00000 0.02597 0.01696 =
0.02450 -0.00209 -0.00375 0.00119
N3 6 0.901550 0.841144 0.210599 11.00000 0.01858 0.01747 =
0.01984 -0.00130 -0.00303 0.00019
N4 6 0.805684 0.680238 0.124793 11.00000 0.01981 0.01648 =
0.02174 0.00122 -0.00143 -0.00143
C04F 1 0.563455 0.592349 0.096474 11.00000 0.04023 0.04475 =
0.04165 -0.00227 -0.00377 -0.02326
AFIX 137
H04A 2 0.527152 0.636264 0.087400 11.00000 -1.50000
H04B 2 0.533395 0.553314 0.116069 11.00000 -1.50000
H04C 2 0.586502 0.568765 0.065010 11.00000 -1.50000
AFIX 0
C37 1 0.948360 1.013404 0.212121 11.00000 0.02636 0.01917 =
0.02541 -0.00157 -0.00328 -0.00030
AFIX 13
H37 2 0.945371 1.005606 0.250296 11.00000 -1.20000
AFIX 0
C38 1 0.865351 1.051869 0.197197 11.00000 0.03098 0.02201 =
0.03523 -0.00126 -0.00474 0.00127
AFIX 137
H38A 2 0.822513 1.015476 0.205074 11.00000 -1.50000
H38B 2 0.866169 1.064372 0.160328 11.00000 -1.50000
H38C 2 0.855456 1.099816 0.216856 11.00000 -1.50000
AFIX 0
C39 1 1.016399 1.073569 0.201647 11.00000 0.03490 0.02301 =
0.04333 -0.00235 -0.00793 -0.00504
AFIX 137
H39A 2 1.019182 1.086673 0.164881 11.00000 -1.50000
H39B 2 1.068165 1.050458 0.212120 11.00000 -1.50000
H39C 2 1.004189 1.121014 0.221422 11.00000 -1.50000
AFIX 0
C40 1 0.933972 0.916869 0.111305 11.00000 0.02001 0.02470 =
0.02192 0.00280 -0.00110 -0.00227
AFIX 13
H40 2 0.875275 0.931560 0.112190 11.00000 -1.20000
AFIX 0
C41 1 0.977161 0.983334 0.080149 11.00000 0.03468 0.02940 =
0.02952 0.00730 -0.00061 -0.00866
AFIX 137
H41A 2 1.035529 0.974116 0.081093 11.00000 -1.50000
H41B 2 0.962760 1.033945 0.095582 11.00000 -1.50000
H41C 2 0.960079 0.983319 0.044376 11.00000 -1.50000
AFIX 0
C42 1 0.944218 0.841029 0.077349 11.00000 0.02822 0.02943 =
0.02473 -0.00278 0.00682 -0.00691
AFIX 137
H42A 2 0.925534 0.795930 0.097185 11.00000 -1.50000
H42B 2 1.001040 0.832472 0.067500 11.00000 -1.50000
H42C 2 0.912425 0.847711 0.046331 11.00000 -1.50000
AFIX 0
C43 1 1.080730 0.885519 0.186139 11.00000 0.01713 0.02638 =
0.03042 0.00376 0.00001 -0.00368
AFIX 13
H43 2 1.107941 0.928733 0.167182 11.00000 -1.20000
AFIX 0
C44 1 1.112644 0.886642 0.242273 11.00000 0.02261 0.03999 =
0.03993 0.00003 -0.00671 -0.00132
AFIX 137
H44A 2 1.089524 0.843868 0.262392 11.00000 -1.50000
H44B 2 1.096978 0.936515 0.258306 11.00000 -1.50000
H44C 2 1.171387 0.880245 0.241223 11.00000 -1.50000
AFIX 0
C45 1 1.110523 0.808789 0.159115 11.00000 0.02200 0.03470 =
0.04953 -0.00534 -0.00180 0.00587
AFIX 137
H45A 2 1.097077 0.811549 0.122666 11.00000 -1.50000
H45B 2 1.084308 0.764285 0.175490 11.00000 -1.50000
H45C 2 1.168918 0.802284 0.162197 11.00000 -1.50000
AFIX 0
C46 1 0.746642 0.802751 0.254238 11.00000 0.01914 0.02578 =
0.02073 -0.00359 -0.00046 -0.00175
AFIX 13
H46 2 0.748446 0.762587 0.226594 11.00000 -1.20000
AFIX 0
C47 1 0.701572 0.876839 0.230929 11.00000 0.02187 0.03287 =
0.02817 -0.00442 -0.00207 0.00432
AFIX 137
H47A 2 0.731508 0.895209 0.200445 11.00000 -1.50000
H47B 2 0.697788 0.918223 0.256646 11.00000 -1.50000
H47C 2 0.647408 0.863131 0.221209 11.00000 -1.50000
AFIX 0
C48 1 0.692717 0.768833 0.299317 11.00000 0.02513 0.04513 =
0.03744 0.00611 0.00496 -0.00513
AFIX 137
H48A 2 0.692334 0.804148 0.328693 11.00000 -1.50000
H48B 2 0.714579 0.717439 0.309720 11.00000 -1.50000
H48C 2 0.637705 0.763822 0.287569 11.00000 -1.50000
AFIX 0
C49 1 0.861221 0.890723 0.327785 11.00000 0.03077 0.04446 =
0.03194 -0.01576 0.00709 -0.00953
AFIX 13
H49 2 0.837131 0.860137 0.356951 11.00000 -1.20000
AFIX 0
C50 1 0.811340 0.966271 0.329292 11.00000 0.05449 0.04829 =
0.04179 -0.01596 -0.00434 0.00602
AFIX 137
H50A 2 0.754105 0.954631 0.329805 11.00000 -1.50000
H50B 2 0.824189 0.997911 0.298752 11.00000 -1.50000
H50C 2 0.823459 0.995142 0.360293 11.00000 -1.50000
AFIX 0
C51 1 0.947978 0.904438 0.346661 11.00000 0.04444 0.04370 =
0.02921 -0.01382 -0.00179 -0.01346
AFIX 137
H51A 2 0.975205 0.940018 0.322745 11.00000 -1.50000
H51B 2 0.978343 0.854514 0.348036 11.00000 -1.50000
H51C 2 0.944746 0.927376 0.381029 11.00000 -1.50000
AFIX 0
C52 1 0.898692 0.718762 0.297713 11.00000 0.02678 0.02602 =
0.02737 0.00404 -0.00772 -0.00218
AFIX 13
H52 2 0.868262 0.679294 0.278816 11.00000 -1.20000
AFIX 0
C53 1 0.880312 0.701243 0.356126 11.00000 0.04054 0.04337 =
0.02960 0.01159 -0.00708 -0.00620
AFIX 137
H53A 2 0.915446 0.731668 0.377235 11.00000 -1.50000
H53B 2 0.889995 0.645507 0.363167 11.00000 -1.50000
H53C 2 0.824018 0.715614 0.364452 11.00000 -1.50000
AFIX 0
C54 1 0.989043 0.698441 0.284725 11.00000 0.03011 0.03910 =
0.04299 0.01449 -0.00661 0.00649
AFIX 137
H54A 2 1.023010 0.729943 0.305936 11.00000 -1.50000
H54B 2 1.000456 0.709658 0.248278 11.00000 -1.50000
H54C 2 1.000378 0.642966 0.291809 11.00000 -1.50000
AFIX 0
C55 1 0.673982 0.796407 0.105015 11.00000 0.02451 0.02288 =
0.02308 0.00124 -0.00766 -0.00089
AFIX 13
H55 2 0.681448 0.807428 0.142248 11.00000 -1.20000
AFIX 0
C56 1 0.720112 0.861386 0.073880 11.00000 0.03158 0.02162 =
0.03601 0.00437 -0.01007 -0.00167
AFIX 137
H56A 2 0.777891 0.848266 0.073115 11.00000 -1.50000
H56B 2 0.710337 0.911898 0.090570 11.00000 -1.50000
H56C 2 0.700737 0.864321 0.038631 11.00000 -1.50000
AFIX 0
C57 1 0.581656 0.810893 0.095150 11.00000 0.02688 0.03098 =
0.04737 -0.00084 -0.01156 -0.00293
AFIX 137
H57A 2 0.550786 0.771758 0.114093 11.00000 -1.50000
H57B 2 0.572039 0.806797 0.058279 11.00000 -1.50000
H57C 2 0.564726 0.863132 0.106941 11.00000 -1.50000
AFIX 0
C58 1 0.641243 0.695117 -0.009124 11.00000 0.04571 0.04524 =
0.02866 0.00393 -0.01679 -0.01170
AFIX 137
H58A 2 0.641277 0.752168 -0.011637 11.00000 -1.50000
H58B 2 0.591957 0.679149 0.008907 11.00000 -1.50000
H58C 2 0.643655 0.673032 -0.043745 11.00000 -1.50000
AFIX 0
C59 1 0.794776 0.692802 -0.006610 11.00000 0.04840 0.04383 =
0.02351 -0.00227 0.00030 -0.00905
AFIX 137
H59A 2 0.842200 0.671518 0.010941 11.00000 -1.50000
H59B 2 0.794925 0.749926 -0.006300 11.00000 -1.50000
H59C 2 0.795972 0.674766 -0.042255 11.00000 -1.50000
AFIX 0
C60 1 0.716975 0.664401 0.021760 11.00000 0.03913 0.02877 =
0.02051 -0.00065 -0.00681 -0.00776
AFIX 13
H60 2 0.718506 0.606250 0.018895 11.00000 -1.20000
AFIX 0
C61 1 0.633016 0.622387 0.130108 11.00000 0.02846 0.02979 =
0.03145 0.00522 -0.00408 -0.01150
AFIX 13
H61 2 0.664290 0.574205 0.140573 11.00000 -1.20000
AFIX 0
C63 1 0.596442 0.656548 0.181729 11.00000 0.03253 0.05071 =
0.03375 0.00533 0.00122 -0.01524
AFIX 137
H63A 2 0.639011 0.679888 0.201136 11.00000 -1.50000
H63B 2 0.572618 0.614568 0.202247 11.00000 -1.50000
H63C 2 0.554870 0.696508 0.174020 11.00000 -1.50000
AFIX 0
C64 1 0.979404 0.632179 0.121132 11.00000 0.02635 0.02772 =
0.04094 -0.00897 -0.00163 0.00337
AFIX 13
H64 2 0.977781 0.684611 0.137668 11.00000 -1.20000
AFIX 0
C65 1 1.004512 0.648315 0.063662 11.00000 0.03380 0.03643 =
0.04681 -0.01065 0.00960 -0.00111
AFIX 137
H65A 2 0.962026 0.679697 0.047090 11.00000 -1.50000
H65B 2 1.012605 0.598655 0.045664 11.00000 -1.50000
H65C 2 1.054624 0.676696 0.062256 11.00000 -1.50000
AFIX 0
C66 1 1.048831 0.585195 0.148246 11.00000 0.02967 0.04678 =
0.06277 -0.01007 -0.00732 0.01090
AFIX 137
H66A 2 1.035967 0.580603 0.185125 11.00000 -1.50000
H66B 2 1.099202 0.612547 0.143231 11.00000 -1.50000
H66C 2 1.054803 0.533009 0.133365 11.00000 -1.50000
AFIX 0
C67 1 0.864444 0.555593 0.201087 11.00000 0.03564 0.02308 =
0.02772 0.00050 -0.00951 -0.00053
AFIX 13
H67 2 0.896805 0.592229 0.221071 11.00000 -1.20000
AFIX 0
C68 1 0.779266 0.559723 0.227682 11.00000 0.04541 0.03181 =
0.02772 0.00830 -0.00542 -0.00479
AFIX 137
H68A 2 0.745339 0.521037 0.212429 11.00000 -1.50000
H68B 2 0.754884 0.612009 0.222764 11.00000 -1.50000
H68C 2 0.784096 0.548715 0.264551 11.00000 -1.50000
AFIX 0
C69 1 0.903701 0.472775 0.212163 11.00000 0.06787 0.02736 =
0.04103 0.00610 -0.01411 0.01032
AFIX 137
H69A 2 0.957632 0.469265 0.196137 11.00000 -1.50000
H69B 2 0.870456 0.432679 0.197874 11.00000 -1.50000
H69C 2 0.907523 0.464682 0.249394 11.00000 -1.50000
AFIX 0
C70 1 0.852779 0.513089 0.081222 11.00000 0.04887 0.02212 =
0.02742 -0.00522 -0.00669 0.00224
AFIX 13
H70 2 0.846867 0.539790 0.047066 11.00000 -1.20000
AFIX 0
C71 1 0.926491 0.453363 0.075507 11.00000 0.05538 0.02635 =
0.05163 -0.01386 0.00031 0.00705
AFIX 137
H71A 2 0.933966 0.425197 0.108119 11.00000 -1.50000
H71B 2 0.975138 0.481633 0.066504 11.00000 -1.50000
H71C 2 0.916201 0.416123 0.048345 11.00000 -1.50000
AFIX 0
C72 1 0.774827 0.464867 0.090953 11.00000 0.05690 0.02627 =
0.04188 -0.00890 -0.01493 -0.00595
AFIX 137
H72A 2 0.774601 0.421753 0.066551 11.00000 -1.50000
H72B 2 0.727081 0.498951 0.086187 11.00000 -1.50000
H72C 2 0.774334 0.443916 0.126169 11.00000 -1.50000
AFIX 0
CL1 4 0.778725 0.381895 0.763633 11.00000 0.03862 0.13236 =
0.05321 0.01364 -0.00588 0.00524
CL2 4 0.625800 0.375548 0.824088 11.00000 0.04104 0.06944 =
0.08235 0.01701 0.00359 0.01458
C123 1 0.722098 0.329685 0.810651 11.00000 0.04672 0.06217 =
0.04569 -0.00051 -0.00887 0.02376
AFIX 23
H12H 2 0.752591 0.325736 0.842807 11.00000 -1.20000
H12I 2 0.714585 0.276086 0.798312 11.00000 -1.20000
AFIX 0
CL3 4 0.889984 0.178047 0.331757 11.00000 0.07154 0.07599 =
0.08062 -0.00369 0.02124 -0.01715
C124 1 0.896026 0.272601 0.304574 11.00000 0.05087 0.08794 =
0.05025 0.00549 0.00668 0.02285
PART 1
AFIX 23
H12D 2 0.880354 0.311623 0.331097 21.00000 -1.20000
H12E 2 0.857440 0.278300 0.276338 21.00000 -1.20000
AFIX 23
PART 0
PART 2
H12F 2 0.871649 0.272571 0.270255 -21.00000 -1.20000
H12G 2 0.863485 0.309347 0.326384 -21.00000 -1.20000
AFIX 0
PART 0
PART 1
CL4B 4 0.993688 0.291761 0.280250 21.00000 0.05500 0.04082 =
0.06102 0.00278 0.00593 0.00870
PART 0
PART 2
CL4A 4 0.993323 0.307288 0.297736 -21.00000 0.05373 0.04963 =
0.17935 0.02582 -0.03179 -0.00472
PART 0
F00F 5 0.556140 0.270565 0.059632 11.00000 0.02431 0.02292 =
0.03349 0.00264 0.00943 0.00326
F00H 5 0.793160 0.016650 0.032242 11.00000 0.02938 0.02156 =
0.03056 0.00398 -0.00063 0.00393
F00L 5 0.765164 0.420533 -0.073950 11.00000 0.03774 0.02761 =
0.03725 0.00918 0.01024 -0.00092
F00M 5 0.713270 0.073760 0.128605 11.00000 0.02171 0.03415 =
0.02766 0.00842 -0.00556 -0.00125
F00O 5 0.797880 0.269452 -0.047849 11.00000 0.02369 0.02530 =
0.03421 0.00194 0.00901 0.00297
F00P 5 0.627761 0.498436 -0.034846 11.00000 0.03870 0.01848 =
0.04650 0.00633 0.00142 0.00505
F00Q 5 0.591970 -0.007628 0.169148 11.00000 0.03424 0.03359 =
0.03659 0.01719 0.00095 -0.00209
F00S 5 0.696872 0.241507 0.125860 11.00000 0.02809 0.03357 =
0.02758 -0.00823 0.00316 0.00340
F00T 5 0.548216 0.147218 -0.015184 11.00000 0.02500 0.03742 =
0.02595 0.00536 -0.00763 -0.00058
F00U 5 0.893932 0.143990 0.000183 11.00000 0.01931 0.03386 =
0.03334 -0.00533 0.00496 -0.00084
F00Y 5 0.425469 0.065629 0.027420 11.00000 0.01924 0.03878 =
0.04880 -0.00245 -0.00880 -0.00442
F00Z 5 0.703730 0.082319 -0.166616 11.00000 0.04237 0.04708 =
0.02192 -0.00857 -0.00113 -0.00899
F01C 5 1.011939 0.195566 0.058272 11.00000 0.01713 0.04687 =
0.06223 -0.00207 -0.00359 -0.00369
F01D 5 0.446277 -0.014094 0.120603 11.00000 0.02401 0.03420 =
0.05473 0.00930 0.00804 -0.00806
F01E 5 0.977314 0.268841 0.151605 11.00000 0.04096 0.03995 =
0.05962 -0.00539 -0.02676 -0.00856
F01J 5 0.817305 0.288525 0.184717 11.00000 0.05527 0.03838 =
0.03167 -0.01324 -0.01085 -0.00281
F01K 5 0.779992 -0.060089 -0.143223 11.00000 0.05042 0.03530 =
0.04307 -0.02237 0.00979 -0.00586
F011 5 0.670567 0.189207 -0.094080 11.00000 0.03669 0.02993 =
0.02491 0.00046 -0.00670 0.00533
F014 5 0.525033 0.420222 0.032521 11.00000 0.02554 0.02457 =
0.04504 -0.00191 0.00512 0.00846
F019 5 0.824347 -0.090867 -0.042166 11.00000 0.04685 0.02072 =
0.05284 -0.00480 0.00679 0.00914
C73 1 0.731926 0.110217 -0.026482 11.00000 0.01593 0.02106 =
0.02469 -0.00070 0.00087 -0.00380
C74 1 0.709986 0.121291 -0.078035 11.00000 0.01914 0.02157 =
0.02862 -0.00198 -0.00056 -0.00126
C75 1 0.725920 0.066613 -0.117265 11.00000 0.02446 0.03336 =
0.02501 -0.00441 0.00163 -0.01135
C76 1 0.764444 -0.005550 -0.105623 11.00000 0.02759 0.02722 =
0.03439 -0.01290 0.00746 -0.00994
C77 1 0.786632 -0.020664 -0.054913 11.00000 0.02318 0.01819 =
0.04207 -0.00389 0.00612 -0.00383
C78 1 0.769959 0.035814 -0.017288 11.00000 0.01664 0.02323 =
0.02716 0.00089 0.00239 -0.00334
C79 1 0.678250 0.260338 0.006080 11.00000 0.01880 0.02107 =
0.01925 -0.00124 -0.00435 0.00150
C80 1 0.727893 0.304178 -0.027229 11.00000 0.02012 0.02296 =
0.02057 -0.00238 0.00061 0.00209
C81 1 0.712874 0.382467 -0.041524 11.00000 0.02743 0.02181 =
0.02516 -0.00004 0.00089 -0.00364
C82 1 0.643466 0.421738 -0.021781 11.00000 0.02679 0.01764 =
0.02826 0.00253 -0.00640 0.00181
C83 1 0.592437 0.382063 0.011807 11.00000 0.02045 0.02199 =
0.02627 -0.00382 -0.00273 0.00423
C84 1 0.610078 0.303414 0.025465 11.00000 0.01899 0.02433 =
0.01925 0.00013 -0.00127 -0.00207
C85 1 0.636392 0.118583 0.055064 11.00000 0.01817 0.01849 =
0.02134 -0.00220 0.00016 0.00137
C86 1 0.561275 0.110835 0.031384 11.00000 0.02038 0.02458 =
0.02106 -0.00091 -0.00061 0.00228
C87 1 0.497421 0.068386 0.052290 11.00000 0.01745 0.02122 =
0.03648 -0.00660 -0.00313 0.00257
C88 1 0.507265 0.028022 0.098855 11.00000 0.02012 0.02116 =
0.03779 -0.00132 0.00631 -0.00309
C89 1 0.580843 0.031539 0.123398 11.00000 0.02535 0.02010 =
0.02674 0.00312 0.00421 0.00394
C90 1 0.643374 0.075812 0.101188 11.00000 0.01786 0.01954 =
0.02547 -0.00115 -0.00307 0.00274
C91 1 0.788015 0.188130 0.060393 11.00000 0.02224 0.01360 =
0.02390 0.00358 -0.00390 -0.00213
C92 1 0.870077 0.179336 0.045780 11.00000 0.02356 0.01994 =
0.02720 0.00148 -0.00054 -0.00204
C93 1 0.933664 0.205802 0.075417 11.00000 0.01970 0.02627 =
0.04187 0.00524 -0.00446 -0.00442
C94 1 0.916545 0.242886 0.122294 11.00000 0.03116 0.02002 =
0.04060 0.00166 -0.01764 -0.00673
C95 1 0.835901 0.253116 0.138767 11.00000 0.03770 0.01916 =
0.02590 -0.00231 -0.00816 -0.00049
C96 1 0.774324 0.227137 0.107830 11.00000 0.02368 0.01898 =
0.02667 0.00238 -0.00161 0.00119
B1 3 0.708614 0.168876 0.023610 11.00000 0.01825 0.02009 =
0.02039 0.00142 0.00043 0.00090
F00G 5 0.698147 0.496835 0.547816 11.00000 0.03260 0.02294 =
0.02514 -0.00317 -0.00046 0.00153
F00I 5 0.785311 0.440137 0.638391 11.00000 0.02245 0.03544 =
0.02991 -0.01116 0.00254 -0.00301
F00J 5 0.603741 0.366159 0.519448 11.00000 0.02324 0.03290 =
0.03137 0.00015 -0.00749 -0.00103
F00K 5 0.944624 0.245215 0.563196 11.00000 0.02569 0.02842 =
0.03214 -0.00494 -0.01200 0.00072
F00N 5 0.952898 0.369680 0.490244 11.00000 0.02766 0.03715 =
0.02617 -0.00404 0.00511 -0.00527
F00R 5 0.807169 0.271657 0.636402 11.00000 0.02459 0.03522 =
0.02951 0.00642 -0.00496 -0.00052
F00V 5 0.701429 0.250282 0.464764 11.00000 0.02226 0.02781 =
0.03589 -0.00689 -0.01075 0.00296
F00W 5 0.827667 0.336250 0.415733 11.00000 0.03587 0.03120 =
0.02321 -0.00090 0.00416 0.00453
F00X 5 0.489009 0.313949 0.584292 11.00000 0.01848 0.04153 =
0.05843 -0.00121 0.00042 -0.00447
F01A 5 0.908389 0.515371 0.677609 11.00000 0.03492 0.04524 =
0.04336 -0.02540 -0.00447 -0.00388
F01B 5 0.689446 0.222955 0.702353 11.00000 0.04760 0.03962 =
0.03043 0.01128 0.00128 -0.00665
F01F 5 0.705353 0.582234 0.372514 11.00000 0.03846 0.03463 =
0.04079 0.01626 -0.01233 -0.00529
F01L 5 0.528399 0.243837 0.677785 11.00000 0.03490 0.03238 =
0.05276 0.00278 0.01869 -0.00792
F010 5 0.744949 0.107345 0.426605 11.00000 0.03252 0.03479 =
0.03986 -0.01862 -0.01056 -0.00062
F012 5 0.984208 0.103784 0.524944 11.00000 0.02580 0.03243 =
0.04180 -0.00459 -0.00606 0.00946
F013 5 0.787889 0.444209 0.344922 11.00000 0.03251 0.04451 =
0.02262 0.00503 -0.00232 -0.00723
F015 5 1.077078 0.443933 0.531826 11.00000 0.02388 0.04484 =
0.04272 0.00365 0.00408 -0.00966
F016 5 0.888225 0.033435 0.454617 11.00000 0.04014 0.02833 =
0.04193 -0.01626 -0.00501 0.00981
F017 5 0.657999 0.604851 0.474790 11.00000 0.03987 0.02191 =
0.04397 -0.00034 -0.00889 0.00577
F018 5 1.055719 0.519877 0.625387 11.00000 0.02668 0.04785 =
0.05918 -0.01446 -0.00828 -0.01550
C98 1 0.856232 0.437863 0.609655 11.00000 0.01835 0.02330 =
0.02797 -0.00079 -0.00043 -0.00176
C99 1 0.919575 0.478864 0.630945 11.00000 0.02967 0.02165 =
0.03073 -0.00569 -0.00582 -0.00068
C100 1 0.993608 0.481311 0.604731 11.00000 0.02157 0.02473 =
0.04163 -0.00066 -0.00933 -0.00683
C101 1 1.003899 0.442906 0.557588 11.00000 0.01888 0.02405 =
0.03573 0.00667 -0.00063 -0.00279
C102 1 0.939021 0.403820 0.537653 11.00000 0.02409 0.01882 =
0.02260 0.00114 -0.00180 -0.00104
C103 1 0.863374 0.396679 0.562878 11.00000 0.02062 0.01737 =
0.02450 0.00265 -0.00180 -0.00157
C105 1 0.892477 0.215315 0.528473 11.00000 0.01865 0.02879 =
0.01827 -0.00123 -0.00219 -0.00486
C106 1 0.914996 0.141299 0.509346 11.00000 0.01971 0.02688 =
0.02549 0.00179 -0.00032 0.00190
C107 1 0.866359 0.105036 0.474339 11.00000 0.02899 0.02202 =
0.02376 -0.00471 0.00493 0.00178
C108 1 0.794041 0.142893 0.460173 11.00000 0.02345 0.02678 =
0.02249 -0.00486 -0.00356 -0.00464
C109 1 0.773895 0.216589 0.480298 11.00000 0.01826 0.02314 =
0.02411 -0.00012 -0.00215 -0.00119
C110 1 0.821807 0.258621 0.513961 11.00000 0.02022 0.02249 =
0.01864 0.00271 0.00097 -0.00387
C111 1 0.763231 0.408643 0.486191 11.00000 0.01769 0.02181 =
0.02328 -0.00015 -0.00237 -0.00507
C112 1 0.784388 0.401118 0.433569 11.00000 0.02099 0.02408 =
0.02783 -0.00233 -0.00195 -0.00497
C113 1 0.765319 0.457197 0.395376 11.00000 0.02087 0.03598 =
0.02268 0.00258 -0.00199 -0.00992
C114 1 0.723170 0.526559 0.409123 11.00000 0.02415 0.02588 =
0.03077 0.01078 -0.00995 -0.00945
C115 1 0.700585 0.537782 0.460529 11.00000 0.02081 0.01941 =
0.03700 0.00098 -0.00609 -0.00463
C116 1 0.721236 0.480586 0.497467 11.00000 0.02105 0.02051 =
0.02647 -0.00208 -0.00343 -0.00586
C117 1 0.712968 0.324831 0.575053 11.00000 0.02395 0.01617 =
0.02443 -0.00481 -0.00151 -0.00302
C118 1 0.728570 0.285895 0.622352 11.00000 0.02398 0.01981 =
0.02626 -0.00311 -0.00335 -0.00161
C119 1 0.668966 0.259154 0.657146 11.00000 0.03410 0.02031 =
0.02658 0.00041 0.00181 -0.00231
C120 1 0.587454 0.269171 0.644607 11.00000 0.02925 0.01820 =
0.03777 -0.00262 0.01106 -0.00533
C121 1 0.567843 0.304760 0.597913 11.00000 0.01885 0.02131 =
0.04119 -0.00561 -0.00059 -0.00433
C122 1 0.629652 0.331598 0.564580 11.00000 0.02112 0.01934 =
0.02847 -0.00181 -0.00326 -0.00085
B2 3 0.789945 0.347423 0.534679 11.00000 0.01935 0.01992 =
0.02271 0.00002 -0.00398 0.00083
HKLF 4
REM rdpm78_a.res in P-1
REM R1 = 0.0305 for 22123 Fo > 4sig(Fo) and 0.0377 for all 25354 data
REM 1697 parameters refined using 1593 restraints
END
WGHT 0.0191 10.9474
REM Highest difference peak 1.360, deepest hole -0.547, 1-sigma level 0.072
Q1 1 0.3428 0.2812 0.3190 11.00000 0.05 1.36
Q2 1 0.3496 0.2613 0.4006 11.00000 0.05 1.10
Q3 1 0.7789 0.9187 0.3563 11.00000 0.05 1.08
Q4 1 0.8198 0.8067 0.1151 11.00000 0.05 0.89
Q5 1 0.8244 0.7881 0.1939 11.00000 0.05 0.67
Q6 1 0.6113 0.3355 0.7984 11.00000 0.05 0.62
Q7 1 0.4032 0.2957 0.3352 11.00000 0.05 0.53
Q8 1 0.8503 0.9276 0.3012 11.00000 0.05 0.51
Q9 1 0.2868 0.2738 0.3418 11.00000 0.05 0.50
Q10 1 0.7577 0.8024 0.1409 11.00000 0.05 0.50
Q11 1 0.4047 0.2628 0.3610 11.00000 0.05 0.49
Q12 1 0.4815 0.3764 0.3594 11.00000 0.05 0.48
Q13 1 0.8834 0.7993 0.1588 11.00000 0.05 0.46
Q14 1 0.3553 0.2004 0.3773 11.00000 0.05 0.43
Q15 1 0.8459 0.8348 0.2197 11.00000 0.05 0.43
Q16 1 0.9535 0.9161 0.1417 11.00000 0.05 0.42
Q17 1 0.7957 0.8197 0.2608 11.00000 0.05 0.41
Q18 1 0.8604 0.7449 0.1226 11.00000 0.05 0.39
Q19 1 0.7673 0.7809 0.1724 11.00000 0.05 0.39
Q20 1 0.2941 0.3218 0.3623 11.00000 0.05 0.38
;
_shelx_res_checksum 68987
_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 2.027
_oxdiff_exptl_absorpt_empirical_full_min 0.528
#######################################################################
#
# 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_xdpm73
_database_code_depnum_ccdc_archive 'CCDC 1880946'
loop_
_audit_author_name
_audit_author_address
'Hannah Nicholas'
;The University of Manchester
United Kingdom
;
_audit_update_record
;
2018-11-23 deposited with the CCDC. 2019-09-18 downloaded from the CCDC.
;
# end Validation Reply Form
_audit_creation_date 2018-08-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic '[Yb(Ntt)2(F)]'
_chemical_formula_moiety 'C36 H84 F N2 Si4 Yb'
_chemical_formula_sum 'C36 H84 F N2 Si4 Yb'
_chemical_formula_weight 849.45
_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'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -7.2108 4.4329 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.7293(3)
_cell_length_b 11.1712(4)
_cell_length_c 24.4919(8)
_cell_angle_alpha 84.182(3)
_cell_angle_beta 80.590(3)
_cell_angle_gamma 68.517(3)
_cell_volume 2190.28(13)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 12784
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 74.3530
_cell_measurement_theta_min 1.8590
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 5.206
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.32640
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear yellow'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier .
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.288
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 898
_exptl_crystal_preparation ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.05
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0349
_diffrn_reflns_av_unetI/netI 0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 17168
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 68.251
_diffrn_reflns_theta_min 1.830
_diffrn_ambient_temperature 150(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.956
_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 70.71 258.71 1.00 8.00 -- 100.00 73.87 -55.79 188
2 \w 70.71 258.71 1.00 8.00 -- 100.00 73.87 119.21 188
3 \f -171.08 30.04 1.00 8.00 124.98 100.50 73.87 -- 201
4 \w -46.10 111.90 1.00 5.00 -- -25.00 73.87 164.21 158
5 \f -12.99 330.22 1.00 8.00-130.79 111.00 73.87 -- 343
6 \w 72.94 229.94 1.00 5.00 -- 75.00 73.87-175.79 157
7 \w 117.83 225.83 1.00 8.00 -- 111.00 73.87 24.21 108
8 \w -63.01 48.99 1.00 5.00 -- -35.00 73.87 -65.79 112
9 \f 167.02 299.18 1.00 8.00 169.21 112.00 73.87 -- 132
10 \f 110.67 210.73 1.00 8.00 159.16 110.00 73.87 -- 100
11 \w 122.67 227.67 1.00 8.00 -- 112.00 73.87 -5.79 105
12 \w 75.90 160.90 1.00 8.00 -- 105.00 73.87-110.79 85
13 \w 27.14 129.11 1.00 5.00 -- -24.50 73.87 61.71 102
;
_diffrn_measurement_device 'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.1207372000
_diffrn_orient_matrix_UB_12 0.0008768000
_diffrn_orient_matrix_UB_13 -0.0395451000
_diffrn_orient_matrix_UB_21 0.1231654000
_diffrn_orient_matrix_UB_22 0.0180657000
_diffrn_orient_matrix_UB_23 -0.0499814000
_diffrn_orient_matrix_UB_31 0.0831133000
_diffrn_orient_matrix_UB_32 -0.1472470000
_diffrn_orient_matrix_UB_33 -0.0034594000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7366
_reflns_number_total 7685
_reflns_odcompleteness_completeness 90.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 73.97
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XH (Sheldrick, 2008)'
_computing_structure_solution 'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max 1.487
_refine_diff_density_min -1.433
_refine_diff_density_rms 0.108
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.047
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 421
_refine_ls_number_reflns 7685
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0376
_refine_ls_R_factor_gt 0.0355
_refine_ls_restrained_S_all 1.047
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+3.1881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0925
_refine_ls_wR_factor_ref 0.0937
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16), C19(H19), C22(H22),
C25(H25), C28(H28), C31(H31), C34(H34)
2.b Idealised Me refined as rotating group:
C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C8(H8a,
H8b,H8c), C9(H9a,H9b,H9c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C14(H14a,
H14b,H14c), C15(H15a,H15b,H15c), C17(H17a,H17b,H17c), C18(H18a,H18b,H18c),
C20(H20a,H20b,H20c), C21(H21a,H21b,H21c), C23(H23a,H23b,H23c), C24(H24a,H24b,
H24c), C26(H26a,H26b,H26c), C27(H27a,H27b,H27c), C29(H29a,H29b,H29c), C30(H30a,
H30b,H30c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C35(H35a,H35b,H35c),
C36(H36a,H36b,H36c)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.53899(2) 0.31458(2) 0.74480(2) 0.01640(7) Uani 1 1 d . . . . .
Si1 Si 0.78466(11) 0.09457(8) 0.64336(4) 0.01856(18) Uani 1 1 d . . . . .
Si2 Si 0.73812(10) 0.38247(8) 0.62909(3) 0.01518(17) Uani 1 1 d . . . . .
Si3 Si 0.68257(10) 0.18804(8) 0.86634(3) 0.01498(17) Uani 1 1 d . . . . .
Si4 Si 0.43165(10) 0.47573(8) 0.85872(3) 0.01455(17) Uani 1 1 d . . . . .
F1 F 0.3376(3) 0.2755(2) 0.74021(9) 0.0296(5) Uani 1 1 d . . . . .
N1 N 0.7096(3) 0.2508(3) 0.66668(11) 0.0161(5) Uani 1 1 d . . . . .
N2 N 0.5545(3) 0.3263(2) 0.83420(11) 0.0153(5) Uani 1 1 d . . . . .
C1 C 0.6749(5) 0.0852(3) 0.58308(15) 0.0275(8) Uani 1 1 d . . . . .
H1 H 0.722423 0.125416 0.550673 0.033 Uiso 1 1 calc R . . . .
C2 C 0.7041(6) -0.0525(4) 0.56703(18) 0.0395(10) Uani 1 1 d . . . . .
H2A H 0.821196 -0.101455 0.561976 0.059 Uiso 1 1 calc GR . . . .
H2B H 0.660026 -0.048294 0.533166 0.059 Uiso 1 1 calc GR . . . .
H2C H 0.649377 -0.093259 0.595967 0.059 Uiso 1 1 calc GR . . . .
C3 C 0.4885(5) 0.1634(4) 0.59128(19) 0.0364(9) Uani 1 1 d . . . . .
H3A H 0.434142 0.123688 0.620826 0.055 Uiso 1 1 calc GR . . . .
H3B H 0.443552 0.166042 0.557728 0.055 Uiso 1 1 calc GR . . . .
H3C H 0.470632 0.249433 0.600437 0.055 Uiso 1 1 calc GR . . . .
C4 C 1.0198(5) 0.0487(4) 0.62049(15) 0.0264(7) Uani 1 1 d . . . . .
H4 H 1.031479 0.124812 0.599246 0.032 Uiso 1 1 calc R . . . .
C5 C 1.1090(6) -0.0627(4) 0.58132(18) 0.0414(10) Uani 1 1 d . . . . .
H5A H 1.100092 -0.140892 0.599135 0.062 Uiso 1 1 calc GR . . . .
H5B H 1.224143 -0.072497 0.572415 0.062 Uiso 1 1 calc GR . . . .
H5C H 1.058594 -0.044181 0.547944 0.062 Uiso 1 1 calc GR . . . .
C6 C 1.1135(5) 0.0332(4) 0.66985(17) 0.0323(8) Uani 1 1 d . . . . .
H6A H 1.062179 0.108042 0.691635 0.049 Uiso 1 1 calc GR . . . .
H6B H 1.226952 0.023661 0.656697 0.049 Uiso 1 1 calc GR . . . .
H6C H 1.110065 -0.041686 0.692224 0.049 Uiso 1 1 calc GR . . . .
C7 C 0.7550(5) -0.0234(4) 0.70259(15) 0.0256(7) Uani 1 1 d . . . . .
H7 H 0.782232 0.003703 0.735441 0.031 Uiso 1 1 calc R . . . .
C8 C 0.8715(5) -0.1644(4) 0.69484(18) 0.0358(9) Uani 1 1 d . . . . .
H8A H 0.854689 -0.194027 0.661619 0.054 Uiso 1 1 calc GR . . . .
H8B H 0.847451 -0.217124 0.726051 0.054 Uiso 1 1 calc GR . . . .
H8C H 0.984857 -0.169996 0.692008 0.054 Uiso 1 1 calc GR . . . .
C9 C 0.5769(5) -0.0220(4) 0.71758(16) 0.0309(8) Uani 1 1 d . . . . .
H9A H 0.500830 0.065396 0.719906 0.046 Uiso 1 1 calc GR . . . .
H9B H 0.566786 -0.067318 0.752657 0.046 Uiso 1 1 calc GR . . . .
H9C H 0.551391 -0.063262 0.689559 0.046 Uiso 1 1 calc GR . . . .
C10 C 0.7139(4) 0.3952(3) 0.55235(14) 0.0219(7) Uani 1 1 d . . . . .
H10 H 0.625943 0.362070 0.549601 0.026 Uiso 1 1 calc R . . . .
C11 C 0.8704(5) 0.3119(4) 0.51568(14) 0.0290(8) Uani 1 1 d . . . . .
H11A H 0.959348 0.342752 0.516163 0.044 Uiso 1 1 calc GR . . . .
H11B H 0.847036 0.317016 0.478374 0.044 Uiso 1 1 calc GR . . . .
H11C H 0.902381 0.223982 0.529664 0.044 Uiso 1 1 calc GR . . . .
C12 C 0.6590(5) 0.5330(4) 0.52645(15) 0.0282(8) Uani 1 1 d . . . . .
H12A H 0.550450 0.582341 0.544184 0.042 Uiso 1 1 calc GR . . . .
H12B H 0.655816 0.530440 0.487609 0.042 Uiso 1 1 calc GR . . . .
H12C H 0.736526 0.572422 0.531399 0.042 Uiso 1 1 calc GR . . . .
C13 C 0.9449(4) 0.3937(3) 0.63698(14) 0.0210(7) Uani 1 1 d . . . . .
H13 H 1.029326 0.310300 0.626494 0.025 Uiso 1 1 calc R . . . .
C14 C 0.9988(5) 0.4956(4) 0.60065(16) 0.0288(8) Uani 1 1 d . . . . .
H14A H 1.002457 0.481853 0.562317 0.043 Uiso 1 1 calc GR . . . .
H14B H 1.107095 0.488661 0.607410 0.043 Uiso 1 1 calc GR . . . .
H14C H 0.920675 0.579847 0.609497 0.043 Uiso 1 1 calc GR . . . .
C15 C 0.9558(5) 0.4067(4) 0.69763(15) 0.0280(8) Uani 1 1 d . . . . .
H15A H 0.890403 0.492949 0.708244 0.042 Uiso 1 1 calc GR . . . .
H15B H 1.069565 0.388090 0.702193 0.042 Uiso 1 1 calc GR . . . .
H15C H 0.914422 0.347177 0.720538 0.042 Uiso 1 1 calc GR . . . .
C16 C 0.5607(4) 0.5245(3) 0.66525(14) 0.0188(6) Uani 1 1 d . . . . .
H16 H 0.564492 0.504576 0.705013 0.023 Uiso 1 1 calc R . . . .
C17 C 0.3879(4) 0.5295(3) 0.65572(15) 0.0243(7) Uani 1 1 d . . . . .
H17A H 0.375646 0.549591 0.617257 0.036 Uiso 1 1 calc GR . . . .
H17B H 0.303233 0.594645 0.677717 0.036 Uiso 1 1 calc GR . . . .
H17C H 0.377496 0.447415 0.666240 0.036 Uiso 1 1 calc GR . . . .
C18 C 0.5696(5) 0.6599(3) 0.65525(16) 0.0278(8) Uani 1 1 d . . . . .
H18A H 0.670036 0.659531 0.666520 0.042 Uiso 1 1 calc GR . . . .
H18B H 0.475482 0.720006 0.676394 0.042 Uiso 1 1 calc GR . . . .
H18C H 0.568836 0.684694 0.616574 0.042 Uiso 1 1 calc GR . . . .
C19 C 0.6147(5) 0.0488(3) 0.85573(15) 0.0244(7) Uani 1 1 d . . . . .
H19 H 0.645223 0.033396 0.816056 0.029 Uiso 1 1 calc R . . . .
C20 C 0.4263(5) 0.0779(4) 0.86714(17) 0.0326(8) Uani 1 1 d . . . . .
H20A H 0.389058 0.088630 0.906053 0.049 Uiso 1 1 calc GR . . . .
H20B H 0.402275 0.007791 0.855623 0.049 Uiso 1 1 calc GR . . . .
H20C H 0.369810 0.155584 0.846854 0.049 Uiso 1 1 calc GR . . . .
C21 C 0.7046(6) -0.0810(4) 0.88507(19) 0.0391(10) Uani 1 1 d . . . . .
H21A H 0.822115 -0.098696 0.879106 0.059 Uiso 1 1 calc GR . . . .
H21B H 0.681970 -0.148315 0.870300 0.059 Uiso 1 1 calc GR . . . .
H21C H 0.665613 -0.076993 0.924073 0.059 Uiso 1 1 calc GR . . . .
C22 C 0.8951(4) 0.1545(3) 0.82274(14) 0.0205(7) Uani 1 1 d . . . . .
H22 H 0.870626 0.173312 0.784481 0.025 Uiso 1 1 calc R . . . .
C23 C 1.0227(4) 0.0176(4) 0.82237(16) 0.0287(8) Uani 1 1 d . . . . .
H23A H 1.049073 -0.009955 0.859220 0.043 Uiso 1 1 calc GR . . . .
H23B H 1.121762 0.015861 0.798175 0.043 Uiso 1 1 calc GR . . . .
H23C H 0.977617 -0.039237 0.809499 0.043 Uiso 1 1 calc GR . . . .
C24 C 0.9776(4) 0.2498(3) 0.83153(15) 0.0241(7) Uani 1 1 d . . . . .
H24A H 0.899066 0.336139 0.829061 0.036 Uiso 1 1 calc GR . . . .
H24B H 1.071697 0.239973 0.803558 0.036 Uiso 1 1 calc GR . . . .
H24C H 1.013534 0.232789 0.867451 0.036 Uiso 1 1 calc GR . . . .
C25 C 0.6943(4) 0.1986(3) 0.94279(14) 0.0214(7) Uani 1 1 d . . . . .
H25 H 0.684181 0.287156 0.947931 0.026 Uiso 1 1 calc R . . . .
C26 C 0.5549(5) 0.1720(4) 0.98336(15) 0.0284(8) Uani 1 1 d . . . . .
H26A H 0.449388 0.221531 0.971400 0.043 Uiso 1 1 calc GR . . . .
H26B H 0.556614 0.195973 1.019743 0.043 Uiso 1 1 calc GR . . . .
H26C H 0.571564 0.082050 0.984256 0.043 Uiso 1 1 calc GR . . . .
C27 C 0.8606(5) 0.1101(4) 0.96114(16) 0.0327(8) Uani 1 1 d . . . . .
H27A H 0.879155 0.022446 0.954228 0.049 Uiso 1 1 calc GR . . . .
H27B H 0.857625 0.117966 1.000002 0.049 Uiso 1 1 calc GR . . . .
H27C H 0.949052 0.134473 0.940659 0.049 Uiso 1 1 calc GR . . . .
C28 C 0.2861(4) 0.5591(3) 0.80385(14) 0.0199(7) Uani 1 1 d . . . . .
H28 H 0.350336 0.529565 0.767911 0.024 Uiso 1 1 calc R . . . .
C29 C 0.1317(5) 0.5215(4) 0.80942(18) 0.0340(9) Uani 1 1 d . . . . .
H29A H 0.164562 0.429376 0.812733 0.051 Uiso 1 1 calc GR . . . .
H29B H 0.076593 0.553257 0.777214 0.051 Uiso 1 1 calc GR . . . .
H29C H 0.057241 0.558192 0.841805 0.051 Uiso 1 1 calc GR . . . .
C30 C 0.2290(5) 0.7062(4) 0.79988(18) 0.0354(9) Uani 1 1 d . . . . .
H30A H 0.168868 0.739927 0.834778 0.053 Uiso 1 1 calc GR . . . .
H30B H 0.158205 0.739272 0.771538 0.053 Uiso 1 1 calc GR . . . .
H30C H 0.324216 0.731778 0.790839 0.053 Uiso 1 1 calc GR . . . .
C31 C 0.3030(4) 0.4768(3) 0.92943(14) 0.0217(7) Uani 1 1 d . . . . .
H31 H 0.384045 0.434955 0.955158 0.026 Uiso 1 1 calc R . . . .
C32 C 0.1862(5) 0.4005(4) 0.93735(16) 0.0313(8) Uani 1 1 d . . . . .
H32A H 0.086221 0.450052 0.921948 0.047 Uiso 1 1 calc GR . . . .
H32B H 0.159166 0.382798 0.976175 0.047 Uiso 1 1 calc GR . . . .
H32C H 0.239895 0.320925 0.918916 0.047 Uiso 1 1 calc GR . . . .
C33 C 0.2065(5) 0.6133(4) 0.95060(16) 0.0319(8) Uani 1 1 d . . . . .
H33A H 0.281366 0.659073 0.948697 0.048 Uiso 1 1 calc GR . . . .
H33B H 0.157001 0.607187 0.988290 0.048 Uiso 1 1 calc GR . . . .
H33C H 0.120931 0.658544 0.927987 0.048 Uiso 1 1 calc GR . . . .
C34 C 0.5492(4) 0.5869(3) 0.86423(13) 0.0190(6) Uani 1 1 d . . . . .
H34 H 0.464902 0.672054 0.872035 0.023 Uiso 1 1 calc R . . . .
C35 C 0.6562(5) 0.6037(3) 0.80968(15) 0.0248(7) Uani 1 1 d . . . . .
H35A H 0.739526 0.521946 0.799826 0.037 Uiso 1 1 calc GR . . . .
H35B H 0.708965 0.663130 0.814255 0.037 Uiso 1 1 calc GR . . . .
H35C H 0.587023 0.636405 0.780871 0.037 Uiso 1 1 calc GR . . . .
C36 C 0.6561(4) 0.5502(3) 0.91174(15) 0.0238(7) Uani 1 1 d . . . . .
H36A H 0.588461 0.542889 0.946076 0.036 Uiso 1 1 calc GR . . . .
H36B H 0.701761 0.615465 0.913971 0.036 Uiso 1 1 calc GR . . . .
H36C H 0.744866 0.469219 0.904802 0.036 Uiso 1 1 calc GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Yb1 0.01711(10) 0.01825(11) 0.01369(11) -0.00119(6) -0.00107(7) -0.00644(7)
Si1 0.0269(4) 0.0170(4) 0.0149(4) -0.0013(3) -0.0031(3) -0.0112(4)
Si2 0.0173(4) 0.0175(4) 0.0137(4) -0.0014(3) -0.0022(3) -0.0095(3)
Si3 0.0147(4) 0.0122(4) 0.0166(4) 0.0015(3) -0.0034(3) -0.0031(3)
Si4 0.0129(4) 0.0141(4) 0.0154(4) -0.0028(3) -0.0024(3) -0.0025(3)
F1 0.0225(10) 0.0380(12) 0.0332(12) -0.0043(9) -0.0024(9) -0.0162(9)
N1 0.0170(12) 0.0195(14) 0.0145(13) -0.0015(10) -0.0012(10) -0.0098(11)
N2 0.0126(12) 0.0139(13) 0.0157(13) 0.0013(9) -0.0035(10) -0.0002(10)
C1 0.042(2) 0.0219(19) 0.0248(18) -0.0009(13) -0.0086(15) -0.0172(16)
C2 0.068(3) 0.034(2) 0.030(2) -0.0061(16) -0.016(2) -0.029(2)
C3 0.041(2) 0.035(2) 0.044(2) 0.0067(17) -0.0197(19) -0.0236(19)
C4 0.0292(18) 0.0250(19) 0.0221(18) -0.0042(13) 0.0007(14) -0.0071(15)
C5 0.045(2) 0.042(3) 0.032(2) -0.0120(18) 0.0059(18) -0.011(2)
C6 0.0241(18) 0.035(2) 0.037(2) 0.0017(16) -0.0075(16) -0.0079(16)
C7 0.0350(19) 0.0283(19) 0.0198(17) 0.0000(13) -0.0049(14) -0.0185(16)
C8 0.041(2) 0.026(2) 0.041(2) 0.0088(16) -0.0125(18) -0.0132(18)
C9 0.034(2) 0.031(2) 0.030(2) -0.0024(15) 0.0008(16) -0.0167(17)
C10 0.0278(17) 0.0269(18) 0.0169(16) 0.0025(13) -0.0074(13) -0.0158(15)
C11 0.044(2) 0.031(2) 0.0151(16) 0.0007(13) -0.0011(15) -0.0197(17)
C12 0.035(2) 0.033(2) 0.0199(17) 0.0058(14) -0.0072(15) -0.0168(16)
C13 0.0185(15) 0.0260(18) 0.0218(17) -0.0016(13) -0.0005(13) -0.0127(14)
C14 0.0291(18) 0.040(2) 0.0265(19) 0.0027(15) -0.0025(15) -0.0245(17)
C15 0.0291(18) 0.040(2) 0.0229(18) 0.0023(15) -0.0094(14) -0.0204(17)
C16 0.0234(16) 0.0163(16) 0.0184(16) 0.0018(12) -0.0071(13) -0.0079(13)
C17 0.0202(16) 0.0252(18) 0.0258(18) 0.0039(13) -0.0083(14) -0.0053(14)
C18 0.037(2) 0.0206(18) 0.0284(19) 0.0007(13) -0.0060(15) -0.0129(15)
C19 0.0287(18) 0.0204(18) 0.0262(18) -0.0025(13) 0.0002(14) -0.0123(14)
C20 0.036(2) 0.033(2) 0.037(2) -0.0002(16) -0.0037(17) -0.0227(18)
C21 0.047(2) 0.0170(19) 0.050(3) -0.0009(16) 0.003(2) -0.0125(17)
C22 0.0173(15) 0.0189(17) 0.0226(17) 0.0002(12) -0.0038(13) -0.0030(13)
C23 0.0215(17) 0.0217(19) 0.034(2) -0.0021(14) -0.0015(15) 0.0017(14)
C24 0.0170(15) 0.0239(18) 0.0301(19) 0.0007(13) -0.0046(13) -0.0055(14)
C25 0.0242(17) 0.0180(17) 0.0196(16) 0.0031(12) -0.0074(13) -0.0041(13)
C26 0.0341(19) 0.0262(19) 0.0227(18) 0.0029(14) -0.0008(15) -0.0106(16)
C27 0.031(2) 0.034(2) 0.0257(19) 0.0066(15) -0.0135(16) -0.0010(16)
C28 0.0193(15) 0.0140(16) 0.0216(17) -0.0038(12) -0.0069(13) 0.0023(12)
C29 0.0282(19) 0.041(2) 0.036(2) -0.0034(17) -0.0145(16) -0.0104(17)
C30 0.040(2) 0.020(2) 0.040(2) -0.0009(15) -0.0215(18) 0.0022(16)
C31 0.0175(15) 0.0278(19) 0.0171(16) -0.0043(13) -0.0007(12) -0.0047(14)
C32 0.0259(18) 0.039(2) 0.027(2) -0.0019(15) 0.0052(15) -0.0133(17)
C33 0.0296(19) 0.035(2) 0.0254(19) -0.0112(15) 0.0048(15) -0.0057(16)
C34 0.0196(15) 0.0173(16) 0.0193(16) -0.0021(12) -0.0030(13) -0.0052(13)
C35 0.0301(18) 0.0249(19) 0.0222(17) -0.0001(13) -0.0027(14) -0.0139(15)
C36 0.0271(17) 0.0246(18) 0.0233(17) -0.0019(13) -0.0082(14) -0.0113(14)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 Si1 3.5282(9) . ?
Yb1 Si2 3.2477(8) . ?
Yb1 Si3 3.3910(9) . ?
Yb1 Si4 3.2910(8) . ?
Yb1 F1 1.983(2) . ?
Yb1 N1 2.226(3) . ?
Yb1 N2 2.235(3) . ?
Si1 N1 1.744(3) . ?
Si1 C1 1.917(4) . ?
Si1 C4 1.924(4) . ?
Si1 C7 1.910(4) . ?
Si2 N1 1.730(3) . ?
Si2 C10 1.911(3) . ?
Si2 C13 1.897(3) . ?
Si2 C16 1.933(3) . ?
Si3 N2 1.741(3) . ?
Si3 C19 1.909(3) . ?
Si3 C22 1.909(3) . ?
Si3 C25 1.909(3) . ?
Si4 N2 1.726(3) . ?
Si4 C28 1.930(3) . ?
Si4 C31 1.903(3) . ?
Si4 C34 1.905(3) . ?
C1 H1 0.9800 . ?
C1 C2 1.545(5) . ?
C1 C3 1.529(6) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4 0.9800 . ?
C4 C5 1.537(5) . ?
C4 C6 1.529(5) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7 0.9800 . ?
C7 C8 1.541(6) . ?
C7 C9 1.533(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10 0.9800 . ?
C10 C11 1.542(5) . ?
C10 C12 1.538(5) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.536(5) . ?
C13 C15 1.529(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16 0.9800 . ?
C16 C17 1.543(5) . ?
C16 C18 1.535(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19 0.9800 . ?
C19 C20 1.538(5) . ?
C19 C21 1.541(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22 0.9800 . ?
C22 C23 1.527(5) . ?
C22 C24 1.535(5) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9800 . ?
C25 C26 1.538(5) . ?
C25 C27 1.536(5) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28 0.9800 . ?
C28 C29 1.535(5) . ?
C28 C30 1.530(5) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31 0.9800 . ?
C31 C32 1.530(5) . ?
C31 C33 1.543(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34 0.9800 . ?
C34 C35 1.537(5) . ?
C34 C36 1.540(5) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Si2 Yb1 Si1 53.90(2) . . ?
Si2 Yb1 Si3 129.34(2) . . ?
Si2 Yb1 Si4 126.52(2) . . ?
Si3 Yb1 Si1 106.13(2) . . ?
Si4 Yb1 Si1 159.82(2) . . ?
Si4 Yb1 Si3 56.52(2) . . ?
F1 Yb1 Si1 92.99(6) . . ?
F1 Yb1 Si2 117.12(7) . . ?
F1 Yb1 Si3 109.15(7) . . ?
F1 Yb1 Si4 102.30(6) . . ?
F1 Yb1 N1 106.52(9) . . ?
F1 Yb1 N2 108.09(9) . . ?
N1 Yb1 Si1 23.89(7) . . ?
N1 Yb1 Si2 30.10(7) . . ?
N1 Yb1 Si3 117.87(7) . . ?
N1 Yb1 Si4 150.40(7) . . ?
N1 Yb1 N2 138.71(9) . . ?
N2 Yb1 Si1 132.77(7) . . ?
N2 Yb1 Si2 134.19(7) . . ?
N2 Yb1 Si3 27.36(7) . . ?
N2 Yb1 Si4 29.16(7) . . ?
N1 Si1 C1 110.72(15) . . ?
N1 Si1 C4 107.37(15) . . ?
N1 Si1 C7 110.19(14) . . ?
C1 Si1 Yb1 115.53(12) . . ?
C1 Si1 C4 110.81(17) . . ?
C4 Si1 Yb1 126.54(11) . . ?
C7 Si1 Yb1 80.28(11) . . ?
C7 Si1 C1 110.23(16) . . ?
C7 Si1 C4 107.43(17) . . ?
N1 Si2 C10 115.95(14) . . ?
N1 Si2 C13 111.34(14) . . ?
N1 Si2 C16 102.02(13) . . ?
C10 Si2 Yb1 136.16(11) . . ?
C10 Si2 C16 108.29(15) . . ?
C13 Si2 Yb1 113.58(11) . . ?
C13 Si2 C10 109.77(15) . . ?
C13 Si2 C16 109.00(15) . . ?
C16 Si2 Yb1 63.14(10) . . ?
N2 Si3 C19 107.98(15) . . ?
N2 Si3 C22 103.77(14) . . ?
N2 Si3 C25 116.21(14) . . ?
C19 Si3 Yb1 85.59(12) . . ?
C22 Si3 Yb1 83.50(11) . . ?
C22 Si3 C19 106.09(15) . . ?
C25 Si3 Yb1 152.37(11) . . ?
C25 Si3 C19 110.86(16) . . ?
C25 Si3 C22 111.26(15) . . ?
N2 Si4 C28 105.82(13) . . ?
N2 Si4 C31 116.25(14) . . ?
N2 Si4 C34 114.64(14) . . ?
C28 Si4 Yb1 67.86(10) . . ?
C31 Si4 Yb1 138.69(11) . . ?
C31 Si4 C28 109.55(15) . . ?
C31 Si4 C34 104.81(15) . . ?
C34 Si4 Yb1 115.77(10) . . ?
C34 Si4 C28 105.23(15) . . ?
Si1 N1 Yb1 124.99(14) . . ?
Si2 N1 Yb1 109.74(13) . . ?
Si2 N1 Si1 124.93(15) . . ?
Si3 N2 Yb1 116.48(13) . . ?
Si4 N2 Yb1 111.71(13) . . ?
Si4 N2 Si3 131.81(16) . . ?
Si1 C1 H1 106.0 . . ?
C2 C1 Si1 115.2(3) . . ?
C2 C1 H1 106.0 . . ?
C3 C1 Si1 113.2(3) . . ?
C3 C1 H1 106.0 . . ?
C3 C1 C2 109.6(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4 104.7 . . ?
C5 C4 Si1 118.7(3) . . ?
C5 C4 H4 104.7 . . ?
C6 C4 Si1 111.6(2) . . ?
C6 C4 H4 104.7 . . ?
C6 C4 C5 111.0(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7 106.2 . . ?
C8 C7 Si1 114.9(3) . . ?
C8 C7 H7 106.2 . . ?
C9 C7 Si1 114.9(3) . . ?
C9 C7 H7 106.2 . . ?
C9 C7 C8 107.8(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si2 C10 H10 106.5 . . ?
C11 C10 Si2 113.7(2) . . ?
C11 C10 H10 106.5 . . ?
C12 C10 Si2 114.8(2) . . ?
C12 C10 H10 106.5 . . ?
C12 C10 C11 108.1(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si2 C13 H13 105.8 . . ?
C14 C13 Si2 117.8(2) . . ?
C14 C13 H13 105.8 . . ?
C15 C13 Si2 111.0(2) . . ?
C15 C13 H13 105.8 . . ?
C15 C13 C14 109.6(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si2 C16 H16 105.2 . . ?
C17 C16 Si2 112.0(2) . . ?
C17 C16 H16 105.2 . . ?
C18 C16 Si2 118.6(2) . . ?
C18 C16 H16 105.2 . . ?
C18 C16 C17 109.5(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si3 C19 H19 105.1 . . ?
C20 C19 Si3 115.2(3) . . ?
C20 C19 H19 105.1 . . ?
C20 C19 C21 108.9(3) . . ?
C21 C19 Si3 116.1(3) . . ?
C21 C19 H19 105.1 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si3 C22 H22 104.4 . . ?
C23 C22 Si3 119.3(2) . . ?
C23 C22 H22 104.4 . . ?
C23 C22 C24 109.8(3) . . ?
C24 C22 Si3 113.0(2) . . ?
C24 C22 H22 104.4 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si3 C25 H25 106.8 . . ?
C26 C25 Si3 114.9(2) . . ?
C26 C25 H25 106.8 . . ?
C27 C25 Si3 113.5(2) . . ?
C27 C25 H25 106.8 . . ?
C27 C25 C26 107.5(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si4 C28 H28 106.2 . . ?
C29 C28 Si4 114.1(3) . . ?
C29 C28 H28 106.2 . . ?
C30 C28 Si4 115.2(2) . . ?
C30 C28 H28 106.2 . . ?
C30 C28 C29 108.1(3) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si4 C31 H31 105.2 . . ?
C32 C31 Si4 117.5(2) . . ?
C32 C31 H31 105.2 . . ?
C32 C31 C33 109.1(3) . . ?
C33 C31 Si4 113.4(3) . . ?
C33 C31 H31 105.2 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Si4 C34 H34 106.4 . . ?
C35 C34 Si4 112.8(2) . . ?
C35 C34 H34 106.4 . . ?
C35 C34 C36 109.4(3) . . ?
C36 C34 Si4 114.8(2) . . ?
C36 C34 H34 106.4 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
_shelx_res_file
;
TITL xdpm73_a.res in P-1
xdpm73.res
created by SHELXL-2017/1 at 17:46:07 on 15-Jul-2017
REM Old TITL xdpm73 in P-1 #2
REM SHELXT solution in P-1
REM R1 0.224, Rweak 0.023, Alpha 0.042, Orientation as input
REM Formula found by SHELXT: C34 F2 N14 Si7 I
CELL 1.54184 8.729258 11.171192 24.49191 84.1821 80.5905 68.5165
ZERR 2 0.00027 0.000354 0.000754 0.0026 0.0026 0.0029
LATT 1
SFAC C H F N Si Yb
UNIT 72 168 2 4 8 2
L.S. 10
PLAN 20
CONN 30 Yb1
FREE Yb1 C17
FREE Yb1 C16
FREE Yb1 C28
BOND $H
list 4
fmap 2
acta
SHEL 100 0.83
OMIT 0 3 5
OMIT 9 -2 2
OMIT 9 -2 4
OMIT 0 1 2
OMIT 9 -2 6
REM
REM
REM
WGHT 0.059800 3.188100
FVAR 3.70852
YB1 6 0.538994 0.314581 0.744805 11.00000 0.01711 0.01825 =
0.01369 -0.00119 -0.00107 -0.00644
SI1 5 0.784665 0.094568 0.643356 11.00000 0.02695 0.01697 =
0.01487 -0.00129 -0.00306 -0.01123
SI2 5 0.738123 0.382472 0.629091 11.00000 0.01734 0.01751 =
0.01368 -0.00137 -0.00217 -0.00951
SI3 5 0.682575 0.188035 0.866342 11.00000 0.01466 0.01219 =
0.01663 0.00145 -0.00342 -0.00306
SI4 5 0.431648 0.475727 0.858719 11.00000 0.01289 0.01408 =
0.01536 -0.00280 -0.00238 -0.00251
F1 3 0.337592 0.275486 0.740212 11.00000 0.02246 0.03802 =
0.03322 -0.00430 -0.00243 -0.01622
N1 4 0.709558 0.250770 0.666683 11.00000 0.01695 0.01952 =
0.01454 -0.00147 -0.00125 -0.00983
N2 4 0.554456 0.326258 0.834205 11.00000 0.01264 0.01387 =
0.01574 0.00134 -0.00354 -0.00020
C1 1 0.674878 0.085223 0.583081 11.00000 0.04204 0.02193 =
0.02478 -0.00090 -0.00859 -0.01721
AFIX 13
H1 2 0.722423 0.125416 0.550673 11.00000 -1.20000
AFIX 0
C2 1 0.704140 -0.052488 0.567027 11.00000 0.06786 0.03407 =
0.02984 -0.00609 -0.01611 -0.02860
AFIX 137
H2A 2 0.821196 -0.101455 0.561976 11.00000 -1.50000
H2B 2 0.660026 -0.048294 0.533166 11.00000 -1.50000
H2C 2 0.649377 -0.093259 0.595967 11.00000 -1.50000
AFIX 0
C3 1 0.488451 0.163369 0.591281 11.00000 0.04143 0.03524 =
0.04412 0.00666 -0.01965 -0.02363
AFIX 137
H3A 2 0.434142 0.123688 0.620826 11.00000 -1.50000
H3B 2 0.443552 0.166042 0.557728 11.00000 -1.50000
H3C 2 0.470632 0.249433 0.600437 11.00000 -1.50000
AFIX 0
C4 1 1.019842 0.048689 0.620486 11.00000 0.02920 0.02497 =
0.02213 -0.00422 0.00074 -0.00709
AFIX 13
H4 2 1.031479 0.124812 0.599246 11.00000 -1.20000
AFIX 0
C5 1 1.109039 -0.062671 0.581319 11.00000 0.04460 0.04189 =
0.03210 -0.01201 0.00585 -0.01081
AFIX 137
H5A 2 1.100092 -0.140892 0.599135 11.00000 -1.50000
H5B 2 1.224143 -0.072497 0.572415 11.00000 -1.50000
H5C 2 1.058594 -0.044181 0.547944 11.00000 -1.50000
AFIX 0
C6 1 1.113467 0.033240 0.669852 11.00000 0.02411 0.03459 =
0.03656 0.00173 -0.00745 -0.00786
AFIX 137
H6A 2 1.062179 0.108042 0.691635 11.00000 -1.50000
H6B 2 1.226952 0.023661 0.656697 11.00000 -1.50000
H6C 2 1.110065 -0.041686 0.692224 11.00000 -1.50000
AFIX 0
C7 1 0.754999 -0.023442 0.702595 11.00000 0.03502 0.02832 =
0.01979 0.00003 -0.00486 -0.01849
AFIX 13
H7 2 0.782232 0.003703 0.735441 11.00000 -1.20000
AFIX 0
C8 1 0.871481 -0.164441 0.694837 11.00000 0.04138 0.02582 =
0.04137 0.00881 -0.01248 -0.01317
AFIX 137
H8A 2 0.854689 -0.194027 0.661619 11.00000 -1.50000
H8B 2 0.847451 -0.217124 0.726051 11.00000 -1.50000
H8C 2 0.984857 -0.169996 0.692008 11.00000 -1.50000
AFIX 0
C9 1 0.576858 -0.022024 0.717579 11.00000 0.03402 0.03090 =
0.03046 -0.00240 0.00080 -0.01674
AFIX 137
H9A 2 0.500830 0.065396 0.719906 11.00000 -1.50000
H9B 2 0.566786 -0.067318 0.752657 11.00000 -1.50000
H9C 2 0.551391 -0.063262 0.689559 11.00000 -1.50000
AFIX 0
C10 1 0.713882 0.395168 0.552353 11.00000 0.02781 0.02693 =
0.01691 0.00254 -0.00744 -0.01580
AFIX 13
H10 2 0.625943 0.362070 0.549601 11.00000 -1.20000
AFIX 0
C11 1 0.870428 0.311872 0.515679 11.00000 0.04442 0.03135 =
0.01514 0.00069 -0.00113 -0.01966
AFIX 137
H11A 2 0.959348 0.342752 0.516163 11.00000 -1.50000
H11B 2 0.847036 0.317016 0.478374 11.00000 -1.50000
H11C 2 0.902381 0.223982 0.529664 11.00000 -1.50000
AFIX 0
C12 1 0.659014 0.533045 0.526453 11.00000 0.03507 0.03325 =
0.01994 0.00580 -0.00723 -0.01678
AFIX 137
H12A 2 0.550450 0.582341 0.544184 11.00000 -1.50000
H12B 2 0.655816 0.530440 0.487609 11.00000 -1.50000
H12C 2 0.736526 0.572422 0.531399 11.00000 -1.50000
AFIX 0
C13 1 0.944934 0.393687 0.636980 11.00000 0.01854 0.02602 =
0.02185 -0.00156 -0.00053 -0.01268
AFIX 13
H13 2 1.029326 0.310300 0.626494 11.00000 -1.20000
AFIX 0
C14 1 0.998843 0.495560 0.600646 11.00000 0.02913 0.03986 =
0.02655 0.00268 -0.00255 -0.02446
AFIX 137
H14A 2 1.002457 0.481853 0.562317 11.00000 -1.50000
H14B 2 1.107095 0.488661 0.607410 11.00000 -1.50000
H14C 2 0.920675 0.579847 0.609497 11.00000 -1.50000
AFIX 0
C15 1 0.955846 0.406684 0.697629 11.00000 0.02911 0.04028 =
0.02285 0.00232 -0.00940 -0.02038
AFIX 137
H15A 2 0.890403 0.492949 0.708244 11.00000 -1.50000
H15B 2 1.069565 0.388090 0.702193 11.00000 -1.50000
H15C 2 0.914422 0.347177 0.720538 11.00000 -1.50000
AFIX 0
C16 1 0.560653 0.524536 0.665250 11.00000 0.02341 0.01630 =
0.01836 0.00180 -0.00708 -0.00793
AFIX 13
H16 2 0.564492 0.504576 0.705013 11.00000 -1.20000
AFIX 0
C17 1 0.387937 0.529518 0.655715 11.00000 0.02018 0.02523 =
0.02582 0.00389 -0.00829 -0.00534
AFIX 137
H17A 2 0.375646 0.549591 0.617257 11.00000 -1.50000
H17B 2 0.303233 0.594645 0.677717 11.00000 -1.50000
H17C 2 0.377496 0.447415 0.666240 11.00000 -1.50000
AFIX 0
C18 1 0.569589 0.659868 0.655248 11.00000 0.03694 0.02056 =
0.02845 0.00073 -0.00602 -0.01290
AFIX 137
H18A 2 0.670036 0.659531 0.666520 11.00000 -1.50000
H18B 2 0.475482 0.720006 0.676394 11.00000 -1.50000
H18C 2 0.568836 0.684694 0.616574 11.00000 -1.50000
AFIX 0
C19 1 0.614736 0.048771 0.855732 11.00000 0.02870 0.02036 =
0.02615 -0.00251 0.00017 -0.01228
AFIX 13
H19 2 0.645223 0.033396 0.816056 11.00000 -1.20000
AFIX 0
C20 1 0.426253 0.077936 0.867137 11.00000 0.03600 0.03276 =
0.03714 -0.00019 -0.00365 -0.02272
AFIX 137
H20A 2 0.389058 0.088630 0.906053 11.00000 -1.50000
H20B 2 0.402275 0.007791 0.855623 11.00000 -1.50000
H20C 2 0.369810 0.155584 0.846854 11.00000 -1.50000
AFIX 0
C21 1 0.704575 -0.081042 0.885067 11.00000 0.04723 0.01697 =
0.05039 -0.00092 0.00319 -0.01247
AFIX 137
H21A 2 0.822115 -0.098696 0.879106 11.00000 -1.50000
H21B 2 0.681970 -0.148315 0.870300 11.00000 -1.50000
H21C 2 0.665613 -0.076993 0.924073 11.00000 -1.50000
AFIX 0
C22 1 0.895068 0.154469 0.822741 11.00000 0.01734 0.01893 =
0.02256 0.00018 -0.00381 -0.00303
AFIX 13
H22 2 0.870626 0.173312 0.784481 11.00000 -1.20000
AFIX 0
C23 1 1.022731 0.017576 0.822375 11.00000 0.02149 0.02170 =
0.03424 -0.00213 -0.00153 0.00168
AFIX 137
H23A 2 1.049073 -0.009955 0.859220 11.00000 -1.50000
H23B 2 1.121762 0.015861 0.798175 11.00000 -1.50000
H23C 2 0.977617 -0.039237 0.809499 11.00000 -1.50000
AFIX 0
C24 1 0.977570 0.249770 0.831526 11.00000 0.01697 0.02389 =
0.03010 0.00067 -0.00458 -0.00547
AFIX 137
H24A 2 0.899066 0.336139 0.829061 11.00000 -1.50000
H24B 2 1.071697 0.239973 0.803558 11.00000 -1.50000
H24C 2 1.013534 0.232789 0.867451 11.00000 -1.50000
AFIX 0
C25 1 0.694260 0.198590 0.942785 11.00000 0.02425 0.01799 =
0.01964 0.00310 -0.00738 -0.00410
AFIX 13
H25 2 0.684181 0.287156 0.947931 11.00000 -1.20000
AFIX 0
C26 1 0.554860 0.172042 0.983358 11.00000 0.03413 0.02621 =
0.02267 0.00287 -0.00077 -0.01064
AFIX 137
H26A 2 0.449388 0.221531 0.971400 11.00000 -1.50000
H26B 2 0.556614 0.195973 1.019743 11.00000 -1.50000
H26C 2 0.571564 0.082050 0.984256 11.00000 -1.50000
AFIX 0
C27 1 0.860626 0.110066 0.961140 11.00000 0.03072 0.03419 =
0.02574 0.00662 -0.01355 -0.00098
AFIX 137
H27A 2 0.879155 0.022446 0.954228 11.00000 -1.50000
H27B 2 0.857625 0.117966 1.000002 11.00000 -1.50000
H27C 2 0.949052 0.134473 0.940659 11.00000 -1.50000
AFIX 0
C28 1 0.286091 0.559141 0.803853 11.00000 0.01927 0.01399 =
0.02161 -0.00377 -0.00689 0.00230
AFIX 13
H28 2 0.350336 0.529565 0.767911 11.00000 -1.20000
AFIX 0
C29 1 0.131655 0.521462 0.809423 11.00000 0.02822 0.04055 =
0.03552 -0.00341 -0.01445 -0.01036
AFIX 137
H29A 2 0.164562 0.429376 0.812733 11.00000 -1.50000
H29B 2 0.076593 0.553257 0.777214 11.00000 -1.50000
H29C 2 0.057241 0.558192 0.841805 11.00000 -1.50000
AFIX 0
C30 1 0.229029 0.706232 0.799882 11.00000 0.04040 0.02029 =
0.03994 -0.00091 -0.02146 0.00222
AFIX 137
H30A 2 0.168868 0.739927 0.834778 11.00000 -1.50000
H30B 2 0.158205 0.739272 0.771538 11.00000 -1.50000
H30C 2 0.324216 0.731778 0.790839 11.00000 -1.50000
AFIX 0
C31 1 0.302957 0.476800 0.929429 11.00000 0.01754 0.02783 =
0.01710 -0.00432 -0.00066 -0.00475
AFIX 13
H31 2 0.384045 0.434955 0.955158 11.00000 -1.20000
AFIX 0
C32 1 0.186187 0.400543 0.937355 11.00000 0.02587 0.03923 =
0.02736 -0.00191 0.00515 -0.01334
AFIX 137
H32A 2 0.086221 0.450052 0.921948 11.00000 -1.50000
H32B 2 0.159166 0.382798 0.976175 11.00000 -1.50000
H32C 2 0.239895 0.320925 0.918916 11.00000 -1.50000
AFIX 0
C33 1 0.206451 0.613290 0.950600 11.00000 0.02963 0.03475 =
0.02543 -0.01118 0.00482 -0.00567
AFIX 137
H33A 2 0.281366 0.659073 0.948697 11.00000 -1.50000
H33B 2 0.157001 0.607187 0.988290 11.00000 -1.50000
H33C 2 0.120931 0.658544 0.927987 11.00000 -1.50000
AFIX 0
C34 1 0.549210 0.586945 0.864234 11.00000 0.01961 0.01734 =
0.01933 -0.00207 -0.00304 -0.00518
AFIX 13
H34 2 0.464902 0.672054 0.872035 11.00000 -1.20000
AFIX 0
C35 1 0.656224 0.603677 0.809676 11.00000 0.03013 0.02493 =
0.02219 -0.00012 -0.00272 -0.01390
AFIX 137
H35A 2 0.739526 0.521946 0.799826 11.00000 -1.50000
H35B 2 0.708965 0.663130 0.814255 11.00000 -1.50000
H35C 2 0.587023 0.636405 0.780871 11.00000 -1.50000
AFIX 0
C36 1 0.656142 0.550167 0.911744 11.00000 0.02712 0.02458 =
0.02327 -0.00186 -0.00824 -0.01127
AFIX 137
H36A 2 0.588461 0.542889 0.946076 11.00000 -1.50000
H36B 2 0.701761 0.615465 0.913971 11.00000 -1.50000
H36C 2 0.744866 0.469219 0.904802 11.00000 -1.50000
AFIX 0
HKLF 4
REM xdpm73_a.res in P-1
REM R1 = 0.0355 for 7366 Fo > 4sig(Fo) and 0.0376 for all 7685 data
REM 421 parameters refined using 0 restraints
END
WGHT 0.0598 3.1881
REM Highest difference peak 1.487, deepest hole -1.433, 1-sigma level 0.108
Q1 1 0.5890 0.2241 0.7497 11.00000 0.05 1.49
Q2 1 0.5594 0.3009 0.7009 11.00000 0.05 1.32
Q3 1 0.6201 0.3290 0.7525 11.00000 0.05 1.26
Q4 1 0.5337 0.3205 0.7900 11.00000 0.05 1.19
Q5 1 0.4353 0.3626 0.7696 11.00000 0.05 1.07
Q6 1 0.4850 0.4226 0.7399 11.00000 0.05 0.99
Q7 1 0.6633 0.2749 0.7160 11.00000 0.05 0.96
Q8 1 0.4930 0.2688 0.7132 11.00000 0.05 0.88
Q9 1 0.4795 0.4632 0.7681 11.00000 0.05 0.77
Q10 1 0.5907 0.2806 0.8104 11.00000 0.05 0.73
Q11 1 0.6039 0.2939 0.8511 11.00000 0.05 0.68
Q12 1 0.6975 0.1871 0.9045 11.00000 0.05 0.64
Q13 1 0.4014 0.2848 0.7632 11.00000 0.05 0.63
Q14 1 0.6143 0.1603 0.7196 11.00000 0.05 0.62
Q15 1 0.7323 0.3857 0.5860 11.00000 0.05 0.62
Q16 1 0.6584 0.2171 0.8048 11.00000 0.05 0.59
Q17 1 0.8062 0.1630 0.8426 11.00000 0.05 0.52
Q18 1 0.7136 0.3544 0.7148 11.00000 0.05 0.50
Q19 1 0.7355 0.0666 0.6100 11.00000 0.05 0.48
Q20 1 0.5897 0.3277 0.6502 11.00000 0.05 0.48
;
_shelx_res_checksum 39401
_manchester_internal_archive_date 10/07/2017
_manchester_internal_coll_client FO/CAPG/DP
_manchester_internal_coll_date 10/07/2017
_manchester_internal_coll_frame_method '\w & \f scans'
_manchester_internal_coll_frame_time 5&8s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_name xdpm73
_manchester_internal_coll_type custom
_manchester_internal_coll_user FO
_manchester_internal_process_date 10/07/2017
_manchester_internal_process_user FO
_manchester_internal_refinement_date 10/07/2017
_manchester_internal_refinement_user FO
_manchester_internal_solution_date 10/07/2017
_manchester_internal_solution_user FO
_manchester_internal_validation_date 10/07/2017
_manchester_internal_validation_user FO
_olex2_exptl_crystal_mounting_method 'in fomblin oil on micromount'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.244
_oxdiff_exptl_absorpt_empirical_full_min 0.440
# start Validation Reply Form
_vrf_PLAT029_xdpm73
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.957 Note
RESPONSE: The completeness of the dataset is above the required minimum
for Cu (95%).
;