# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_2-F
_database_code_depnum_ccdc_archive 'CCDC 1833620'
_audit_update_record
;
2018-03-29 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;
_manchester_internal_coll_name adpm391
_manchester_internal_coll_client CAPG/BLLR
_manchester_internal_coll_type custom
_manchester_internal_coll_frame_time 2.0
_manchester_internal_coll_frame_width 0.8
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user CAPG
_manchester_internal_coll_date 28/10/16
_manchester_internal_process_user CAPG
_manchester_internal_process_date 27/3/18
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 27/3/18
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 27/3/18
_manchester_internal_validation_user CAPG
_manchester_internal_validation_date 28/3/18
_manchester_internal_archive_date 28/3/18
_audit_creation_date 2018-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2018/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H84 F N2 Si4 Sm'
_chemical_formula_sum 'C36 H84 F N2 Si4 Sm'
_chemical_formula_weight 826.76
_chemical_melting_point ?
_chemical_oxdiff_formula Sm(N(SiC9H21)2)2F
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 '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 8.7196(2)
_cell_length_b 10.9283(3)
_cell_length_c 25.1607(8)
_cell_angle_alpha 91.865(2)
_cell_angle_beta 98.509(2)
_cell_angle_gamma 112.973(3)
_cell_volume 2172.36(11)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 6858
_cell_measurement_temperature 150.01(10)
_cell_measurement_theta_max 27.7730
_cell_measurement_theta_min 2.5280
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.491
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.817
_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 yellow'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.264
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 882
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-11 0 -4 0.0689
11 -10 -13 0.0810
-11 11 -8 0.0904
6 10 -2 0.0800
-10 0 21 0.0698
11 -1 4 0.0459
11 -1 -21 0.0460
-1 -14 6 0.1507
4 -15 7 0.1477
-9 14 5 0.0968
3 11 -18 0.0768
0 -1 -34 0.0527
0 1 35 0.0480
3 -11 25 0.0982
-3 11 -26 0.0728
11 -9 8 0.0892
_exptl_crystal_preparation 'By Benjamin Reant and CAPG.'
_exptl_crystal_recrystallization_method 'From toluene.'
_exptl_crystal_size_max 0.261
_exptl_crystal_size_mid 0.128
_exptl_crystal_size_min 0.101
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
-11.0046 0.0059 -3.9797 0.0941 -1.0088 0.0230
10.9991 -9.9962 -13.0270 0.5128 0.6549 0.5367
-11.0015 11.0053 -7.9651 0.0533 -0.7481 -0.7071
6.0053 9.9965 -1.9976 -0.0734 0.7841 -0.6791
-10.0010 -0.0056 21.0106 -0.5947 -0.7775 0.1452
11.0043 -1.0057 3.9785 -0.0804 0.9830 0.0415
11.0010 -0.9946 -21.0135 0.6099 0.8414 -0.0845
-1.0042 -13.9992 5.9829 0.0254 -0.4163 0.9378
3.9974 -15.0013 6.9727 0.0190 0.0119 0.9878
-8.9980 13.9981 5.0309 -0.3440 -0.4179 -0.8431
3.0024 11.0045 -17.9861 0.3502 0.4503 -0.8125
-0.0048 -0.9847 -33.9903 0.9526 -0.2184 -0.1069
0.0049 0.9843 34.9900 -0.9802 0.2241 0.1119
3.0007 -11.0098 24.9735 -0.5346 0.1273 0.8243
-3.0009 11.0102 -25.9732 0.5622 -0.1329 -0.8293
11.0022 -9.0057 7.9675 -0.0808 0.7996 0.5780
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0365
_diffrn_reflns_av_unetI/netI 0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_number 15060
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.350
_diffrn_reflns_theta_min 2.117
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 150.01(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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 -20.00 60.00 0.80 2.00 -- 18.86 -99.00 30.00 100
2 \w 16.00 66.40 0.80 2.00 -- 18.86-114.00 -57.00 63
3 \w -11.00 45.00 0.80 2.00 -- 18.86 77.00 150.00 70
4 \w -86.00 48.40 0.80 2.00 -- -17.77 0.00 0.00 168
5 \w 25.00 82.60 0.80 2.00 -- 18.86 77.00-180.00 72
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0014296000
_diffrn_orient_matrix_UB_12 -0.0137257000
_diffrn_orient_matrix_UB_13 -0.0276279000
_diffrn_orient_matrix_UB_21 0.0896334000
_diffrn_orient_matrix_UB_22 0.0257284000
_diffrn_orient_matrix_UB_23 0.0056684000
_diffrn_orient_matrix_UB_31 -0.0039423000
_diffrn_orient_matrix_UB_32 -0.0645652000
_diffrn_orient_matrix_UB_33 0.0050150000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6815
_reflns_number_total 7965
_reflns_odcompleteness_completeness 99.96
_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 1.070
_refine_diff_density_min -0.493
_refine_diff_density_rms 0.105
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.051
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 421
_refine_ls_number_reflns 7965
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0500
_refine_ls_R_factor_gt 0.0400
_refine_ls_restrained_S_all 1.051
_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^)+(0.0240P)^2^+0.9140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0772
_refine_ls_wR_factor_ref 0.0837
_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
Sm1 Sm 0.34204(3) 0.76623(2) 0.75178(2) 0.02051(8) Uani 1 1 d . . . . .
Si1 Si 0.40200(13) 0.94018(10) 0.64062(4) 0.0169(2) Uani 1 1 d . . . . .
Si2 Si 0.34443(13) 0.63657(10) 0.62586(4) 0.0159(2) Uani 1 1 d . . . . .
Si3 Si 0.38686(13) 0.57277(9) 0.86034(4) 0.0154(2) Uani 1 1 d . . . . .
Si4 Si 0.62235(13) 0.86977(9) 0.87059(4) 0.0143(2) Uani 1 1 d . . . . .
F1 F 0.0996(3) 0.7438(2) 0.75585(10) 0.0302(6) Uani 1 1 d . . . . .
N1 N 0.3723(4) 0.7846(3) 0.66074(12) 0.0163(7) Uani 1 1 d . . . . .
N2 N 0.4636(3) 0.7267(3) 0.83474(12) 0.0117(7) Uani 1 1 d . . . . .
C1 C 0.3539(5) 1.0343(4) 0.69761(17) 0.0239(10) Uani 1 1 d . . . . .
H1 H 0.387250 1.000744 0.731124 0.029 Uiso 1 1 calc R . . . .
C2 C 0.1659(5) 1.0046(4) 0.69434(18) 0.0307(11) Uani 1 1 d . . . . .
H2A H 0.129226 1.044639 0.664347 0.046 Uiso 1 1 calc GR . . . .
H2B H 0.148877 1.040939 0.727153 0.046 Uiso 1 1 calc GR . . . .
H2C H 0.101569 0.909793 0.689468 0.046 Uiso 1 1 calc GR . . . .
C3 C 0.4567(6) 1.1864(4) 0.70523(18) 0.0315(11) Uani 1 1 d . . . . .
H3A H 0.574659 1.204986 0.715692 0.047 Uiso 1 1 calc GR . . . .
H3B H 0.419977 1.225520 0.732832 0.047 Uiso 1 1 calc GR . . . .
H3C H 0.439570 1.223441 0.671909 0.047 Uiso 1 1 calc GR . . . .
C4 C 0.6313(5) 1.0464(4) 0.63624(17) 0.0271(10) Uani 1 1 d . . . . .
H4 H 0.640988 1.138834 0.636637 0.033 Uiso 1 1 calc R . . . .
C5 C 0.7497(5) 1.0420(4) 0.68664(18) 0.0331(11) Uani 1 1 d . . . . .
H5A H 0.717586 1.070684 0.718114 0.050 Uiso 1 1 calc GR . . . .
H5B H 0.863862 1.100144 0.684587 0.050 Uiso 1 1 calc GR . . . .
H5C H 0.741961 0.952291 0.688923 0.050 Uiso 1 1 calc GR . . . .
C6 C 0.6955(6) 1.0202(5) 0.58620(19) 0.0411(13) Uani 1 1 d . . . . .
H6A H 0.693387 0.931637 0.584668 0.062 Uiso 1 1 calc GR . . . .
H6B H 0.809409 1.084024 0.587516 0.062 Uiso 1 1 calc GR . . . .
H6C H 0.624578 1.028307 0.554692 0.062 Uiso 1 1 calc GR . . . .
C7 C 0.2656(5) 0.9416(4) 0.57547(16) 0.0244(10) Uani 1 1 d . . . . .
H7 H 0.305506 0.903521 0.547397 0.029 Uiso 1 1 calc R . . . .
C8 C 0.0744(5) 0.8560(4) 0.56812(18) 0.0357(12) Uani 1 1 d . . . . .
H8A H 0.055973 0.773235 0.583507 0.054 Uiso 1 1 calc GR . . . .
H8B H 0.027074 0.838072 0.530321 0.054 Uiso 1 1 calc GR . . . .
H8C H 0.020790 0.903273 0.585944 0.054 Uiso 1 1 calc GR . . . .
C9 C 0.2926(6) 1.0837(4) 0.56034(18) 0.0354(12) Uani 1 1 d . . . . .
H9A H 0.248742 1.124986 0.585039 0.053 Uiso 1 1 calc GR . . . .
H9B H 0.234419 1.078298 0.524258 0.053 Uiso 1 1 calc GR . . . .
H9C H 0.411239 1.136151 0.562344 0.053 Uiso 1 1 calc GR . . . .
C10 C 0.1760(5) 0.5045(3) 0.65825(16) 0.0193(9) Uani 1 1 d . . . . .
H10 H 0.210335 0.531774 0.697141 0.023 Uiso 1 1 calc R . . . .
C11 C 0.0028(5) 0.5114(4) 0.64375(18) 0.0271(10) Uani 1 1 d . . . . .
H11A H 0.013498 0.600793 0.652642 0.041 Uiso 1 1 calc GR . . . .
H11B H -0.075058 0.451111 0.663742 0.041 Uiso 1 1 calc GR . . . .
H11C H -0.038560 0.486620 0.605765 0.041 Uiso 1 1 calc GR . . . .
C12 C 0.1585(5) 0.3605(3) 0.65219(17) 0.0279(10) Uani 1 1 d . . . . .
H12A H 0.116990 0.324881 0.615067 0.042 Uiso 1 1 calc GR . . . .
H12B H 0.080502 0.308443 0.674169 0.042 Uiso 1 1 calc GR . . . .
H12C H 0.266840 0.357414 0.663518 0.042 Uiso 1 1 calc GR . . . .
C13 C 0.2660(5) 0.6148(4) 0.55049(16) 0.0227(9) Uani 1 1 d . . . . .
H13 H 0.178123 0.650324 0.544907 0.027 Uiso 1 1 calc R . . . .
C14 C 0.3995(6) 0.6920(4) 0.51667(18) 0.0349(11) Uani 1 1 d . . . . .
H14A H 0.455169 0.783732 0.531526 0.052 Uiso 1 1 calc GR . . . .
H14B H 0.345328 0.687379 0.480101 0.052 Uiso 1 1 calc GR . . . .
H14C H 0.481215 0.653238 0.517269 0.052 Uiso 1 1 calc GR . . . .
C15 C 0.1815(5) 0.4672(4) 0.52541(17) 0.0293(10) Uani 1 1 d . . . . .
H15A H 0.258037 0.424295 0.534364 0.044 Uiso 1 1 calc GR . . . .
H15B H 0.154625 0.464437 0.486869 0.044 Uiso 1 1 calc GR . . . .
H15C H 0.079710 0.421466 0.539496 0.044 Uiso 1 1 calc GR . . . .
C16 C 0.5490(5) 0.6099(4) 0.63943(17) 0.0263(10) Uani 1 1 d . . . . .
H16 H 0.637370 0.693569 0.632531 0.032 Uiso 1 1 calc R . . . .
C17 C 0.5957(6) 0.5952(5) 0.69887(18) 0.0387(12) Uani 1 1 d . . . . .
H17A H 0.585742 0.664696 0.720595 0.058 Uiso 1 1 calc GR . . . .
H17B H 0.710043 0.601887 0.706208 0.058 Uiso 1 1 calc GR . . . .
H17C H 0.520711 0.509768 0.707302 0.058 Uiso 1 1 calc GR . . . .
C18 C 0.5648(7) 0.5027(5) 0.6048(2) 0.0581(16) Uani 1 1 d . . . . .
H18A H 0.480524 0.417459 0.609653 0.087 Uiso 1 1 calc GR . . . .
H18B H 0.675283 0.502540 0.615088 0.087 Uiso 1 1 calc GR . . . .
H18C H 0.548843 0.519339 0.567632 0.087 Uiso 1 1 calc GR . . . .
C19 C 0.2360(5) 0.4421(3) 0.80376(16) 0.0191(9) Uani 1 1 d . . . . .
H19 H 0.289187 0.461363 0.771589 0.023 Uiso 1 1 calc R . . . .
C20 C 0.0626(5) 0.4456(4) 0.78843(17) 0.0275(10) Uani 1 1 d . . . . .
H20A H -0.000374 0.416557 0.817175 0.041 Uiso 1 1 calc GR . . . .
H20B H 0.003191 0.387232 0.756066 0.041 Uiso 1 1 calc GR . . . .
H20C H 0.075456 0.535063 0.782378 0.041 Uiso 1 1 calc GR . . . .
C21 C 0.2098(5) 0.2967(3) 0.81365(17) 0.0267(10) Uani 1 1 d . . . . .
H21A H 0.317121 0.289512 0.818943 0.040 Uiso 1 1 calc GR . . . .
H21B H 0.137061 0.237344 0.782936 0.040 Uiso 1 1 calc GR . . . .
H21C H 0.158877 0.273224 0.845197 0.040 Uiso 1 1 calc GR . . . .
C22 C 0.2678(5) 0.5762(3) 0.91790(16) 0.0218(9) Uani 1 1 d . . . . .
H22 H 0.354970 0.623382 0.949391 0.026 Uiso 1 1 calc R . . . .
C23 C 0.1582(5) 0.6571(4) 0.90843(18) 0.0297(11) Uani 1 1 d . . . . .
H23A H 0.224822 0.743609 0.898611 0.044 Uiso 1 1 calc GR . . . .
H23B H 0.116920 0.667116 0.940920 0.044 Uiso 1 1 calc GR . . . .
H23C H 0.064248 0.611094 0.879844 0.044 Uiso 1 1 calc GR . . . .
C24 C 0.1599(5) 0.4391(4) 0.93543(17) 0.0327(11) Uani 1 1 d . . . . .
H24A H 0.064079 0.392461 0.907524 0.049 Uiso 1 1 calc GR . . . .
H24B H 0.121421 0.452293 0.968137 0.049 Uiso 1 1 calc GR . . . .
H24C H 0.227080 0.387566 0.941533 0.049 Uiso 1 1 calc GR . . . .
C25 C 0.5739(5) 0.5269(3) 0.88392(16) 0.0183(9) Uani 1 1 d . . . . .
H25 H 0.661100 0.608451 0.904250 0.022 Uiso 1 1 calc R . . . .
C26 C 0.6524(5) 0.4993(4) 0.83635(17) 0.0276(10) Uani 1 1 d . . . . .
H26A H 0.573781 0.419273 0.814726 0.041 Uiso 1 1 calc GR . . . .
H26B H 0.754624 0.488419 0.850010 0.041 Uiso 1 1 calc GR . . . .
H26C H 0.677732 0.573057 0.814653 0.041 Uiso 1 1 calc GR . . . .
C27 C 0.5523(6) 0.4189(4) 0.92274(18) 0.0347(11) Uani 1 1 d . . . . .
H27A H 0.521153 0.444778 0.954970 0.052 Uiso 1 1 calc GR . . . .
H27B H 0.656961 0.408217 0.931871 0.052 Uiso 1 1 calc GR . . . .
H27C H 0.465369 0.335971 0.905766 0.052 Uiso 1 1 calc GR . . . .
C28 C 0.5830(4) 1.0090(3) 0.83466(16) 0.0177(9) Uani 1 1 d . . . . .
H28 H 0.567767 0.981851 0.796080 0.021 Uiso 1 1 calc R . . . .
C29 C 0.7235(5) 1.1514(3) 0.84367(17) 0.0270(10) Uani 1 1 d . . . . .
H29A H 0.745112 1.184573 0.881001 0.040 Uiso 1 1 calc GR . . . .
H29B H 0.687791 1.208828 0.821661 0.040 Uiso 1 1 calc GR . . . .
H29C H 0.824878 1.149328 0.833936 0.040 Uiso 1 1 calc GR . . . .
C30 C 0.4143(5) 1.0142(4) 0.84270(17) 0.0239(10) Uani 1 1 d . . . . .
H30A H 0.325457 0.926546 0.834202 0.036 Uiso 1 1 calc GR . . . .
H30B H 0.389631 1.074344 0.819337 0.036 Uiso 1 1 calc GR . . . .
H30C H 0.422256 1.044981 0.879591 0.036 Uiso 1 1 calc GR . . . .
C31 C 0.8405(5) 0.8805(4) 0.86273(16) 0.0188(9) Uani 1 1 d . . . . .
H31 H 0.842160 0.794165 0.871390 0.023 Uiso 1 1 calc R . . . .
C32 C 0.8677(5) 0.8927(4) 0.80414(17) 0.0275(10) Uani 1 1 d . . . . .
H32A H 0.769369 0.829830 0.780600 0.041 Uiso 1 1 calc GR . . . .
H32B H 0.964402 0.874301 0.799757 0.041 Uiso 1 1 calc GR . . . .
H32C H 0.886504 0.981629 0.795296 0.041 Uiso 1 1 calc GR . . . .
C33 C 0.9938(5) 0.9867(4) 0.90006(17) 0.0278(10) Uani 1 1 d . . . . .
H33A H 0.996954 1.073840 0.893938 0.042 Uiso 1 1 calc GR . . . .
H33B H 1.095759 0.981147 0.892522 0.042 Uiso 1 1 calc GR . . . .
H33C H 0.984370 0.971452 0.937025 0.042 Uiso 1 1 calc GR . . . .
C34 C 0.6132(5) 0.8960(4) 0.94500(16) 0.0206(9) Uani 1 1 d . . . . .
H34 H 0.492854 0.863217 0.947434 0.025 Uiso 1 1 calc R . . . .
C35 C 0.6930(5) 1.0424(4) 0.96998(16) 0.0262(10) Uani 1 1 d . . . . .
H35A H 0.810467 1.081099 0.966865 0.039 Uiso 1 1 calc GR . . . .
H35B H 0.682665 1.045623 1.007407 0.039 Uiso 1 1 calc GR . . . .
H35C H 0.635626 1.091814 0.951227 0.039 Uiso 1 1 calc GR . . . .
C36 C 0.6873(5) 0.8153(4) 0.98272(16) 0.0278(10) Uani 1 1 d . . . . .
H36A H 0.635277 0.722480 0.969262 0.042 Uiso 1 1 calc GR . . . .
H36B H 0.665164 0.825670 1.018485 0.042 Uiso 1 1 calc GR . . . .
H36C H 0.807191 0.847733 0.983730 0.042 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
Sm1 0.02067(13) 0.02625(13) 0.01527(13) 0.00356(9) 0.00286(9) 0.01007(10)
Si1 0.0198(6) 0.0177(5) 0.0161(6) 0.0040(4) 0.0046(5) 0.0099(5)
Si2 0.0164(6) 0.0175(5) 0.0156(6) 0.0005(4) 0.0024(4) 0.0091(5)
Si3 0.0169(6) 0.0127(5) 0.0151(6) 0.0022(4) 0.0025(4) 0.0044(4)
Si4 0.0140(6) 0.0128(5) 0.0149(6) 0.0015(4) 0.0026(4) 0.0040(4)
F1 0.0272(14) 0.0368(13) 0.0337(16) 0.0079(11) 0.0091(11) 0.0186(11)
N1 0.0177(18) 0.0172(16) 0.0141(18) 0.0019(13) 0.0033(14) 0.0070(14)
N2 0.0100(16) 0.0130(15) 0.0109(17) 0.0019(12) 0.0026(13) 0.0028(13)
C1 0.033(3) 0.020(2) 0.023(2) 0.0068(17) 0.0017(19) 0.0154(19)
C2 0.040(3) 0.033(2) 0.028(3) 0.006(2) 0.012(2) 0.023(2)
C3 0.044(3) 0.021(2) 0.030(3) -0.0025(19) 0.005(2) 0.015(2)
C4 0.027(3) 0.030(2) 0.025(3) 0.0096(19) 0.0076(19) 0.010(2)
C5 0.018(2) 0.037(3) 0.039(3) 0.007(2) 0.005(2) 0.006(2)
C6 0.034(3) 0.049(3) 0.036(3) -0.001(2) 0.012(2) 0.010(2)
C7 0.033(3) 0.032(2) 0.017(2) 0.0057(18) 0.0033(19) 0.022(2)
C8 0.038(3) 0.040(3) 0.031(3) 0.003(2) -0.006(2) 0.022(2)
C9 0.052(3) 0.038(3) 0.025(3) 0.015(2) 0.006(2) 0.027(2)
C10 0.021(2) 0.0174(19) 0.019(2) 0.0023(16) 0.0002(17) 0.0084(17)
C11 0.021(2) 0.029(2) 0.031(3) 0.0029(19) 0.0052(19) 0.0093(19)
C12 0.032(3) 0.020(2) 0.031(3) 0.0022(18) 0.006(2) 0.0082(19)
C13 0.026(2) 0.026(2) 0.019(2) 0.0017(17) 0.0026(18) 0.0139(19)
C14 0.051(3) 0.034(2) 0.022(3) 0.003(2) 0.011(2) 0.018(2)
C15 0.037(3) 0.027(2) 0.021(3) -0.0050(18) -0.002(2) 0.013(2)
C16 0.025(2) 0.033(2) 0.023(3) -0.0047(19) 0.0011(19) 0.016(2)
C17 0.039(3) 0.059(3) 0.031(3) -0.001(2) -0.002(2) 0.037(3)
C18 0.055(4) 0.078(4) 0.050(4) -0.015(3) -0.005(3) 0.043(3)
C19 0.024(2) 0.0137(19) 0.018(2) 0.0000(16) 0.0064(18) 0.0058(17)
C20 0.027(3) 0.023(2) 0.027(3) 0.0004(18) 0.003(2) 0.0045(19)
C21 0.026(2) 0.016(2) 0.033(3) 0.0011(18) 0.008(2) 0.0028(18)
C22 0.022(2) 0.019(2) 0.018(2) 0.0034(16) 0.0053(18) 0.0000(18)
C23 0.023(2) 0.029(2) 0.034(3) -0.0039(19) 0.011(2) 0.006(2)
C24 0.037(3) 0.031(2) 0.024(3) 0.0050(19) 0.017(2) 0.003(2)
C25 0.024(2) 0.0143(19) 0.018(2) 0.0039(16) -0.0008(17) 0.0097(17)
C26 0.025(2) 0.028(2) 0.032(3) 0.0048(19) -0.001(2) 0.0157(19)
C27 0.041(3) 0.031(2) 0.031(3) 0.009(2) 0.001(2) 0.016(2)
C28 0.013(2) 0.0152(19) 0.021(2) -0.0019(16) -0.0013(17) 0.0032(16)
C29 0.028(3) 0.015(2) 0.032(3) 0.0028(18) 0.001(2) 0.0035(18)
C30 0.026(2) 0.020(2) 0.026(3) -0.0010(17) -0.0020(19) 0.0122(18)
C31 0.018(2) 0.0172(19) 0.022(2) 0.0062(16) 0.0060(17) 0.0056(17)
C32 0.021(2) 0.036(2) 0.028(3) 0.0020(19) 0.0100(19) 0.0105(19)
C33 0.017(2) 0.033(2) 0.028(3) 0.0026(19) 0.0011(19) 0.0049(19)
C34 0.017(2) 0.022(2) 0.021(2) -0.0015(17) 0.0022(17) 0.0064(17)
C35 0.029(3) 0.025(2) 0.021(2) -0.0018(18) 0.0027(19) 0.0081(19)
C36 0.033(3) 0.027(2) 0.016(2) 0.0015(18) 0.0021(19) 0.004(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 F1 2.049(2) . ?
Sm1 N1 2.350(3) . ?
Sm1 N2 2.330(3) . ?
Si1 N1 1.722(3) . ?
Si1 C1 1.925(4) . ?
Si1 C4 1.903(4) . ?
Si1 C7 1.882(4) . ?
Si2 N1 1.727(3) . ?
Si2 C10 1.919(4) . ?
Si2 C13 1.892(4) . ?
Si2 C16 1.902(4) . ?
Si3 N2 1.735(3) . ?
Si3 C19 1.908(4) . ?
Si3 C22 1.910(4) . ?
Si3 C25 1.907(4) . ?
Si4 N2 1.739(3) . ?
Si4 C28 1.912(4) . ?
Si4 C31 1.900(4) . ?
Si4 C34 1.903(4) . ?
C1 H1 0.9800 . ?
C1 C2 1.531(5) . ?
C1 C3 1.539(5) . ?
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 1.527(6) . ?
C4 C6 1.513(6) . ?
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 1.539(6) . ?
C7 C9 1.546(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 1.532(5) . ?
C10 C12 1.520(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 1.538(5) . ?
C13 C15 1.554(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 1.521(6) . ?
C16 C18 1.498(6) . ?
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 1.519(5) . ?
C19 C21 1.549(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 1.535(5) . ?
C22 C24 1.546(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 1.540(5) . ?
C25 C27 1.529(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 1.543(5) . ?
C28 C30 1.537(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 1.529(5) . ?
C31 C33 1.537(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 1.542(5) . ?
C34 C36 1.554(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
F1 Sm1 N1 106.78(10) . . ?
F1 Sm1 N2 108.56(10) . . ?
N2 Sm1 N1 143.37(11) . . ?
N1 Si1 C1 106.47(16) . . ?
N1 Si1 C4 113.03(17) . . ?
N1 Si1 C7 115.62(17) . . ?
C4 Si1 C1 104.17(18) . . ?
C7 Si1 C1 108.52(18) . . ?
C7 Si1 C4 108.31(18) . . ?
N1 Si2 C10 103.12(16) . . ?
N1 Si2 C13 117.25(16) . . ?
N1 Si2 C16 109.39(17) . . ?
C13 Si2 C10 108.17(17) . . ?
C13 Si2 C16 109.34(19) . . ?
C16 Si2 C10 109.21(18) . . ?
N2 Si3 C19 108.74(16) . . ?
N2 Si3 C22 111.47(16) . . ?
N2 Si3 C25 107.97(16) . . ?
C19 Si3 C22 108.84(17) . . ?
C25 Si3 C19 108.58(17) . . ?
C25 Si3 C22 111.17(18) . . ?
N2 Si4 C28 102.30(15) . . ?
N2 Si4 C31 111.43(16) . . ?
N2 Si4 C34 115.87(15) . . ?
C31 Si4 C28 108.49(16) . . ?
C31 Si4 C34 109.92(18) . . ?
C34 Si4 C28 108.31(17) . . ?
Si1 N1 Sm1 113.45(15) . . ?
Si1 N1 Si2 132.44(19) . . ?
Si2 N1 Sm1 113.89(14) . . ?
Si3 N2 Sm1 122.54(14) . . ?
Si3 N2 Si4 123.92(18) . . ?
Si4 N2 Sm1 113.23(13) . . ?
Si1 C1 H1 105.8 . . ?
C2 C1 Si1 114.1(3) . . ?
C2 C1 H1 105.8 . . ?
C2 C1 C3 109.4(3) . . ?
C3 C1 Si1 115.1(3) . . ?
C3 C1 H1 105.8 . . ?
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 106.0 . . ?
C5 C4 Si1 110.8(3) . . ?
C5 C4 H4 106.0 . . ?
C6 C4 Si1 117.4(3) . . ?
C6 C4 H4 106.0 . . ?
C6 C4 C5 109.8(4) . . ?
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 105.1 . . ?
C8 C7 Si1 118.0(3) . . ?
C8 C7 H7 105.1 . . ?
C8 C7 C9 108.8(3) . . ?
C9 C7 Si1 113.5(3) . . ?
C9 C7 H7 105.1 . . ?
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 104.8 . . ?
C11 C10 Si2 111.7(3) . . ?
C11 C10 H10 104.8 . . ?
C12 C10 Si2 118.7(3) . . ?
C12 C10 H10 104.8 . . ?
C12 C10 C11 110.5(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 106.4 . . ?
C14 C13 Si2 115.1(3) . . ?
C14 C13 H13 106.4 . . ?
C14 C13 C15 107.5(3) . . ?
C15 C13 Si2 114.3(3) . . ?
C15 C13 H13 106.4 . . ?
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 105.4 . . ?
C17 C16 Si2 111.1(3) . . ?
C17 C16 H16 105.4 . . ?
C18 C16 Si2 118.3(3) . . ?
C18 C16 H16 105.4 . . ?
C18 C16 C17 110.2(4) . . ?
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 106.2 . . ?
C20 C19 Si3 115.6(3) . . ?
C20 C19 H19 106.2 . . ?
C20 C19 C21 107.9(3) . . ?
C21 C19 Si3 114.2(3) . . ?
C21 C19 H19 106.2 . . ?
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 105.8 . . ?
C23 C22 Si3 113.7(3) . . ?
C23 C22 H22 105.8 . . ?
C23 C22 C24 108.6(3) . . ?
C24 C22 Si3 116.3(3) . . ?
C24 C22 H22 105.8 . . ?
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 104.8 . . ?
C26 C25 Si3 112.0(3) . . ?
C26 C25 H25 104.8 . . ?
C27 C25 Si3 118.7(3) . . ?
C27 C25 H25 104.8 . . ?
C27 C25 C26 110.3(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 105.0 . . ?
C29 C28 Si4 119.1(3) . . ?
C29 C28 H28 105.0 . . ?
C30 C28 Si4 111.9(3) . . ?
C30 C28 H28 105.0 . . ?
C30 C28 C29 109.7(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 105.8 . . ?
C32 C31 Si4 111.8(3) . . ?
C32 C31 H31 105.8 . . ?
C32 C31 C33 109.3(3) . . ?
C33 C31 Si4 117.5(3) . . ?
C33 C31 H31 105.8 . . ?
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 115.5(3) . . ?
C35 C34 H34 106.0 . . ?
C35 C34 C36 107.5(3) . . ?
C36 C34 Si4 115.0(3) . . ?
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 . . ?
_shelx_res_file
;
TITL adpm391_a.res in P-1
adpm391.res
created by SHELXL-2018/1 at 10:18:11 on 28-Mar-2018
REM Old TITL adpm391 in P1
REM SHELXT solution in P-1
REM R1 0.089, Rweak 0.010, Alpha 0.023, Orientation as input
REM Formula found by SHELXT: C36 N2 F Si4 Sm
CELL 0.71073 8.7196 10.9283 25.1607 91.865 98.509 112.973
ZERR 2 0.0002 0.0003 0.0008 0.002 0.002 0.003
LATT 1
SFAC C H F N Si Sm
UNIT 72 168 2 4 8 2
L.S. 10
PLAN 20
CONN 20 Sm1
FREE Sm1 Si1
FREE Sm1 Si4
FREE Sm1 Si2
BOND $H
list 4
fmap 2
acta
SHEL 100 0.83
REM
REM
REM
WGHT 0.024000 0.914000
FVAR 4.31945
SM1 6 0.342037 0.766231 0.751776 11.00000 0.02067 0.02625 =
0.01527 0.00356 0.00286 0.01007
SI1 5 0.401998 0.940183 0.640622 11.00000 0.01978 0.01768 =
0.01614 0.00403 0.00460 0.00987
SI2 5 0.344432 0.636566 0.625855 11.00000 0.01642 0.01751 =
0.01562 0.00052 0.00238 0.00906
SI3 5 0.386863 0.572765 0.860340 11.00000 0.01687 0.01273 =
0.01509 0.00219 0.00253 0.00443
SI4 5 0.622351 0.869768 0.870589 11.00000 0.01404 0.01280 =
0.01485 0.00152 0.00262 0.00397
F1 3 0.099629 0.743758 0.755846 11.00000 0.02725 0.03680 =
0.03372 0.00792 0.00906 0.01861
N1 4 0.372339 0.784604 0.660738 11.00000 0.01770 0.01723 =
0.01410 0.00194 0.00331 0.00701
N2 4 0.463567 0.726679 0.834738 11.00000 0.00997 0.01296 =
0.01091 0.00188 0.00256 0.00284
C1 1 0.353947 1.034270 0.697607 11.00000 0.03275 0.02011 =
0.02274 0.00678 0.00165 0.01545
AFIX 13
H1 2 0.387250 1.000744 0.731124 11.00000 -1.20000
AFIX 0
C2 1 0.165860 1.004647 0.694339 11.00000 0.04038 0.03340 =
0.02846 0.00611 0.01223 0.02304
AFIX 137
H2A 2 0.129226 1.044639 0.664347 11.00000 -1.50000
H2B 2 0.148877 1.040939 0.727153 11.00000 -1.50000
H2C 2 0.101569 0.909793 0.689468 11.00000 -1.50000
AFIX 0
C3 1 0.456701 1.186355 0.705227 11.00000 0.04408 0.02147 =
0.03027 -0.00252 0.00518 0.01542
AFIX 137
H3A 2 0.574659 1.204986 0.715692 11.00000 -1.50000
H3B 2 0.419977 1.225520 0.732832 11.00000 -1.50000
H3C 2 0.439570 1.223441 0.671909 11.00000 -1.50000
AFIX 0
C4 1 0.631318 1.046391 0.636236 11.00000 0.02680 0.02985 =
0.02510 0.00957 0.00763 0.01007
AFIX 13
H4 2 0.640988 1.138834 0.636637 11.00000 -1.20000
AFIX 0
C5 1 0.749667 1.041967 0.686644 11.00000 0.01824 0.03712 =
0.03929 0.00742 0.00484 0.00599
AFIX 137
H5A 2 0.717586 1.070684 0.718114 11.00000 -1.50000
H5B 2 0.863862 1.100144 0.684587 11.00000 -1.50000
H5C 2 0.741961 0.952291 0.688923 11.00000 -1.50000
AFIX 0
C6 1 0.695545 1.020195 0.586204 11.00000 0.03404 0.04890 =
0.03613 -0.00074 0.01225 0.01015
AFIX 137
H6A 2 0.693387 0.931637 0.584668 11.00000 -1.50000
H6B 2 0.809409 1.084024 0.587516 11.00000 -1.50000
H6C 2 0.624578 1.028307 0.554692 11.00000 -1.50000
AFIX 0
C7 1 0.265588 0.941644 0.575469 11.00000 0.03305 0.03188 =
0.01700 0.00565 0.00326 0.02241
AFIX 13
H7 2 0.305506 0.903521 0.547397 11.00000 -1.20000
AFIX 0
C8 1 0.074363 0.855997 0.568119 11.00000 0.03770 0.03982 =
0.03136 0.00335 -0.00584 0.02163
AFIX 137
H8A 2 0.055973 0.773235 0.583507 11.00000 -1.50000
H8B 2 0.027074 0.838072 0.530321 11.00000 -1.50000
H8C 2 0.020790 0.903273 0.585944 11.00000 -1.50000
AFIX 0
C9 1 0.292553 1.083742 0.560343 11.00000 0.05233 0.03807 =
0.02496 0.01543 0.00637 0.02713
AFIX 137
H9A 2 0.248742 1.124986 0.585039 11.00000 -1.50000
H9B 2 0.234419 1.078298 0.524258 11.00000 -1.50000
H9C 2 0.411239 1.136151 0.562344 11.00000 -1.50000
AFIX 0
C10 1 0.175969 0.504506 0.658255 11.00000 0.02092 0.01740 =
0.01934 0.00229 0.00021 0.00840
AFIX 13
H10 2 0.210335 0.531774 0.697141 11.00000 -1.20000
AFIX 0
C11 1 0.002802 0.511401 0.643747 11.00000 0.02093 0.02940 =
0.03059 0.00291 0.00523 0.00930
AFIX 137
H11A 2 0.013498 0.600793 0.652642 11.00000 -1.50000
H11B 2 -0.075058 0.451111 0.663742 11.00000 -1.50000
H11C 2 -0.038560 0.486620 0.605765 11.00000 -1.50000
AFIX 0
C12 1 0.158462 0.360545 0.652194 11.00000 0.03165 0.01960 =
0.03075 0.00220 0.00608 0.00821
AFIX 137
H12A 2 0.116990 0.324881 0.615067 11.00000 -1.50000
H12B 2 0.080502 0.308443 0.674169 11.00000 -1.50000
H12C 2 0.266840 0.357414 0.663518 11.00000 -1.50000
AFIX 0
C13 1 0.265956 0.614826 0.550489 11.00000 0.02558 0.02615 =
0.01920 0.00166 0.00264 0.01393
AFIX 13
H13 2 0.178123 0.650324 0.544907 11.00000 -1.20000
AFIX 0
C14 1 0.399454 0.692046 0.516670 11.00000 0.05109 0.03363 =
0.02230 0.00285 0.01066 0.01786
AFIX 137
H14A 2 0.455169 0.783732 0.531526 11.00000 -1.50000
H14B 2 0.345328 0.687379 0.480101 11.00000 -1.50000
H14C 2 0.481215 0.653238 0.517269 11.00000 -1.50000
AFIX 0
C15 1 0.181517 0.467151 0.525409 11.00000 0.03678 0.02675 =
0.02148 -0.00500 -0.00192 0.01278
AFIX 137
H15A 2 0.258037 0.424295 0.534364 11.00000 -1.50000
H15B 2 0.154625 0.464437 0.486869 11.00000 -1.50000
H15C 2 0.079710 0.421466 0.539496 11.00000 -1.50000
AFIX 0
C16 1 0.549007 0.609858 0.639431 11.00000 0.02546 0.03331 =
0.02285 -0.00467 0.00109 0.01638
AFIX 13
H16 2 0.637370 0.693569 0.632531 11.00000 -1.20000
AFIX 0
C17 1 0.595680 0.595200 0.698865 11.00000 0.03937 0.05921 =
0.03069 -0.00085 -0.00163 0.03674
AFIX 137
H17A 2 0.585742 0.664696 0.720595 11.00000 -1.50000
H17B 2 0.710043 0.601887 0.706208 11.00000 -1.50000
H17C 2 0.520711 0.509768 0.707302 11.00000 -1.50000
AFIX 0
C18 1 0.564835 0.502677 0.604847 11.00000 0.05499 0.07771 =
0.05025 -0.01544 -0.00538 0.04265
AFIX 137
H18A 2 0.480524 0.417459 0.609653 11.00000 -1.50000
H18B 2 0.675283 0.502540 0.615088 11.00000 -1.50000
H18C 2 0.548843 0.519339 0.567632 11.00000 -1.50000
AFIX 0
C19 1 0.236016 0.442149 0.803761 11.00000 0.02435 0.01374 =
0.01845 -0.00001 0.00642 0.00585
AFIX 13
H19 2 0.289187 0.461363 0.771589 11.00000 -1.20000
AFIX 0
C20 1 0.062610 0.445565 0.788434 11.00000 0.02695 0.02274 =
0.02680 0.00037 0.00281 0.00447
AFIX 137
H20A 2 -0.000374 0.416557 0.817175 11.00000 -1.50000
H20B 2 0.003191 0.387232 0.756066 11.00000 -1.50000
H20C 2 0.075456 0.535063 0.782378 11.00000 -1.50000
AFIX 0
C21 1 0.209775 0.296740 0.813649 11.00000 0.02643 0.01642 =
0.03282 0.00109 0.00819 0.00277
AFIX 137
H21A 2 0.317121 0.289512 0.818943 11.00000 -1.50000
H21B 2 0.137061 0.237344 0.782936 11.00000 -1.50000
H21C 2 0.158877 0.273224 0.845197 11.00000 -1.50000
AFIX 0
C22 1 0.267820 0.576216 0.917901 11.00000 0.02200 0.01878 =
0.01771 0.00340 0.00530 0.00002
AFIX 13
H22 2 0.354970 0.623382 0.949391 11.00000 -1.20000
AFIX 0
C23 1 0.158180 0.657086 0.908432 11.00000 0.02324 0.02933 =
0.03412 -0.00386 0.01115 0.00645
AFIX 137
H23A 2 0.224822 0.743609 0.898611 11.00000 -1.50000
H23B 2 0.116920 0.667116 0.940920 11.00000 -1.50000
H23C 2 0.064248 0.611094 0.879844 11.00000 -1.50000
AFIX 0
C24 1 0.159872 0.439147 0.935435 11.00000 0.03662 0.03098 =
0.02443 0.00503 0.01652 0.00307
AFIX 137
H24A 2 0.064079 0.392461 0.907524 11.00000 -1.50000
H24B 2 0.121421 0.452293 0.968137 11.00000 -1.50000
H24C 2 0.227080 0.387566 0.941533 11.00000 -1.50000
AFIX 0
C25 1 0.573917 0.526885 0.883921 11.00000 0.02360 0.01435 =
0.01779 0.00390 -0.00075 0.00968
AFIX 13
H25 2 0.661100 0.608451 0.904250 11.00000 -1.20000
AFIX 0
C26 1 0.652404 0.499312 0.836348 11.00000 0.02513 0.02833 =
0.03218 0.00481 -0.00111 0.01570
AFIX 137
H26A 2 0.573781 0.419273 0.814726 11.00000 -1.50000
H26B 2 0.754624 0.488419 0.850010 11.00000 -1.50000
H26C 2 0.677732 0.573057 0.814653 11.00000 -1.50000
AFIX 0
C27 1 0.552343 0.418918 0.922744 11.00000 0.04146 0.03098 =
0.03137 0.00900 0.00117 0.01557
AFIX 137
H27A 2 0.521153 0.444778 0.954970 11.00000 -1.50000
H27B 2 0.656961 0.408217 0.931871 11.00000 -1.50000
H27C 2 0.465369 0.335971 0.905766 11.00000 -1.50000
AFIX 0
C28 1 0.583019 1.008994 0.834664 11.00000 0.01305 0.01520 =
0.02094 -0.00195 -0.00128 0.00317
AFIX 13
H28 2 0.567767 0.981851 0.796080 11.00000 -1.20000
AFIX 0
C29 1 0.723460 1.151374 0.843665 11.00000 0.02818 0.01488 =
0.03177 0.00283 0.00128 0.00355
AFIX 137
H29A 2 0.745112 1.184573 0.881001 11.00000 -1.50000
H29B 2 0.687791 1.208828 0.821661 11.00000 -1.50000
H29C 2 0.824878 1.149328 0.833936 11.00000 -1.50000
AFIX 0
C30 1 0.414251 1.014205 0.842703 11.00000 0.02628 0.02030 =
0.02554 -0.00102 -0.00204 0.01218
AFIX 137
H30A 2 0.325457 0.926546 0.834202 11.00000 -1.50000
H30B 2 0.389631 1.074344 0.819337 11.00000 -1.50000
H30C 2 0.422256 1.044981 0.879591 11.00000 -1.50000
AFIX 0
C31 1 0.840468 0.880463 0.862731 11.00000 0.01761 0.01724 =
0.02153 0.00616 0.00599 0.00559
AFIX 13
H31 2 0.842160 0.794165 0.871390 11.00000 -1.20000
AFIX 0
C32 1 0.867722 0.892694 0.804143 11.00000 0.02058 0.03570 =
0.02755 0.00200 0.01000 0.01055
AFIX 137
H32A 2 0.769369 0.829830 0.780600 11.00000 -1.50000
H32B 2 0.964402 0.874301 0.799757 11.00000 -1.50000
H32C 2 0.886504 0.981629 0.795296 11.00000 -1.50000
AFIX 0
C33 1 0.993779 0.986698 0.900058 11.00000 0.01700 0.03277 =
0.02788 0.00259 0.00112 0.00493
AFIX 137
H33A 2 0.996954 1.073840 0.893938 11.00000 -1.50000
H33B 2 1.095759 0.981147 0.892522 11.00000 -1.50000
H33C 2 0.984370 0.971452 0.937025 11.00000 -1.50000
AFIX 0
C34 1 0.613208 0.896002 0.944999 11.00000 0.01701 0.02167 =
0.02118 -0.00154 0.00225 0.00636
AFIX 13
H34 2 0.492854 0.863217 0.947434 11.00000 -1.20000
AFIX 0
C35 1 0.693018 1.042446 0.969981 11.00000 0.02906 0.02493 =
0.02132 -0.00181 0.00269 0.00813
AFIX 137
H35A 2 0.810467 1.081099 0.966865 11.00000 -1.50000
H35B 2 0.682665 1.045623 1.007407 11.00000 -1.50000
H35C 2 0.635626 1.091814 0.951227 11.00000 -1.50000
AFIX 0
C36 1 0.687289 0.815255 0.982724 11.00000 0.03264 0.02653 =
0.01623 0.00147 0.00213 0.00407
AFIX 137
H36A 2 0.635277 0.722480 0.969262 11.00000 -1.50000
H36B 2 0.665164 0.825670 1.018485 11.00000 -1.50000
H36C 2 0.807191 0.847733 0.983730 11.00000 -1.50000
AFIX 0
HKLF 4
REM adpm391_a.res in P-1
REM R1 = 0.0400 for 6815 Fo > 4sig(Fo) and 0.0500 for all 7965 data
REM 421 parameters refined using 0 restraints
END
WGHT 0.0240 0.9140
REM Highest difference peak 1.070, deepest hole -0.493, 1-sigma level 0.105
Q1 1 -0.0248 0.7011 0.7457 11.00000 0.05 0.70
Q2 1 0.3145 0.6812 0.7434 11.00000 0.05 0.56
Q3 1 0.1929 0.7416 0.7348 11.00000 0.05 0.51
Q4 1 0.3223 0.9486 0.6080 11.00000 0.05 0.50
Q5 1 0.7198 0.7428 0.6539 11.00000 0.05 0.49
Q6 1 0.0577 0.6629 0.6276 11.00000 0.05 0.45
Q7 1 0.6443 1.1100 0.5872 11.00000 0.05 0.44
Q8 1 0.3028 0.5017 0.8293 11.00000 0.05 0.44
Q9 1 0.3762 0.9753 0.6692 11.00000 0.05 0.42
Q10 1 0.0445 0.5273 0.8307 11.00000 0.05 0.41
Q11 1 0.6347 0.8808 0.9090 11.00000 0.05 0.41
Q12 1 0.4471 0.6337 0.6408 11.00000 0.05 0.41
Q13 1 0.9069 0.8139 0.7687 11.00000 0.05 0.40
Q14 1 0.3950 0.3779 0.9605 11.00000 0.05 0.40
Q15 1 0.8305 0.9963 0.6691 11.00000 0.05 0.39
Q16 1 0.0309 0.3355 0.6318 11.00000 0.05 0.38
Q17 1 0.4500 0.7529 0.7991 11.00000 0.05 0.37
Q18 1 -0.1490 0.8452 0.5948 11.00000 0.05 0.36
Q19 1 0.2213 0.6523 0.5229 11.00000 0.05 0.36
Q20 1 0.1740 0.8640 0.5098 11.00000 0.05 0.36
;
_shelx_res_checksum 69542
_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 1.136
_oxdiff_exptl_absorpt_empirical_full_min 0.869
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_2-I
_database_code_depnum_ccdc_archive 'CCDC 1833623'
_audit_update_record
;
2018-04-28 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;
_manchester_internal_coll_name adpm350
_manchester_internal_coll_client CAPG
_manchester_internal_coll_type custom
_manchester_internal_coll_frame_time 2.0
_manchester_internal_coll_frame_width 0.9
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user CAPG
_manchester_internal_coll_date 13/7/16
_manchester_internal_process_user CAPG
_manchester_internal_process_date 27/3/18
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 27/3/18
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 28/4/18
_manchester_internal_validation_user CAPG
_manchester_internal_validation_date 28/4/18
_manchester_internal_archive_date 28/4/18
_refine_special_details
;
A channel was identified that runs throughout the crystal approximately along
the C axis. The solvent of crystallisation was hexane, and the channel
contained roughly zig-zaig chains of electron density smeared along C. A model
hexane moiety was assemled using DFIX for all 1-2 and 1-3 distances, and this
whole moiety was then fixed at an occupancy of 0.5. The atoms were all refined
isotropically as no good model could be made without excessive use of
restraints.
;
_audit_creation_date 2018-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_shelx_SHELXL_version_number 2018/1
loop_
_audit_author_email
conrad.goodwin@manchester.ac.uk
jon.kragskow@student.manchester.ac.uk
david.mills@manchester.ac.uk
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H84 I N2 Si4 Sm, 0.5(C6 H14)'
_chemical_formula_sum 'C39 H91 I N2 Si4 Sm'
_chemical_formula_weight 977.74
_chemical_melting_point ?
_chemical_oxdiff_formula Sm(N(SiC9H21)2)2I
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'
I I -0.4742 1.8119 '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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 56
_space_group_name_H-M_alt 'P c c n'
_space_group_name_Hall '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
_cell_length_a 20.0340(4)
_cell_length_b 20.2409(4)
_cell_length_c 24.0385(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 9747.8(3)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 11905
_cell_measurement_temperature 150.01(10)
_cell_measurement_theta_max 28.6260
_cell_measurement_theta_min 2.6340
_shelx_estimated_absorpt_T_max 0.757
_shelx_estimated_absorpt_T_min 0.522
_exptl_absorpt_coefficient_mu 1.963
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.561
_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 yellow'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.332
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 4080
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-25 -10 12 0.1066
2 6 -33 0.1183
21 10 -19 0.1090
-12 -2 -31 0.1432
-1 29 1 0.0557
-3 -6 33 0.1105
-1 -28 -6 0.0730
15 1 29 0.1326
24 10 -13 0.1131
_exptl_crystal_preparation 'By Jon Kragskow and CAPG.'
_exptl_crystal_recrystallization_method 'From hexane.'
_exptl_crystal_size_max 0.381
_exptl_crystal_size_mid 0.231
_exptl_crystal_size_min 0.15
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
-25.0028 -10.0023 12.0025 0.0854 -1.0111 -0.0485
1.9997 6.0038 -33.0038 -0.0612 0.5110 -0.8557
21.0022 10.0029 -19.0031 -0.0920 0.9705 -0.1987
-12.0019 -1.9974 -31.0030 0.0855 -0.0213 -1.0077
-1.0012 29.0038 1.0013 -0.9913 0.2270 -0.0052
-2.9998 -6.0038 33.0039 0.0529 -0.5420 0.8407
-0.9991 -28.0031 -6.0018 0.9599 -0.2201 -0.1591
15.0023 0.9974 29.0026 -0.0194 0.1288 0.9998
24.0027 10.0024 -13.0026 -0.0899 0.9921 0.0067
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0478
_diffrn_reflns_av_unetI/netI 0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 39822
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.350
_diffrn_reflns_theta_min 2.217
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 150.01(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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 -34.00 39.80 0.90 2.00 -- -17.77 57.00 120.00 82
2 \w -80.00 -53.00 0.90 2.00 -- -17.77 137.00 16.00 30
3 \w 1.00 40.60 0.90 2.00 -- 18.86 -37.00-180.00 44
4 \w -86.00 11.20 0.90 2.00 -- -17.77 -77.00-180.00 108
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0082720000
_diffrn_orient_matrix_UB_12 -0.0337615000
_diffrn_orient_matrix_UB_13 -0.0037865000
_diffrn_orient_matrix_UB_21 0.0309992000
_diffrn_orient_matrix_UB_22 0.0093072000
_diffrn_orient_matrix_UB_23 -0.0119125000
_diffrn_orient_matrix_UB_31 0.0150047000
_diffrn_orient_matrix_UB_32 -0.0005845000
_diffrn_orient_matrix_UB_33 0.0267312000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7087
_reflns_number_total 8929
_reflns_odcompleteness_completeness 99.88
_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 1.172
_refine_diff_density_min -0.564
_refine_diff_density_rms 0.103
_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 8929
_refine_ls_number_restraints 9
_refine_ls_R_factor_all 0.0488
_refine_ls_R_factor_gt 0.0342
_refine_ls_restrained_S_all 1.050
_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^)+(0.0194P)^2^+11.4398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0659
_refine_ls_wR_factor_ref 0.0731
_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
C38-C37 = C38-C39 = C39-C40 = C40-C41 = C42-C41
1.51 with sigma of 0.01
C37-C39
2.45 with sigma of 0.01
C38-C40
2.45 with sigma of 0.01
C39-C41
2.45 with sigma of 0.01
C40-C42
2.45 with sigma of 0.01
3. Others
Fixed Sof: C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C38(0.5) H38A(0.5)
H38B(0.5) C39(0.5) H39A(0.5) H39B(0.5) C40(0.5) H40A(0.5) H40B(0.5) C41(0.5)
H41A(0.5) H41B(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5)
4.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)
4.b Secondary CH2 refined with riding coordinates:
C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B)
4.c Me refined with riding coordinates:
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), C37(H37A,H37B,H37C), C42(H42A,H42B,H42C)
;
_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
Sm1 Sm 0.44591(2) 0.54426(2) 0.73081(2) 0.01626(6) Uani 1 1 d . . . . .
I1 I 0.55633(2) 0.44435(2) 0.71512(2) 0.02690(8) Uani 1 1 d . . . . .
Si1 Si 0.45971(5) 0.66455(5) 0.82560(4) 0.0172(2) Uani 1 1 d . . . . .
Si2 Si 0.39064(5) 0.53210(6) 0.86746(4) 0.0182(2) Uani 1 1 d . . . . .
Si3 Si 0.31682(5) 0.52288(6) 0.64466(4) 0.0169(2) Uani 1 1 d . . . . .
Si4 Si 0.42889(5) 0.61777(5) 0.59982(4) 0.0165(2) Uani 1 1 d . . . . .
N1 N 0.42469(13) 0.58693(15) 0.81880(12) 0.0154(7) Uani 1 1 d . . . . .
N2 N 0.39111(14) 0.56659(15) 0.64950(12) 0.0164(7) Uani 1 1 d . . . . .
C1 C 0.50969(19) 0.6755(2) 0.75755(15) 0.0223(9) Uani 1 1 d . . . . .
H1 H 0.480812 0.659471 0.727555 0.027 Uiso 1 1 calc R . . . .
C2 C 0.57345(18) 0.6334(2) 0.75518(17) 0.0294(10) Uani 1 1 d . . . . .
H2A H 0.562858 0.588461 0.764469 0.044 Uiso 1 1 calc R . . . .
H2B H 0.591842 0.635076 0.718330 0.044 Uiso 1 1 calc R . . . .
H2C H 0.605475 0.650281 0.781258 0.044 Uiso 1 1 calc R . . . .
C3 C 0.5277(2) 0.7472(2) 0.74257(17) 0.0356(11) Uani 1 1 d . . . . .
H3A H 0.488219 0.774032 0.743911 0.053 Uiso 1 1 calc R . . . .
H3B H 0.559846 0.763717 0.768692 0.053 Uiso 1 1 calc R . . . .
H3C H 0.546213 0.748512 0.705764 0.053 Uiso 1 1 calc R . . . .
C4 C 0.40270(19) 0.7390(2) 0.82732(15) 0.0262(10) Uani 1 1 d . . . . .
H4 H 0.432633 0.776896 0.822694 0.031 Uiso 1 1 calc R . . . .
C5 C 0.3547(2) 0.7431(2) 0.77741(17) 0.0368(12) Uani 1 1 d . . . . .
H5A H 0.378683 0.734024 0.743716 0.055 Uiso 1 1 calc R . . . .
H5B H 0.319558 0.711292 0.781907 0.055 Uiso 1 1 calc R . . . .
H5C H 0.335785 0.786674 0.775487 0.055 Uiso 1 1 calc R . . . .
C6 C 0.3646(2) 0.7535(2) 0.88101(16) 0.0355(11) Uani 1 1 d . . . . .
H6A H 0.394572 0.750894 0.912066 0.053 Uiso 1 1 calc R . . . .
H6B H 0.345701 0.797033 0.879130 0.053 Uiso 1 1 calc R . . . .
H6C H 0.329473 0.721650 0.885549 0.053 Uiso 1 1 calc R . . . .
C7 C 0.51820(18) 0.6748(2) 0.88759(15) 0.0222(9) Uani 1 1 d . . . . .
H7 H 0.489557 0.670579 0.920445 0.027 Uiso 1 1 calc R . . . .
C8 C 0.57288(18) 0.6227(2) 0.89538(16) 0.0282(10) Uani 1 1 d . . . . .
H8A H 0.553692 0.579374 0.892516 0.042 Uiso 1 1 calc R . . . .
H8B H 0.606299 0.628140 0.867124 0.042 Uiso 1 1 calc R . . . .
H8C H 0.592932 0.627952 0.931381 0.042 Uiso 1 1 calc R . . . .
C9 C 0.5499(2) 0.7439(2) 0.89231(17) 0.0345(11) Uani 1 1 d . . . . .
H9A H 0.516100 0.776980 0.887493 0.052 Uiso 1 1 calc R . . . .
H9B H 0.570051 0.748774 0.928325 0.052 Uiso 1 1 calc R . . . .
H9C H 0.583418 0.748961 0.864068 0.052 Uiso 1 1 calc R . . . .
C10 C 0.42609(18) 0.44850(19) 0.84559(16) 0.0218(9) Uani 1 1 d . . . . .
H10 H 0.426494 0.449697 0.804833 0.026 Uiso 1 1 calc R . . . .
C11 C 0.49960(19) 0.4396(2) 0.86230(17) 0.0304(10) Uani 1 1 d . . . . .
H11A H 0.524156 0.478825 0.852951 0.046 Uiso 1 1 calc R . . . .
H11B H 0.502454 0.431998 0.901646 0.046 Uiso 1 1 calc R . . . .
H11C H 0.518114 0.402561 0.842753 0.046 Uiso 1 1 calc R . . . .
C12 C 0.3863(2) 0.3859(2) 0.86043(18) 0.0323(11) Uani 1 1 d . . . . .
H12A H 0.340455 0.391683 0.849904 0.048 Uiso 1 1 calc R . . . .
H12B H 0.404651 0.348711 0.840881 0.048 Uiso 1 1 calc R . . . .
H12C H 0.388990 0.378148 0.899773 0.048 Uiso 1 1 calc R . . . .
C13 C 0.29576(18) 0.5276(2) 0.86073(16) 0.0242(9) Uani 1 1 d . . . . .
H13 H 0.287350 0.504873 0.825426 0.029 Uiso 1 1 calc R . . . .
C14 C 0.26189(19) 0.5947(2) 0.85524(16) 0.0316(11) Uani 1 1 d . . . . .
H14A H 0.284724 0.620513 0.827692 0.047 Uiso 1 1 calc R . . . .
H14B H 0.216258 0.588548 0.844205 0.047 Uiso 1 1 calc R . . . .
H14C H 0.263357 0.617181 0.890366 0.047 Uiso 1 1 calc R . . . .
C15 C 0.25825(19) 0.4873(2) 0.90504(17) 0.0354(11) Uani 1 1 d . . . . .
H15A H 0.278982 0.444797 0.909038 0.053 Uiso 1 1 calc R . . . .
H15B H 0.259728 0.510275 0.939953 0.053 Uiso 1 1 calc R . . . .
H15C H 0.212628 0.481642 0.893791 0.053 Uiso 1 1 calc R . . . .
C16 C 0.41446(19) 0.5479(2) 0.94281(15) 0.0223(9) Uani 1 1 d . . . . .
H16 H 0.461796 0.560122 0.942578 0.027 Uiso 1 1 calc R . . . .
C17 C 0.3772(2) 0.6058(2) 0.96972(16) 0.0296(10) Uani 1 1 d . . . . .
H17A H 0.380384 0.643976 0.946111 0.044 Uiso 1 1 calc R . . . .
H17B H 0.331129 0.594256 0.974664 0.044 Uiso 1 1 calc R . . . .
H17C H 0.396806 0.615596 1.005227 0.044 Uiso 1 1 calc R . . . .
C18 C 0.4083(2) 0.4879(2) 0.98164(16) 0.0324(11) Uani 1 1 d . . . . .
H18A H 0.431353 0.450950 0.965590 0.049 Uiso 1 1 calc R . . . .
H18B H 0.427751 0.498341 1.017084 0.049 Uiso 1 1 calc R . . . .
H18C H 0.362073 0.477001 0.986521 0.049 Uiso 1 1 calc R . . . .
C19 C 0.31539(18) 0.4675(2) 0.70950(16) 0.0223(9) Uani 1 1 d . . . . .
H19 H 0.332338 0.494402 0.740292 0.027 Uiso 1 1 calc R . . . .
C20 C 0.3617(2) 0.4071(2) 0.70524(18) 0.0313(10) Uani 1 1 d . . . . .
H20A H 0.405574 0.421268 0.694424 0.047 Uiso 1 1 calc R . . . .
H20B H 0.364004 0.385409 0.740695 0.047 Uiso 1 1 calc R . . . .
H20C H 0.344498 0.376986 0.677939 0.047 Uiso 1 1 calc R . . . .
C21 C 0.24524(19) 0.4439(2) 0.72689(16) 0.0304(11) Uani 1 1 d . . . . .
H21A H 0.215889 0.481234 0.729667 0.046 Uiso 1 1 calc R . . . .
H21B H 0.228322 0.413661 0.699529 0.046 Uiso 1 1 calc R . . . .
H21C H 0.247828 0.422085 0.762286 0.046 Uiso 1 1 calc R . . . .
C22 C 0.24476(18) 0.5828(2) 0.64814(15) 0.0225(9) Uani 1 1 d . . . . .
H22 H 0.257719 0.619368 0.623713 0.027 Uiso 1 1 calc R . . . .
C23 C 0.23954(19) 0.6135(2) 0.70608(16) 0.0302(10) Uani 1 1 d . . . . .
H23A H 0.283150 0.626403 0.718584 0.045 Uiso 1 1 calc R . . . .
H23B H 0.211129 0.651691 0.704555 0.045 Uiso 1 1 calc R . . . .
H23C H 0.221052 0.581829 0.731467 0.045 Uiso 1 1 calc R . . . .
C24 C 0.17535(19) 0.5621(2) 0.62789(19) 0.0361(11) Uani 1 1 d . . . . .
H24A H 0.178888 0.542855 0.591518 0.054 Uiso 1 1 calc R . . . .
H24B H 0.156786 0.530354 0.653186 0.054 Uiso 1 1 calc R . . . .
H24C H 0.146863 0.600215 0.626274 0.054 Uiso 1 1 calc R . . . .
C25 C 0.30939(17) 0.4686(2) 0.58047(16) 0.0232(9) Uani 1 1 d . . . . .
H25 H 0.301053 0.499169 0.549625 0.028 Uiso 1 1 calc R . . . .
C26 C 0.37227(19) 0.4301(2) 0.56378(17) 0.0318(11) Uani 1 1 d . . . . .
H26A H 0.410007 0.459330 0.563787 0.048 Uiso 1 1 calc R . . . .
H26B H 0.379756 0.394973 0.589880 0.048 Uiso 1 1 calc R . . . .
H26C H 0.366394 0.411900 0.527223 0.048 Uiso 1 1 calc R . . . .
C27 C 0.24976(19) 0.4204(2) 0.58007(17) 0.0327(11) Uani 1 1 d . . . . .
H27A H 0.209878 0.443639 0.590425 0.049 Uiso 1 1 calc R . . . .
H27B H 0.244469 0.402260 0.543437 0.049 Uiso 1 1 calc R . . . .
H27C H 0.257831 0.385333 0.606093 0.049 Uiso 1 1 calc R . . . .
C28 C 0.52143(17) 0.5968(2) 0.60774(16) 0.0221(9) Uani 1 1 d . . . . .
H28 H 0.527121 0.588517 0.647621 0.027 Uiso 1 1 calc R . . . .
C29 C 0.53973(18) 0.5310(2) 0.57999(16) 0.0263(10) Uani 1 1 d . . . . .
H29A H 0.506454 0.498551 0.588772 0.039 Uiso 1 1 calc R . . . .
H29B H 0.541813 0.536952 0.540408 0.039 Uiso 1 1 calc R . . . .
H29C H 0.582378 0.516460 0.593440 0.039 Uiso 1 1 calc R . . . .
C30 C 0.57399(19) 0.6491(2) 0.59413(18) 0.0319(11) Uani 1 1 d . . . . .
H30A H 0.562133 0.690055 0.611655 0.048 Uiso 1 1 calc R . . . .
H30B H 0.616719 0.634770 0.607607 0.048 Uiso 1 1 calc R . . . .
H30C H 0.576155 0.655261 0.554575 0.048 Uiso 1 1 calc R . . . .
C31 C 0.40257(17) 0.6019(2) 0.52462(15) 0.0202(9) Uani 1 1 d . . . . .
H31 H 0.401162 0.553872 0.519909 0.024 Uiso 1 1 calc R . . . .
C32 C 0.33268(18) 0.6279(2) 0.50893(15) 0.0279(10) Uani 1 1 d . . . . .
H32A H 0.300540 0.612089 0.535384 0.042 Uiso 1 1 calc R . . . .
H32B H 0.332987 0.675325 0.509181 0.042 Uiso 1 1 calc R . . . .
H32C H 0.321026 0.612436 0.472444 0.042 Uiso 1 1 calc R . . . .
C33 C 0.45263(19) 0.6282(2) 0.48139(16) 0.0286(10) Uani 1 1 d . . . . .
H33A H 0.496604 0.612670 0.490338 0.043 Uiso 1 1 calc R . . . .
H33B H 0.440274 0.612769 0.445071 0.043 Uiso 1 1 calc R . . . .
H33C H 0.452235 0.675658 0.481807 0.043 Uiso 1 1 calc R . . . .
C34 C 0.41676(18) 0.70916(19) 0.61675(15) 0.0211(9) Uani 1 1 d . . . . .
H34 H 0.442068 0.717268 0.650965 0.025 Uiso 1 1 calc R . . . .
C35 C 0.34441(19) 0.7290(2) 0.62963(17) 0.0304(10) Uani 1 1 d . . . . .
H35A H 0.326051 0.699183 0.656644 0.046 Uiso 1 1 calc R . . . .
H35B H 0.343582 0.773193 0.644154 0.046 Uiso 1 1 calc R . . . .
H35C H 0.318363 0.727094 0.596149 0.046 Uiso 1 1 calc R . . . .
C36 C 0.4443(2) 0.7582(2) 0.57334(17) 0.0336(11) Uani 1 1 d . . . . .
H36A H 0.489620 0.746785 0.564550 0.050 Uiso 1 1 calc R . . . .
H36B H 0.417623 0.756041 0.540221 0.050 Uiso 1 1 calc R . . . .
H36C H 0.442842 0.802141 0.588227 0.050 Uiso 1 1 calc R . . . .
C37 C 0.2388(12) 0.2541(16) 0.7451(4) 0.110(6) Uiso 0.5 1 d D . P A -1
H37A H 0.265115 0.236838 0.715117 0.165 Uiso 0.5 1 calc R . P A -1
H37B H 0.194985 0.234874 0.743998 0.165 Uiso 0.5 1 calc R . P A -1
H37C H 0.235251 0.301216 0.741481 0.165 Uiso 0.5 1 calc R . P A -1
C38 C 0.2714(6) 0.2376(8) 0.7994(4) 0.093(5) Uiso 0.5 1 d D . P A -1
H38A H 0.275680 0.190022 0.802385 0.112 Uiso 0.5 1 calc R . P A -1
H38B H 0.315941 0.256356 0.799868 0.112 Uiso 0.5 1 calc R . P A -1
C39 C 0.2336(6) 0.2627(8) 0.8481(4) 0.081(4) Uiso 0.5 1 d D . P A -1
H39A H 0.229598 0.310381 0.845465 0.097 Uiso 0.5 1 calc R . P A -1
H39B H 0.188909 0.244181 0.847703 0.097 Uiso 0.5 1 calc R . P A -1
C40 C 0.2669(7) 0.2451(10) 0.9009(4) 0.092(5) Uiso 0.5 1 d D . P A -1
H40A H 0.272296 0.197551 0.902357 0.110 Uiso 0.5 1 calc R . P A -1
H40B H 0.311155 0.264631 0.901130 0.110 Uiso 0.5 1 calc R . P A -1
C41 C 0.2314(7) 0.2666(9) 0.9508(5) 0.118(6) Uiso 0.5 1 d D . P A -1
H41A H 0.188362 0.244734 0.952326 0.142 Uiso 0.5 1 calc R . P A -1
H41B H 0.223560 0.313802 0.948685 0.142 Uiso 0.5 1 calc R . P A -1
C42 C 0.2697(9) 0.2514(14) 1.0034(4) 0.156(9) Uiso 0.5 1 d D . P A -1
H42A H 0.244699 0.266214 1.035021 0.234 Uiso 0.5 1 calc R . P A -1
H42B H 0.276863 0.204560 1.006048 0.234 Uiso 0.5 1 calc R . P A -1
H42C H 0.312049 0.273605 1.002408 0.234 Uiso 0.5 1 calc R . P A -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sm1 0.01682(11) 0.01678(12) 0.01518(11) -0.00028(8) -0.00042(7) 0.00357(8)
I1 0.02339(15) 0.02618(17) 0.03113(16) 0.00135(12) 0.00251(11) 0.00984(12)
Si1 0.0217(6) 0.0134(6) 0.0166(6) -0.0006(5) -0.0028(4) 0.0024(5)
Si2 0.0182(6) 0.0181(6) 0.0182(6) 0.0001(5) 0.0023(4) 0.0011(5)
Si3 0.0156(5) 0.0195(6) 0.0156(5) -0.0004(5) 0.0009(4) -0.0008(4)
Si4 0.0185(5) 0.0155(6) 0.0156(5) 0.0004(5) 0.0012(4) -0.0006(4)
N1 0.0163(16) 0.0149(18) 0.0150(16) -0.0017(14) -0.0002(12) 0.0021(13)
N2 0.0160(16) 0.0170(19) 0.0163(17) -0.0009(14) 0.0012(12) -0.0002(13)
C1 0.030(2) 0.017(2) 0.020(2) 0.0003(18) -0.0021(16) -0.0059(18)
C2 0.028(2) 0.032(3) 0.028(2) -0.003(2) 0.0054(17) -0.005(2)
C3 0.052(3) 0.023(3) 0.031(3) 0.004(2) 0.004(2) -0.014(2)
C4 0.031(2) 0.022(2) 0.026(2) -0.0012(19) -0.0069(17) 0.0035(19)
C5 0.045(3) 0.029(3) 0.037(3) 0.002(2) -0.016(2) 0.014(2)
C6 0.044(3) 0.030(3) 0.032(3) -0.007(2) -0.0040(19) 0.011(2)
C7 0.021(2) 0.026(3) 0.019(2) 0.0000(18) -0.0024(15) 0.0012(18)
C8 0.025(2) 0.031(3) 0.028(2) 0.006(2) -0.0078(17) -0.0011(19)
C9 0.041(3) 0.029(3) 0.034(3) -0.004(2) -0.0097(19) -0.007(2)
C10 0.027(2) 0.016(2) 0.022(2) 0.0004(18) 0.0018(16) -0.0004(17)
C11 0.034(2) 0.030(3) 0.027(2) -0.001(2) -0.0015(18) 0.012(2)
C12 0.039(3) 0.020(3) 0.037(3) -0.001(2) 0.0091(19) -0.004(2)
C13 0.025(2) 0.028(3) 0.020(2) -0.0072(19) 0.0010(16) -0.0018(19)
C14 0.023(2) 0.046(3) 0.025(2) 0.005(2) 0.0009(17) 0.004(2)
C15 0.024(2) 0.037(3) 0.045(3) -0.001(2) 0.0144(19) -0.002(2)
C16 0.027(2) 0.021(2) 0.018(2) 0.0046(18) -0.0013(16) 0.0011(18)
C17 0.037(2) 0.032(3) 0.020(2) -0.001(2) -0.0014(17) -0.001(2)
C18 0.040(3) 0.034(3) 0.023(2) 0.005(2) 0.0036(18) 0.001(2)
C19 0.022(2) 0.024(2) 0.021(2) -0.0011(18) 0.0006(16) -0.0123(18)
C20 0.037(3) 0.024(3) 0.033(3) 0.006(2) -0.0055(19) -0.005(2)
C21 0.026(2) 0.038(3) 0.028(2) 0.009(2) 0.0030(17) -0.012(2)
C22 0.022(2) 0.024(2) 0.022(2) 0.0016(18) 0.0016(16) 0.0027(18)
C23 0.028(2) 0.035(3) 0.027(2) -0.004(2) 0.0074(17) 0.006(2)
C24 0.024(2) 0.039(3) 0.045(3) -0.002(2) -0.0061(19) 0.007(2)
C25 0.021(2) 0.029(3) 0.019(2) -0.0015(19) 0.0000(15) -0.0027(18)
C26 0.034(2) 0.032(3) 0.029(2) -0.009(2) 0.0074(18) -0.002(2)
C27 0.030(2) 0.036(3) 0.032(2) -0.009(2) -0.0007(19) -0.011(2)
C28 0.020(2) 0.029(3) 0.017(2) -0.0006(18) 0.0004(15) -0.0022(18)
C29 0.021(2) 0.030(3) 0.027(2) 0.001(2) 0.0028(16) 0.0042(19)
C30 0.025(2) 0.034(3) 0.037(3) -0.002(2) 0.0038(18) -0.008(2)
C31 0.026(2) 0.016(2) 0.018(2) -0.0023(18) 0.0024(15) -0.0022(17)
C32 0.029(2) 0.036(3) 0.019(2) 0.001(2) -0.0008(16) -0.002(2)
C33 0.033(2) 0.032(3) 0.021(2) 0.002(2) 0.0049(17) 0.002(2)
C34 0.030(2) 0.014(2) 0.019(2) 0.0012(17) -0.0037(16) -0.0013(17)
C35 0.042(3) 0.017(2) 0.032(2) -0.001(2) 0.0000(19) 0.007(2)
C36 0.048(3) 0.020(3) 0.033(3) 0.006(2) 0.002(2) -0.004(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 I1 3.0207(3) . ?
Sm1 N1 2.324(3) . ?
Sm1 N2 2.287(3) . ?
Sm1 C1 3.018(4) . ?
Si1 N1 1.728(3) . ?
Si1 C1 1.931(4) . ?
Si1 C4 1.891(4) . ?
Si1 C7 1.907(4) . ?
Si2 N1 1.751(3) . ?
Si2 C10 1.909(4) . ?
Si2 C13 1.910(4) . ?
Si2 C16 1.900(4) . ?
Si3 N2 1.735(3) . ?
Si3 C19 1.920(4) . ?
Si3 C22 1.887(4) . ?
Si3 C25 1.900(4) . ?
Si4 N2 1.753(3) . ?
Si4 C28 1.911(4) . ?
Si4 C31 1.910(4) . ?
Si4 C34 1.910(4) . ?
C1 H1 0.9800 . ?
C1 C2 1.537(5) . ?
C1 C3 1.537(5) . ?
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 1.540(5) . ?
C4 C6 1.528(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 1.532(5) . ?
C7 C9 1.541(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 1.537(5) . ?
C10 C12 1.539(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 1.523(5) . ?
C13 C15 1.538(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 1.533(5) . ?
C16 C18 1.536(5) . ?
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 1.542(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 1.529(5) . ?
C22 C24 1.532(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 1.535(5) . ?
C25 C27 1.542(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 1.534(5) . ?
C28 C30 1.528(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 1.542(5) . ?
C31 C33 1.539(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 1.536(5) . ?
C34 C36 1.542(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 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C37 C38 1.496(8) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C39 1.484(8) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.479(8) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C41 1.461(8) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.510(9) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 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
N1 Sm1 I1 119.76(7) . . ?
N1 Sm1 C1 63.66(10) . . ?
N2 Sm1 I1 112.16(7) . . ?
N2 Sm1 N1 128.06(10) . . ?
N2 Sm1 C1 102.20(11) . . ?
C1 Sm1 I1 107.82(7) . . ?
N1 Si1 C1 103.60(16) . . ?
N1 Si1 C4 118.76(16) . . ?
N1 Si1 C7 114.96(16) . . ?
C4 Si1 C1 103.89(18) . . ?
C4 Si1 C7 105.52(17) . . ?
C7 Si1 C1 109.32(17) . . ?
N1 Si2 C10 103.47(16) . . ?
N1 Si2 C13 111.18(16) . . ?
N1 Si2 C16 115.62(16) . . ?
C10 Si2 C13 107.74(18) . . ?
C16 Si2 C10 108.56(17) . . ?
C16 Si2 C13 109.80(17) . . ?
N2 Si3 C19 104.84(15) . . ?
N2 Si3 C22 108.99(17) . . ?
N2 Si3 C25 114.61(15) . . ?
C22 Si3 C19 109.14(17) . . ?
C22 Si3 C25 110.34(17) . . ?
C25 Si3 C19 108.68(18) . . ?
N2 Si4 C28 102.71(16) . . ?
N2 Si4 C31 115.24(16) . . ?
N2 Si4 C34 111.86(16) . . ?
C31 Si4 C28 108.96(16) . . ?
C34 Si4 C28 108.48(17) . . ?
C34 Si4 C31 109.21(17) . . ?
Si1 N1 Sm1 110.47(14) . . ?
Si1 N1 Si2 132.15(18) . . ?
Si2 N1 Sm1 116.35(15) . . ?
Si3 N2 Sm1 111.61(15) . . ?
Si3 N2 Si4 128.76(17) . . ?
Si4 N2 Sm1 119.46(14) . . ?
Sm1 C1 H1 45.7 . . ?
Si1 C1 Sm1 81.93(13) . . ?
Si1 C1 H1 106.2 . . ?
C2 C1 Sm1 81.7(2) . . ?
C2 C1 Si1 113.5(3) . . ?
C2 C1 H1 106.2 . . ?
C3 C1 Sm1 151.7(3) . . ?
C3 C1 Si1 115.4(3) . . ?
C3 C1 H1 106.2 . . ?
C3 C1 C2 108.7(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 104.6 . . ?
C5 C4 Si1 113.8(3) . . ?
C5 C4 H4 104.6 . . ?
C6 C4 Si1 118.2(3) . . ?
C6 C4 H4 104.6 . . ?
C6 C4 C5 109.6(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 105.1 . . ?
C8 C7 Si1 117.4(3) . . ?
C8 C7 H7 105.1 . . ?
C8 C7 C9 108.7(3) . . ?
C9 C7 Si1 114.2(3) . . ?
C9 C7 H7 105.1 . . ?
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 104.9 . . ?
C11 C10 Si2 112.8(3) . . ?
C11 C10 H10 104.9 . . ?
C11 C10 C12 109.8(3) . . ?
C12 C10 Si2 118.3(3) . . ?
C12 C10 H10 104.9 . . ?
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 105.5 . . ?
C14 C13 Si2 114.1(3) . . ?
C14 C13 H13 105.5 . . ?
C14 C13 C15 108.4(3) . . ?
C15 C13 Si2 116.9(3) . . ?
C15 C13 H13 105.5 . . ?
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 106.3 . . ?
C17 C16 Si2 114.1(3) . . ?
C17 C16 H16 106.3 . . ?
C17 C16 C18 108.0(3) . . ?
C18 C16 Si2 115.2(3) . . ?
C18 C16 H16 106.3 . . ?
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 106.4 . . ?
C20 C19 Si3 113.6(3) . . ?
C20 C19 H19 106.4 . . ?
C20 C19 C21 108.8(3) . . ?
C21 C19 Si3 114.5(3) . . ?
C21 C19 H19 106.4 . . ?
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 104.9 . . ?
C23 C22 Si3 110.8(3) . . ?
C23 C22 H22 104.9 . . ?
C23 C22 C24 109.8(3) . . ?
C24 C22 Si3 120.3(3) . . ?
C24 C22 H22 104.9 . . ?
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 105.2 . . ?
C26 C25 Si3 116.2(3) . . ?
C26 C25 H25 105.2 . . ?
C26 C25 C27 108.2(3) . . ?
C27 C25 Si3 115.6(3) . . ?
C27 C25 H25 105.2 . . ?
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 104.4 . . ?
C29 C28 Si4 112.4(3) . . ?
C29 C28 H28 104.4 . . ?
C30 C28 Si4 119.6(3) . . ?
C30 C28 H28 104.4 . . ?
C30 C28 C29 110.1(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 106.5 . . ?
C32 C31 Si4 115.2(3) . . ?
C32 C31 H31 106.5 . . ?
C33 C31 Si4 113.6(3) . . ?
C33 C31 H31 106.5 . . ?
C33 C31 C32 108.0(3) . . ?
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 114.6(3) . . ?
C35 C34 H34 106.0 . . ?
C35 C34 C36 107.8(3) . . ?
C36 C34 Si4 115.7(3) . . ?
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 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
C37 C38 H38A 109.0 . . ?
C37 C38 H38B 109.0 . . ?
H38A C38 H38B 107.8 . . ?
C39 C38 C37 112.8(8) . . ?
C39 C38 H38A 109.0 . . ?
C39 C38 H38B 109.0 . . ?
C38 C39 H39A 109.4 . . ?
C38 C39 H39B 109.4 . . ?
H39A C39 H39B 108.0 . . ?
C40 C39 C38 111.4(7) . . ?
C40 C39 H39A 109.4 . . ?
C40 C39 H39B 109.4 . . ?
C39 C40 H40A 108.6 . . ?
C39 C40 H40B 108.6 . . ?
H40A C40 H40B 107.6 . . ?
C41 C40 C39 114.5(8) . . ?
C41 C40 H40A 108.6 . . ?
C41 C40 H40B 108.6 . . ?
C40 C41 H41A 109.2 . . ?
C40 C41 H41B 109.2 . . ?
C40 C41 C42 112.3(8) . . ?
H41A C41 H41B 107.9 . . ?
C42 C41 H41A 109.2 . . ?
C42 C41 H41B 109.2 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
_shelx_res_file
;
TITL adpm350_a.res in Pccn
adpm350.res
created by SHELXL-2018/1 at 11:28:08 on 28-Apr-2018
REM Old TITL adpm350 in Pccn
REM SHELXT solution in Pccn
REM R1 0.098, Rweak 0.003, Alpha 0.026, Orientation as input
REM Formula found by SHELXT: C72 N5 Si8 I2 Sm2
CELL 0.71073 20.034 20.2409 24.0385 90 90 90
ZERR 8 0.0004 0.0004 0.0005 0 0 0
LATT 1
SYMM 0.5-X,0.5-Y,+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,-Y,0.5-Z
SFAC C H I N Si Sm
UNIT 312 728 8 16 32 8
EQIV $1 0.5-X,0.5-Y,+Z
DFIX 1.51 0.01 C38 C37 C38 C39 C39 C40 C40 C41 C42 C41
DFIX 2.45 0.01 C37 C39
DFIX 2.45 0.01 C38 C40
DFIX 2.45 0.01 C39 C41
DFIX 2.45 0.01 C40 C42
L.S. 10
PLAN 20
SIZE 0.15 0.231 0.381
CONN 20 Sm1
FREE Sm1 Si3
FREE Sm1 Si1
FREE C39 C41_$1
FREE C39 C41
FREE C38 C40_$1
FREE C38 C40
BOND $H
list 4
fmap 2
acta
SHEL 100 0.83
REM
REM
REM
WGHT 0.019400 11.439799
FVAR 1.07848
SM1 6 0.445915 0.544257 0.730806 11.00000 0.01682 0.01678 =
0.01518 -0.00028 -0.00042 0.00357
I1 3 0.556328 0.444347 0.715119 11.00000 0.02339 0.02618 =
0.03113 0.00135 0.00251 0.00984
SI1 5 0.459710 0.664551 0.825596 11.00000 0.02167 0.01344 =
0.01661 -0.00060 -0.00282 0.00237
SI2 5 0.390644 0.532102 0.867462 11.00000 0.01821 0.01810 =
0.01819 0.00013 0.00228 0.00108
SI3 5 0.316822 0.522877 0.644661 11.00000 0.01557 0.01954 =
0.01564 -0.00038 0.00095 -0.00081
SI4 5 0.428892 0.617769 0.599820 11.00000 0.01848 0.01547 =
0.01560 0.00037 0.00123 -0.00061
N1 4 0.424690 0.586929 0.818797 11.00000 0.01628 0.01494 =
0.01504 -0.00171 -0.00021 0.00211
N2 4 0.391111 0.566593 0.649501 11.00000 0.01595 0.01705 =
0.01634 -0.00091 0.00117 -0.00016
C1 1 0.509687 0.675535 0.757553 11.00000 0.02975 0.01690 =
0.02032 0.00025 -0.00213 -0.00589
AFIX 13
H1 2 0.480812 0.659471 0.727555 11.00000 -1.20000
AFIX 0
C2 1 0.573452 0.633381 0.755180 11.00000 0.02838 0.03222 =
0.02765 -0.00326 0.00538 -0.00495
AFIX 33
H2A 2 0.562858 0.588461 0.764469 11.00000 -1.50000
H2B 2 0.591842 0.635076 0.718330 11.00000 -1.50000
H2C 2 0.605475 0.650281 0.781258 11.00000 -1.50000
AFIX 0
C3 1 0.527680 0.747172 0.742574 11.00000 0.05228 0.02320 =
0.03136 0.00390 0.00408 -0.01372
AFIX 33
H3A 2 0.488219 0.774032 0.743911 11.00000 -1.50000
H3B 2 0.559846 0.763717 0.768692 11.00000 -1.50000
H3C 2 0.546213 0.748512 0.705764 11.00000 -1.50000
AFIX 0
C4 1 0.402695 0.739002 0.827318 11.00000 0.03053 0.02211 =
0.02605 -0.00119 -0.00686 0.00349
AFIX 13
H4 2 0.432633 0.776896 0.822694 11.00000 -1.20000
AFIX 0
C5 1 0.354655 0.743138 0.777405 11.00000 0.04519 0.02854 =
0.03657 0.00200 -0.01615 0.01421
AFIX 33
H5A 2 0.378683 0.734024 0.743716 11.00000 -1.50000
H5B 2 0.319558 0.711292 0.781907 11.00000 -1.50000
H5C 2 0.335785 0.786674 0.775487 11.00000 -1.50000
AFIX 0
C6 1 0.364567 0.753491 0.881005 11.00000 0.04396 0.03000 =
0.03242 -0.00706 -0.00404 0.01131
AFIX 33
H6A 2 0.394572 0.750894 0.912066 11.00000 -1.50000
H6B 2 0.345701 0.797033 0.879130 11.00000 -1.50000
H6C 2 0.329473 0.721650 0.885549 11.00000 -1.50000
AFIX 0
C7 1 0.518198 0.674768 0.887585 11.00000 0.02137 0.02579 =
0.01935 0.00004 -0.00237 0.00122
AFIX 13
H7 2 0.489557 0.670579 0.920445 11.00000 -1.20000
AFIX 0
C8 1 0.572883 0.622700 0.895379 11.00000 0.02548 0.03147 =
0.02758 0.00613 -0.00779 -0.00106
AFIX 33
H8A 2 0.553692 0.579374 0.892516 11.00000 -1.50000
H8B 2 0.606299 0.628140 0.867124 11.00000 -1.50000
H8C 2 0.592932 0.627952 0.931381 11.00000 -1.50000
AFIX 0
C9 1 0.549932 0.743885 0.892314 11.00000 0.04059 0.02866 =
0.03423 -0.00382 -0.00970 -0.00655
AFIX 33
H9A 2 0.516100 0.776980 0.887493 11.00000 -1.50000
H9B 2 0.570051 0.748774 0.928325 11.00000 -1.50000
H9C 2 0.583418 0.748961 0.864068 11.00000 -1.50000
AFIX 0
C10 1 0.426094 0.448497 0.845587 11.00000 0.02725 0.01562 =
0.02244 0.00042 0.00175 -0.00036
AFIX 13
H10 2 0.426494 0.449697 0.804833 11.00000 -1.20000
AFIX 0
C11 1 0.499604 0.439639 0.862303 11.00000 0.03431 0.02975 =
0.02720 -0.00143 -0.00153 0.01183
AFIX 33
H11A 2 0.524156 0.478825 0.852951 11.00000 -1.50000
H11B 2 0.502454 0.431998 0.901646 11.00000 -1.50000
H11C 2 0.518114 0.402561 0.842753 11.00000 -1.50000
AFIX 0
C12 1 0.386303 0.385866 0.860433 11.00000 0.03924 0.02046 =
0.03715 -0.00140 0.00912 -0.00438
AFIX 33
H12A 2 0.340455 0.391683 0.849904 11.00000 -1.50000
H12B 2 0.404651 0.348711 0.840881 11.00000 -1.50000
H12C 2 0.388990 0.378148 0.899773 11.00000 -1.50000
AFIX 0
C13 1 0.295756 0.527604 0.860733 11.00000 0.02514 0.02753 =
0.02004 -0.00721 0.00102 -0.00176
AFIX 13
H13 2 0.287350 0.504873 0.825426 11.00000 -1.20000
AFIX 0
C14 1 0.261894 0.594659 0.855242 11.00000 0.02344 0.04604 =
0.02531 0.00514 0.00090 0.00407
AFIX 33
H14A 2 0.284724 0.620513 0.827692 11.00000 -1.50000
H14B 2 0.216258 0.588548 0.844205 11.00000 -1.50000
H14C 2 0.263357 0.617181 0.890366 11.00000 -1.50000
AFIX 0
C15 1 0.258251 0.487293 0.905041 11.00000 0.02434 0.03681 =
0.04494 -0.00108 0.01440 -0.00247
AFIX 33
H15A 2 0.278982 0.444797 0.909038 11.00000 -1.50000
H15B 2 0.259728 0.510275 0.939953 11.00000 -1.50000
H15C 2 0.212628 0.481642 0.893791 11.00000 -1.50000
AFIX 0
C16 1 0.414464 0.547900 0.942805 11.00000 0.02741 0.02134 =
0.01821 0.00457 -0.00125 0.00109
AFIX 13
H16 2 0.461796 0.560122 0.942578 11.00000 -1.20000
AFIX 0
C17 1 0.377214 0.605849 0.969718 11.00000 0.03689 0.03173 =
0.02004 -0.00070 -0.00137 -0.00142
AFIX 33
H17A 2 0.380384 0.643976 0.946111 11.00000 -1.50000
H17B 2 0.331129 0.594256 0.974664 11.00000 -1.50000
H17C 2 0.396806 0.615596 1.005227 11.00000 -1.50000
AFIX 0
C18 1 0.408335 0.487923 0.981643 11.00000 0.03960 0.03426 =
0.02340 0.00501 0.00356 0.00149
AFIX 33
H18A 2 0.431353 0.450950 0.965590 11.00000 -1.50000
H18B 2 0.427751 0.498341 1.017084 11.00000 -1.50000
H18C 2 0.362073 0.477001 0.986521 11.00000 -1.50000
AFIX 0
C19 1 0.315394 0.467473 0.709495 11.00000 0.02185 0.02450 =
0.02065 -0.00107 0.00058 -0.01232
AFIX 13
H19 2 0.332338 0.494402 0.740292 11.00000 -1.20000
AFIX 0
C20 1 0.361718 0.407116 0.705238 11.00000 0.03674 0.02392 =
0.03333 0.00613 -0.00552 -0.00538
AFIX 33
H20A 2 0.405574 0.421268 0.694424 11.00000 -1.50000
H20B 2 0.364004 0.385409 0.740695 11.00000 -1.50000
H20C 2 0.344498 0.376986 0.677939 11.00000 -1.50000
AFIX 0
C21 1 0.245238 0.443888 0.726885 11.00000 0.02577 0.03758 =
0.02779 0.00949 0.00301 -0.01222
AFIX 33
H21A 2 0.215889 0.481234 0.729667 11.00000 -1.50000
H21B 2 0.228322 0.413661 0.699529 11.00000 -1.50000
H21C 2 0.247828 0.422085 0.762286 11.00000 -1.50000
AFIX 0
C22 1 0.244764 0.582787 0.648141 11.00000 0.02165 0.02421 =
0.02169 0.00159 0.00159 0.00270
AFIX 13
H22 2 0.257719 0.619368 0.623713 11.00000 -1.20000
AFIX 0
C23 1 0.239538 0.613539 0.706077 11.00000 0.02826 0.03494 =
0.02743 -0.00400 0.00744 0.00550
AFIX 33
H23A 2 0.283150 0.626403 0.718584 11.00000 -1.50000
H23B 2 0.211129 0.651691 0.704555 11.00000 -1.50000
H23C 2 0.221052 0.581829 0.731467 11.00000 -1.50000
AFIX 0
C24 1 0.175348 0.562125 0.627890 11.00000 0.02374 0.03944 =
0.04498 -0.00234 -0.00605 0.00706
AFIX 33
H24A 2 0.178888 0.542855 0.591518 11.00000 -1.50000
H24B 2 0.156786 0.530354 0.653186 11.00000 -1.50000
H24C 2 0.146863 0.600215 0.626274 11.00000 -1.50000
AFIX 0
C25 1 0.309386 0.468599 0.580467 11.00000 0.02128 0.02874 =
0.01945 -0.00147 0.00004 -0.00273
AFIX 13
H25 2 0.301053 0.499169 0.549625 11.00000 -1.20000
AFIX 0
C26 1 0.372274 0.430095 0.563776 11.00000 0.03400 0.03223 =
0.02907 -0.00852 0.00739 -0.00214
AFIX 33
H26A 2 0.410007 0.459330 0.563787 11.00000 -1.50000
H26B 2 0.379756 0.394973 0.589880 11.00000 -1.50000
H26C 2 0.366394 0.411900 0.527223 11.00000 -1.50000
AFIX 0
C27 1 0.249765 0.420410 0.580068 11.00000 0.03016 0.03583 =
0.03198 -0.00899 -0.00072 -0.01078
AFIX 33
H27A 2 0.209878 0.443639 0.590425 11.00000 -1.50000
H27B 2 0.244469 0.402260 0.543437 11.00000 -1.50000
H27C 2 0.257831 0.385333 0.606093 11.00000 -1.50000
AFIX 0
C28 1 0.521433 0.596840 0.607741 11.00000 0.02034 0.02885 =
0.01709 -0.00063 0.00041 -0.00225
AFIX 13
H28 2 0.527121 0.588517 0.647621 11.00000 -1.20000
AFIX 0
C29 1 0.539731 0.531047 0.579995 11.00000 0.02114 0.03032 =
0.02734 0.00095 0.00283 0.00424
AFIX 33
H29A 2 0.506454 0.498551 0.588772 11.00000 -1.50000
H29B 2 0.541813 0.536952 0.540408 11.00000 -1.50000
H29C 2 0.582378 0.516460 0.593440 11.00000 -1.50000
AFIX 0
C30 1 0.573993 0.649086 0.594130 11.00000 0.02519 0.03359 =
0.03697 -0.00209 0.00380 -0.00842
AFIX 33
H30A 2 0.562133 0.690055 0.611655 11.00000 -1.50000
H30B 2 0.616719 0.634770 0.607607 11.00000 -1.50000
H30C 2 0.576155 0.655261 0.554575 11.00000 -1.50000
AFIX 0
C31 1 0.402566 0.601944 0.524624 11.00000 0.02618 0.01620 =
0.01821 -0.00234 0.00245 -0.00222
AFIX 13
H31 2 0.401162 0.553872 0.519909 11.00000 -1.20000
AFIX 0
C32 1 0.332684 0.627898 0.508927 11.00000 0.02881 0.03618 =
0.01874 0.00094 -0.00081 -0.00153
AFIX 33
H32A 2 0.300540 0.612089 0.535384 11.00000 -1.50000
H32B 2 0.332987 0.675325 0.509181 11.00000 -1.50000
H32C 2 0.321026 0.612436 0.472444 11.00000 -1.50000
AFIX 0
C33 1 0.452629 0.628234 0.481393 11.00000 0.03337 0.03194 =
0.02063 0.00242 0.00485 0.00158
AFIX 33
H33A 2 0.496604 0.612670 0.490338 11.00000 -1.50000
H33B 2 0.440274 0.612769 0.445071 11.00000 -1.50000
H33C 2 0.452235 0.675658 0.481807 11.00000 -1.50000
AFIX 0
C34 1 0.416764 0.709163 0.616749 11.00000 0.02988 0.01407 =
0.01937 0.00117 -0.00368 -0.00132
AFIX 13
H34 2 0.442068 0.717268 0.650965 11.00000 -1.20000
AFIX 0
C35 1 0.344408 0.729019 0.629632 11.00000 0.04246 0.01687 =
0.03177 -0.00085 0.00004 0.00706
AFIX 33
H35A 2 0.326051 0.699183 0.656644 11.00000 -1.50000
H35B 2 0.343582 0.773193 0.644154 11.00000 -1.50000
H35C 2 0.318363 0.727094 0.596149 11.00000 -1.50000
AFIX 0
C36 1 0.444311 0.758153 0.573343 11.00000 0.04773 0.02015 =
0.03290 0.00575 0.00244 -0.00389
AFIX 33
H36A 2 0.489620 0.746785 0.564550 11.00000 -1.50000
H36B 2 0.417623 0.756041 0.540221 11.00000 -1.50000
H36C 2 0.442842 0.802141 0.588227 11.00000 -1.50000
AFIX 0
PART -1
C37 1 0.238762 0.254114 0.745132 10.50000 0.10967
AFIX 33
H37A 2 0.265115 0.236838 0.715117 10.50000 -1.50000
H37B 2 0.194985 0.234874 0.743998 10.50000 -1.50000
H37C 2 0.235251 0.301216 0.741481 10.50000 -1.50000
AFIX 0
C38 1 0.271382 0.237619 0.799352 10.50000 0.09316
AFIX 23
H38A 2 0.275680 0.190022 0.802385 10.50000 -1.20000
H38B 2 0.315941 0.256356 0.799868 10.50000 -1.20000
AFIX 0
C39 1 0.233555 0.262718 0.848061 10.50000 0.08055
AFIX 23
H39A 2 0.229598 0.310381 0.845465 10.50000 -1.20000
H39B 2 0.188909 0.244181 0.847703 10.50000 -1.20000
AFIX 0
C40 1 0.266921 0.245146 0.900914 10.50000 0.09163
AFIX 23
H40A 2 0.272296 0.197551 0.902357 10.50000 -1.20000
H40B 2 0.311155 0.264631 0.901130 10.50000 -1.20000
AFIX 0
C41 1 0.231417 0.266583 0.950826 10.50000 0.11808
AFIX 23
H41A 2 0.188362 0.244734 0.952326 10.50000 -1.20000
H41B 2 0.223560 0.313802 0.948685 10.50000 -1.20000
AFIX 0
C42 1 0.269746 0.251354 1.003358 10.50000 0.15571
AFIX 33
H42A 2 0.244699 0.266214 1.035021 10.50000 -1.50000
H42B 2 0.276863 0.204560 1.006048 10.50000 -1.50000
H42C 2 0.312049 0.273605 1.002408 10.50000 -1.50000
AFIX 0
HKLF 4
REM adpm350_a.res in Pccn
REM R1 = 0.0342 for 7087 Fo > 4sig(Fo) and 0.0488 for all 8929 data
REM 421 parameters refined using 9 restraints
END
WGHT 0.0194 11.4397
REM Highest difference peak 1.172, deepest hole -0.564, 1-sigma level 0.103
Q1 1 0.2500 0.2500 0.8735 10.50000 0.05 1.17
Q2 1 0.2500 0.2500 0.7096 10.50000 0.05 1.14
Q3 1 0.2500 0.2500 0.7684 10.50000 0.05 1.13
Q4 1 0.2732 0.2356 0.8197 11.00000 0.05 0.90
Q5 1 0.2500 0.2500 0.9235 10.50000 0.05 0.73
Q6 1 0.2500 0.2500 1.0309 10.50000 0.05 0.73
Q7 1 0.1643 0.4596 0.7695 11.00000 0.05 0.59
Q8 1 0.3769 0.7035 0.8425 11.00000 0.05 0.52
Q9 1 0.5555 0.4393 0.7483 11.00000 0.05 0.50
Q10 1 0.4177 0.6670 0.6115 11.00000 0.05 0.50
Q11 1 0.5586 0.6505 0.7157 11.00000 0.05 0.44
Q12 1 0.2225 0.2606 0.9760 11.00000 0.05 0.44
Q13 1 0.4426 0.5474 0.6880 11.00000 0.05 0.42
Q14 1 0.5207 0.4468 0.9109 11.00000 0.05 0.41
Q15 1 0.1584 0.5959 0.6525 11.00000 0.05 0.40
Q16 1 0.4004 0.5309 0.9103 11.00000 0.05 0.40
Q17 1 0.5560 0.4520 0.8228 11.00000 0.05 0.40
Q18 1 0.2806 0.4648 0.7154 11.00000 0.05 0.40
Q19 1 0.3995 0.4794 0.8619 11.00000 0.05 0.40
Q20 1 0.4980 0.6877 0.8583 11.00000 0.05 0.39
;
_shelx_res_checksum 30048
_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 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.814
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_2-Cl
_database_code_depnum_ccdc_archive 'CCDC 1833621'
_audit_update_record
;
2018-03-29 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;
_manchester_internal_coll_name odpm65
_manchester_internal_coll_client CAPG/JGCK
_manchester_internal_coll_type custom
_manchester_internal_coll_frame_time 5.0
_manchester_internal_coll_frame_width 0.8
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user CAPG
_manchester_internal_coll_date 22/7/16
_manchester_internal_process_user CAPG
_manchester_internal_process_date 27/3/18
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 27/3/18
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 27/3/18
_manchester_internal_validation_user CAPG
_manchester_internal_validation_date 28/3/18
_manchester_internal_archive_date 28/3/18
_audit_creation_date 2018-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2018/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H84 Cl N2 Si4 Sm'
_chemical_formula_sum 'C36 H84 Cl N2 Si4 Sm'
_chemical_formula_weight 843.21
_chemical_melting_point ?
_chemical_oxdiff_formula Sm(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'
Sm Sm -0.1638 3.4418 '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 15.8726(4)
_cell_length_b 13.1782(3)
_cell_length_c 22.6012(6)
_cell_angle_alpha 90
_cell_angle_beta 109.299(3)
_cell_angle_gamma 90
_cell_volume 4461.9(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 10088
_cell_measurement_temperature 150.01(1)
_cell_measurement_theta_max 29.0350
_cell_measurement_theta_min 3.0830
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.508
_exptl_absorpt_correction_T_max 0.925
_exptl_absorpt_correction_T_min 0.872
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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_primary yellow
_exptl_crystal_density_diffrn 1.255
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1796
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
14 -4 16 0.1701
2 -18 0 0.2049
0 18 -9 0.2068
-13 7 -16 0.2568
13 13 -18 0.0351
-17 2 27 0.2800
-4 5 31 0.2473
-13 -15 2 0.1812
7 -14 -20 0.2519
-7 -13 -15 0.2287
-8 -1 32 0.2573
_exptl_crystal_preparation 'By Benjamin Reant and CAPG.'
_exptl_crystal_recrystallization_method 'From hexane.'
_exptl_crystal_size_max 0.628
_exptl_crystal_size_mid 0.448
_exptl_crystal_size_min 0.321
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
14.0013 -3.9996 16.0012 -0.6226 0.6227 0.4769
2.0006 -18.0013 -0.0007 0.4297 0.8724 0.0258
-0.0003 18.0012 -9.0003 -0.4127 -0.8729 -0.3079
-13.0012 6.9998 -16.0012 0.4974 -0.7348 -0.4836
13.0013 13.0011 -18.0016 -0.6961 -0.3699 -0.6012
-17.0022 2.0001 27.0032 0.3344 -0.3650 0.8623
-4.0010 5.0008 31.0035 -0.3165 -0.1545 0.9583
-13.0010 -15.0015 1.9999 0.9260 0.3714 0.1093
7.0014 -14.0012 -20.0028 0.3319 0.7025 -0.6085
-7.0002 -13.0015 -15.0019 0.8122 0.3347 -0.4306
-8.0013 -0.9998 32.0035 0.0035 0.0252 1.0061
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0320
_diffrn_reflns_av_unetI/netI 0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 22398
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.350
_diffrn_reflns_theta_min 2.686
_diffrn_ambient_temperature 150.01(1)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.3271
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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 -32.00 17.60 0.80 2.50 -- -12.00 -57.00 -90.00 62
2 \w -25.00 11.00 0.80 2.50 -- -12.00 -99.00-120.00 45
3 \w -85.00 -57.80 0.80 2.50 -- -12.00 -57.00 -90.00 34
4 \w -63.00 41.00 0.80 2.50 -- 11.38 -57.00 90.00 130
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0401925000
_diffrn_orient_matrix_UB_12 -0.0283375000
_diffrn_orient_matrix_UB_13 -0.0108243000
_diffrn_orient_matrix_UB_21 0.0250101000
_diffrn_orient_matrix_UB_22 -0.0456863000
_diffrn_orient_matrix_UB_23 0.0056137000
_diffrn_orient_matrix_UB_31 -0.0017655000
_diffrn_orient_matrix_UB_32 -0.0016329000
_diffrn_orient_matrix_UB_33 0.0309435000
_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'
_diffrn_special_details ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6874
_reflns_number_total 8147
_reflns_odcompleteness_completeness 99.59
_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 0.842
_refine_diff_density_min -0.489
_refine_diff_density_rms 0.080
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.058
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 421
_refine_ls_number_reflns 8147
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0385
_refine_ls_R_factor_gt 0.0286
_refine_ls_restrained_S_all 1.058
_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^)+(0.0288P)^2^+0.3095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0615
_refine_ls_wR_factor_ref 0.0658
_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
Sm1 Sm 0.66893(2) 0.53051(2) 0.27516(2) 0.01679(6) Uani 1 1 d . . . . .
Cl1 Cl 0.49670(4) 0.52429(6) 0.23704(3) 0.02529(17) Uani 1 1 d . . . . .
Si1 Si 0.77090(5) 0.71375(6) 0.37200(3) 0.01675(17) Uani 1 1 d . . . . .
Si2 Si 0.70970(5) 0.53104(6) 0.43798(3) 0.01554(17) Uani 1 1 d . . . . .
Si3 Si 0.77492(5) 0.31433(6) 0.26136(3) 0.01825(17) Uani 1 1 d . . . . .
Si4 Si 0.73009(5) 0.46993(6) 0.14784(3) 0.01658(17) Uani 1 1 d . . . . .
N1 N 0.72500(13) 0.59553(17) 0.37475(9) 0.0153(5) Uani 1 1 d . . . . .
N2 N 0.74056(13) 0.42914(17) 0.22285(9) 0.0158(5) Uani 1 1 d . . . . .
C1 C 0.74323(17) 0.7398(2) 0.28322(11) 0.0198(6) Uani 1 1 d . . . . .
H1 H 0.757109 0.676145 0.264200 0.024 Uiso 1 1 calc R . . . .
C2 C 0.64373(18) 0.7629(2) 0.24964(12) 0.0257(7) Uani 1 1 d . . . . .
H2A H 0.607287 0.709458 0.259232 0.038 Uiso 1 1 calc GR . . . .
H2B H 0.631897 0.765466 0.204272 0.038 Uiso 1 1 calc GR . . . .
H2C H 0.628678 0.828436 0.264031 0.038 Uiso 1 1 calc GR . . . .
C3 C 0.79853(19) 0.8255(2) 0.26723(12) 0.0276(7) Uani 1 1 d . . . . .
H3A H 0.782949 0.830798 0.221613 0.041 Uiso 1 1 calc GR . . . .
H3B H 0.862258 0.810033 0.285887 0.041 Uiso 1 1 calc GR . . . .
H3C H 0.785480 0.889906 0.284031 0.041 Uiso 1 1 calc GR . . . .
C4 C 0.72392(17) 0.8208(2) 0.40836(12) 0.0209(6) Uani 1 1 d . . . . .
H4 H 0.753505 0.814334 0.454713 0.025 Uiso 1 1 calc R . . . .
C5 C 0.62335(17) 0.8165(2) 0.39708(13) 0.0273(7) Uani 1 1 d . . . . .
H5A H 0.590702 0.832113 0.353055 0.041 Uiso 1 1 calc GR . . . .
H5B H 0.607863 0.866222 0.424037 0.041 Uiso 1 1 calc GR . . . .
H5C H 0.607154 0.748309 0.406944 0.041 Uiso 1 1 calc GR . . . .
C6 C 0.7458(2) 0.9287(2) 0.39128(13) 0.0295(7) Uani 1 1 d . . . . .
H6A H 0.809651 0.933491 0.397186 0.044 Uiso 1 1 calc GR . . . .
H6B H 0.730328 0.978177 0.418404 0.044 Uiso 1 1 calc GR . . . .
H6C H 0.711214 0.942977 0.347395 0.044 Uiso 1 1 calc GR . . . .
C7 C 0.89676(16) 0.7076(2) 0.41011(12) 0.0212(6) Uani 1 1 d . . . . .
H7 H 0.906493 0.665131 0.448445 0.025 Uiso 1 1 calc R . . . .
C8 C 0.94100(17) 0.6475(2) 0.36968(12) 0.0268(7) Uani 1 1 d . . . . .
H8A H 0.905574 0.586676 0.352939 0.040 Uiso 1 1 calc GR . . . .
H8B H 1.001431 0.627423 0.395493 0.040 Uiso 1 1 calc GR . . . .
H8C H 0.944085 0.690080 0.334916 0.040 Uiso 1 1 calc GR . . . .
C9 C 0.94880(19) 0.8056(3) 0.43405(14) 0.0354(8) Uani 1 1 d . . . . .
H9A H 0.942330 0.851473 0.398716 0.053 Uiso 1 1 calc GR . . . .
H9B H 1.012067 0.789452 0.454516 0.053 Uiso 1 1 calc GR . . . .
H9C H 0.925308 0.838395 0.464250 0.053 Uiso 1 1 calc GR . . . .
C10 C 0.79317(16) 0.4228(2) 0.46271(11) 0.0180(6) Uani 1 1 d . . . . .
H10 H 0.775940 0.374070 0.426753 0.022 Uiso 1 1 calc R . . . .
C11 C 0.89068(16) 0.4524(2) 0.47199(12) 0.0208(6) Uani 1 1 d . . . . .
H11A H 0.893135 0.490593 0.435383 0.031 Uiso 1 1 calc GR . . . .
H11B H 0.927070 0.390931 0.476889 0.031 Uiso 1 1 calc GR . . . .
H11C H 0.913815 0.494616 0.509611 0.031 Uiso 1 1 calc GR . . . .
C12 C 0.79262(19) 0.3604(2) 0.52011(12) 0.0293(7) Uani 1 1 d . . . . .
H12A H 0.820948 0.399593 0.558373 0.044 Uiso 1 1 calc GR . . . .
H12B H 0.825664 0.297046 0.521669 0.044 Uiso 1 1 calc GR . . . .
H12C H 0.730883 0.344698 0.516843 0.044 Uiso 1 1 calc GR . . . .
C13 C 0.59266(17) 0.4743(2) 0.40353(12) 0.0195(6) Uani 1 1 d . . . . .
H13 H 0.588457 0.453056 0.360164 0.023 Uiso 1 1 calc R . . . .
C14 C 0.51833(17) 0.5532(2) 0.39374(13) 0.0262(7) Uani 1 1 d . . . . .
H14A H 0.517142 0.576872 0.434564 0.039 Uiso 1 1 calc GR . . . .
H14B H 0.460711 0.522397 0.370420 0.039 Uiso 1 1 calc GR . . . .
H14C H 0.529611 0.610817 0.369977 0.039 Uiso 1 1 calc GR . . . .
C15 C 0.56878(18) 0.3784(2) 0.43300(13) 0.0311(7) Uani 1 1 d . . . . .
H15A H 0.612856 0.325334 0.434996 0.047 Uiso 1 1 calc GR . . . .
H15B H 0.509366 0.354818 0.407408 0.047 Uiso 1 1 calc GR . . . .
H15C H 0.568867 0.393914 0.475428 0.047 Uiso 1 1 calc GR . . . .
C16 C 0.71635(17) 0.6116(2) 0.50934(11) 0.0210(6) Uani 1 1 d . . . . .
H16 H 0.682569 0.675508 0.493232 0.025 Uiso 1 1 calc R . . . .
C17 C 0.67151(19) 0.5614(2) 0.55325(12) 0.0281(7) Uani 1 1 d . . . . .
H17A H 0.608879 0.546713 0.529588 0.042 Uiso 1 1 calc GR . . . .
H17B H 0.674625 0.607714 0.587854 0.042 Uiso 1 1 calc GR . . . .
H17C H 0.702614 0.498148 0.570097 0.042 Uiso 1 1 calc GR . . . .
C18 C 0.81166(18) 0.6434(3) 0.54896(12) 0.0285(7) Uani 1 1 d . . . . .
H18A H 0.846224 0.583075 0.567814 0.043 Uiso 1 1 calc GR . . . .
H18B H 0.809047 0.689888 0.582157 0.043 Uiso 1 1 calc GR . . . .
H18C H 0.840366 0.677521 0.522115 0.043 Uiso 1 1 calc GR . . . .
C19 C 0.68373(17) 0.2894(2) 0.29823(12) 0.0207(6) Uani 1 1 d . . . . .
H19 H 0.679003 0.354188 0.319938 0.025 Uiso 1 1 calc R . . . .
C20 C 0.59170(17) 0.2759(3) 0.24772(13) 0.0300(7) Uani 1 1 d . . . . .
H20A H 0.581632 0.330868 0.216953 0.045 Uiso 1 1 calc GR . . . .
H20B H 0.545194 0.277703 0.267397 0.045 Uiso 1 1 calc GR . . . .
H20C H 0.589656 0.210516 0.226624 0.045 Uiso 1 1 calc GR . . . .
C21 C 0.69611(19) 0.2067(2) 0.34834(12) 0.0280(7) Uani 1 1 d . . . . .
H21A H 0.703449 0.140652 0.330705 0.042 Uiso 1 1 calc GR . . . .
H21B H 0.643528 0.204851 0.361908 0.042 Uiso 1 1 calc GR . . . .
H21C H 0.749259 0.221821 0.384371 0.042 Uiso 1 1 calc GR . . . .
C22 C 0.88375(17) 0.3334(2) 0.32822(12) 0.0253(7) Uani 1 1 d . . . . .
H22 H 0.868632 0.381167 0.357609 0.030 Uiso 1 1 calc R . . . .
C23 C 0.95725(18) 0.3880(3) 0.30959(13) 0.0337(8) Uani 1 1 d . . . . .
H23A H 0.980936 0.341862 0.284905 0.050 Uiso 1 1 calc GR . . . .
H23B H 1.005501 0.408562 0.347493 0.050 Uiso 1 1 calc GR . . . .
H23C H 0.932015 0.448164 0.284525 0.050 Uiso 1 1 calc GR . . . .
C24 C 0.9244(2) 0.2401(3) 0.36838(14) 0.0382(8) Uani 1 1 d . . . . .
H24A H 0.880449 0.210525 0.385272 0.057 Uiso 1 1 calc GR . . . .
H24B H 0.977523 0.260551 0.403031 0.057 Uiso 1 1 calc GR . . . .
H24C H 0.941197 0.189604 0.342420 0.057 Uiso 1 1 calc GR . . . .
C25 C 0.78278(19) 0.2020(2) 0.21032(13) 0.0257(7) Uani 1 1 d . . . . .
H25 H 0.734426 0.211443 0.169097 0.031 Uiso 1 1 calc R . . . .
C26 C 0.7671(2) 0.0980(2) 0.23506(13) 0.0371(8) Uani 1 1 d . . . . .
H26A H 0.810558 0.087336 0.276950 0.056 Uiso 1 1 calc GR . . . .
H26B H 0.774125 0.044865 0.206710 0.056 Uiso 1 1 calc GR . . . .
H26C H 0.706541 0.095205 0.237342 0.056 Uiso 1 1 calc GR . . . .
C27 C 0.87140(19) 0.1997(3) 0.19641(13) 0.0343(8) Uani 1 1 d . . . . .
H27A H 0.881043 0.265542 0.179498 0.051 Uiso 1 1 calc GR . . . .
H27B H 0.868914 0.146375 0.165677 0.051 Uiso 1 1 calc GR . . . .
H27C H 0.920645 0.185819 0.235208 0.051 Uiso 1 1 calc GR . . . .
C28 C 0.63936(17) 0.5739(2) 0.12735(12) 0.0206(6) Uani 1 1 d . . . . .
H28 H 0.643883 0.607454 0.167983 0.025 Uiso 1 1 calc R . . . .
C29 C 0.54403(18) 0.5334(2) 0.10113(13) 0.0281(7) Uani 1 1 d . . . . .
H29A H 0.532714 0.508840 0.058273 0.042 Uiso 1 1 calc GR . . . .
H29B H 0.501853 0.587873 0.100826 0.042 Uiso 1 1 calc GR . . . .
H29C H 0.536357 0.477483 0.127482 0.042 Uiso 1 1 calc GR . . . .
C30 C 0.6499(2) 0.6596(2) 0.08387(13) 0.0336(8) Uani 1 1 d . . . . .
H30A H 0.707791 0.692999 0.102842 0.050 Uiso 1 1 calc GR . . . .
H30B H 0.601941 0.709369 0.077959 0.050 Uiso 1 1 calc GR . . . .
H30C H 0.646771 0.630984 0.043178 0.050 Uiso 1 1 calc GR . . . .
C31 C 0.83315(19) 0.5333(2) 0.13905(13) 0.0258(7) Uani 1 1 d . . . . .
H31 H 0.811935 0.567655 0.097261 0.031 Uiso 1 1 calc R . . . .
C32 C 0.87029(19) 0.6185(3) 0.18678(13) 0.0322(8) Uani 1 1 d . . . . .
H32A H 0.822876 0.667614 0.184243 0.048 Uiso 1 1 calc GR . . . .
H32B H 0.919340 0.652615 0.177495 0.048 Uiso 1 1 calc GR . . . .
H32C H 0.892392 0.589663 0.229096 0.048 Uiso 1 1 calc GR . . . .
C33 C 0.9088(2) 0.4636(3) 0.13679(15) 0.0363(8) Uani 1 1 d . . . . .
H33A H 0.934952 0.430198 0.177509 0.054 Uiso 1 1 calc GR . . . .
H33B H 0.954664 0.503649 0.127232 0.054 Uiso 1 1 calc GR . . . .
H33C H 0.885230 0.412128 0.104191 0.054 Uiso 1 1 calc GR . . . .
C34 C 0.69758(18) 0.3680(2) 0.08494(11) 0.0212(6) Uani 1 1 d . . . . .
H34 H 0.747620 0.317750 0.097164 0.025 Uiso 1 1 calc R . . . .
C35 C 0.6938(2) 0.4082(3) 0.01965(12) 0.0296(7) Uani 1 1 d . . . . .
H35A H 0.646968 0.459847 0.005571 0.044 Uiso 1 1 calc GR . . . .
H35B H 0.680485 0.351993 -0.010426 0.044 Uiso 1 1 calc GR . . . .
H35C H 0.751504 0.438197 0.022532 0.044 Uiso 1 1 calc GR . . . .
C36 C 0.61255(18) 0.3060(2) 0.07787(13) 0.0276(7) Uani 1 1 d . . . . .
H36A H 0.607816 0.293268 0.119376 0.041 Uiso 1 1 calc GR . . . .
H36B H 0.615576 0.241169 0.057425 0.041 Uiso 1 1 calc GR . . . .
H36C H 0.560147 0.344126 0.052312 0.041 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
Sm1 0.01807(8) 0.01625(10) 0.01682(8) -0.00014(6) 0.00679(6) 0.00279(6)
Cl1 0.0207(3) 0.0282(5) 0.0257(4) -0.0018(3) 0.0060(3) 0.0004(3)
Si1 0.0182(4) 0.0143(5) 0.0189(4) 0.0018(3) 0.0076(3) 0.0003(3)
Si2 0.0153(3) 0.0164(5) 0.0160(4) 0.0021(3) 0.0066(3) 0.0000(3)
Si3 0.0207(4) 0.0163(5) 0.0179(4) 0.0005(3) 0.0065(3) 0.0035(3)
Si4 0.0188(4) 0.0157(5) 0.0167(4) 0.0006(3) 0.0080(3) 0.0000(3)
N1 0.0163(10) 0.0131(13) 0.0177(11) 0.0006(10) 0.0072(9) 0.0010(10)
N2 0.0177(11) 0.0139(13) 0.0151(11) -0.0002(10) 0.0044(9) 0.0006(10)
C1 0.0264(14) 0.0136(16) 0.0208(14) 0.0021(12) 0.0097(12) 0.0020(12)
C2 0.0332(16) 0.0176(18) 0.0242(15) 0.0012(13) 0.0067(13) 0.0048(14)
C3 0.0417(17) 0.0170(18) 0.0285(15) 0.0035(13) 0.0175(14) -0.0055(14)
C4 0.0263(14) 0.0168(17) 0.0196(13) 0.0018(12) 0.0077(12) 0.0037(13)
C5 0.0294(15) 0.0266(19) 0.0276(15) 0.0015(14) 0.0116(13) 0.0078(14)
C6 0.0407(17) 0.0194(18) 0.0293(16) -0.0038(14) 0.0126(14) -0.0003(15)
C7 0.0198(13) 0.0198(18) 0.0241(14) 0.0053(13) 0.0076(12) -0.0019(12)
C8 0.0201(14) 0.033(2) 0.0285(15) 0.0041(14) 0.0092(12) 0.0012(14)
C9 0.0245(15) 0.031(2) 0.0459(18) 0.0045(17) 0.0056(14) -0.0059(15)
C10 0.0193(13) 0.0168(17) 0.0186(13) 0.0002(12) 0.0074(11) 0.0000(12)
C11 0.0176(13) 0.0223(18) 0.0209(14) 0.0010(12) 0.0042(12) 0.0016(12)
C12 0.0299(16) 0.027(2) 0.0317(16) 0.0117(15) 0.0110(13) 0.0042(14)
C13 0.0181(13) 0.0219(18) 0.0201(14) 0.0027(12) 0.0084(12) -0.0006(12)
C14 0.0186(14) 0.032(2) 0.0287(16) 0.0016(14) 0.0091(13) 0.0030(13)
C15 0.0249(15) 0.031(2) 0.0386(17) 0.0060(15) 0.0126(14) -0.0020(14)
C16 0.0232(14) 0.0229(18) 0.0187(13) 0.0025(13) 0.0093(12) 0.0042(13)
C17 0.0332(16) 0.033(2) 0.0229(15) 0.0027(14) 0.0156(13) 0.0030(15)
C18 0.0299(15) 0.032(2) 0.0240(15) -0.0077(14) 0.0097(13) -0.0012(14)
C19 0.0269(14) 0.0097(16) 0.0270(14) -0.0002(13) 0.0110(12) 0.0008(12)
C20 0.0266(15) 0.029(2) 0.0368(17) 0.0052(15) 0.0138(14) -0.0027(14)
C21 0.0391(17) 0.0197(19) 0.0295(16) 0.0019(14) 0.0172(14) -0.0024(14)
C22 0.0232(14) 0.030(2) 0.0211(14) -0.0016(13) 0.0045(12) 0.0079(14)
C23 0.0211(15) 0.042(2) 0.0341(16) -0.0053(16) 0.0039(13) -0.0001(15)
C24 0.0336(17) 0.047(2) 0.0299(16) 0.0102(16) 0.0057(14) 0.0149(17)
C25 0.0332(16) 0.0210(18) 0.0238(14) -0.0005(13) 0.0106(13) 0.0085(14)
C26 0.065(2) 0.0168(19) 0.0315(16) -0.0028(15) 0.0187(16) 0.0089(17)
C27 0.0427(18) 0.033(2) 0.0278(16) -0.0048(15) 0.0130(14) 0.0127(16)
C28 0.0270(15) 0.0202(17) 0.0151(13) 0.0030(12) 0.0074(12) 0.0044(13)
C29 0.0235(15) 0.034(2) 0.0257(15) 0.0004(14) 0.0065(13) 0.0077(14)
C30 0.0443(18) 0.025(2) 0.0316(16) 0.0100(15) 0.0125(15) 0.0052(16)
C31 0.0280(15) 0.028(2) 0.0263(15) 0.0020(14) 0.0156(13) -0.0021(14)
C32 0.0306(16) 0.035(2) 0.0349(16) -0.0063(16) 0.0161(14) -0.0107(15)
C33 0.0302(17) 0.043(2) 0.0419(19) -0.0032(16) 0.0207(15) -0.0025(16)
C34 0.0285(15) 0.0186(17) 0.0183(13) 0.0013(12) 0.0102(12) 0.0038(13)
C35 0.0401(17) 0.030(2) 0.0200(14) 0.0000(14) 0.0114(13) 0.0027(15)
C36 0.0341(16) 0.0218(19) 0.0248(15) -0.0049(14) 0.0072(13) -0.0014(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
Sm1 Cl1 2.5817(7) . ?
Sm1 N1 2.295(2) . ?
Sm1 N2 2.316(2) . ?
Sm1 C1 2.982(3) . ?
Si1 N1 1.730(2) . ?
Si1 C1 1.938(2) . ?
Si1 C4 1.904(3) . ?
Si1 C7 1.898(3) . ?
Si2 N1 1.747(2) . ?
Si2 C10 1.901(3) . ?
Si2 C13 1.913(3) . ?
Si2 C16 1.905(3) . ?
Si3 N2 1.741(2) . ?
Si3 C19 1.922(3) . ?
Si3 C22 1.899(3) . ?
Si3 C25 1.906(3) . ?
Si4 N2 1.733(2) . ?
Si4 C28 1.930(3) . ?
Si4 C31 1.905(3) . ?
Si4 C34 1.900(3) . ?
C1 H1 1.0000 . ?
C1 C2 1.540(4) . ?
C1 C3 1.544(4) . ?
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 1.532(4) . ?
C4 C6 1.543(4) . ?
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 1.543(4) . ?
C7 C9 1.531(4) . ?
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 1.542(3) . ?
C10 C12 1.539(4) . ?
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 1.533(4) . ?
C13 C15 1.533(4) . ?
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 1.548(4) . ?
C16 C18 1.540(4) . ?
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 1.538(4) . ?
C19 C21 1.537(4) . ?
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 1.543(4) . ?
C22 C24 1.539(4) . ?
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 1.532(4) . ?
C25 C27 1.540(4) . ?
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 1.528(4) . ?
C28 C30 1.542(4) . ?
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 1.533(4) . ?
C31 C33 1.526(4) . ?
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 1.550(3) . ?
C34 C36 1.540(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Sm1 C1 113.80(5) . . ?
N1 Sm1 Cl1 111.33(5) . . ?
N1 Sm1 N2 128.26(7) . . ?
N1 Sm1 C1 65.00(7) . . ?
N2 Sm1 Cl1 117.11(5) . . ?
N2 Sm1 C1 108.29(7) . . ?
N1 Si1 C1 104.06(11) . . ?
N1 Si1 C4 114.96(11) . . ?
N1 Si1 C7 109.77(12) . . ?
C4 Si1 C1 109.18(12) . . ?
C7 Si1 C1 108.77(11) . . ?
C7 Si1 C4 109.83(12) . . ?
N1 Si2 C10 109.50(11) . . ?
N1 Si2 C13 103.66(11) . . ?
N1 Si2 C16 115.95(12) . . ?
C10 Si2 C13 108.35(12) . . ?
C10 Si2 C16 109.35(12) . . ?
C16 Si2 C13 109.71(12) . . ?
N2 Si3 C19 102.06(11) . . ?
N2 Si3 C22 109.57(12) . . ?
N2 Si3 C25 116.41(11) . . ?
C22 Si3 C19 107.15(12) . . ?
C22 Si3 C25 111.12(13) . . ?
C25 Si3 C19 109.81(13) . . ?
N2 Si4 C28 106.12(11) . . ?
N2 Si4 C31 115.46(12) . . ?
N2 Si4 C34 115.28(12) . . ?
C31 Si4 C28 105.19(13) . . ?
C34 Si4 C28 109.04(12) . . ?
C34 Si4 C31 105.21(12) . . ?
Si1 N1 Sm1 109.41(10) . . ?
Si1 N1 Si2 129.91(12) . . ?
Si2 N1 Sm1 120.45(11) . . ?
Si3 N2 Sm1 111.82(10) . . ?
Si4 N2 Sm1 114.57(11) . . ?
Si4 N2 Si3 132.18(13) . . ?
Sm1 C1 H1 48.4 . . ?
Si1 C1 Sm1 81.31(9) . . ?
Si1 C1 H1 106.8 . . ?
C2 C1 Sm1 80.33(16) . . ?
C2 C1 Si1 112.96(17) . . ?
C2 C1 H1 106.8 . . ?
C2 C1 C3 108.1(2) . . ?
C3 C1 Sm1 154.93(18) . . ?
C3 C1 Si1 114.84(18) . . ?
C3 C1 H1 106.8 . . ?
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 105.9 . . ?
C5 C4 Si1 115.8(2) . . ?
C5 C4 H4 105.9 . . ?
C5 C4 C6 107.5(2) . . ?
C6 C4 Si1 114.98(18) . . ?
C6 C4 H4 105.9 . . ?
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 104.8 . . ?
C8 C7 Si1 111.70(18) . . ?
C8 C7 H7 104.8 . . ?
C9 C7 Si1 119.3(2) . . ?
C9 C7 H7 104.8 . . ?
C9 C7 C8 110.1(2) . . ?
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 105.4 . . ?
C11 C10 Si2 114.9(2) . . ?
C11 C10 H10 105.4 . . ?
C12 C10 Si2 116.84(18) . . ?
C12 C10 H10 105.4 . . ?
C12 C10 C11 107.8(2) . . ?
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 104.4 . . ?
C14 C13 Si2 113.0(2) . . ?
C14 C13 H13 104.4 . . ?
C15 C13 Si2 119.44(19) . . ?
C15 C13 H13 104.4 . . ?
C15 C13 C14 109.4(2) . . ?
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 106.7 . . ?
C17 C16 Si2 113.3(2) . . ?
C17 C16 H16 106.7 . . ?
C18 C16 Si2 114.40(18) . . ?
C18 C16 H16 106.7 . . ?
C18 C16 C17 108.4(2) . . ?
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 104.8 . . ?
C20 C19 Si3 111.37(18) . . ?
C20 C19 H19 104.8 . . ?
C21 C19 Si3 120.63(19) . . ?
C21 C19 H19 104.8 . . ?
C21 C19 C20 108.9(2) . . ?
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 104.9 . . ?
C23 C22 Si3 114.56(18) . . ?
C23 C22 H22 104.9 . . ?
C24 C22 Si3 117.2(2) . . ?
C24 C22 H22 104.9 . . ?
C24 C22 C23 109.0(2) . . ?
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 106.5 . . ?
C26 C25 Si3 115.03(19) . . ?
C26 C25 H25 106.5 . . ?
C26 C25 C27 109.1(3) . . ?
C27 C25 Si3 112.7(2) . . ?
C27 C25 H25 106.5 . . ?
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 105.8 . . ?
C29 C28 Si4 114.2(2) . . ?
C29 C28 H28 105.8 . . ?
C29 C28 C30 108.1(2) . . ?
C30 C28 Si4 116.31(19) . . ?
C30 C28 H28 105.8 . . ?
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 105.3 . . ?
C32 C31 Si4 113.04(19) . . ?
C32 C31 H31 105.3 . . ?
C33 C31 Si4 116.8(2) . . ?
C33 C31 H31 105.3 . . ?
C33 C31 C32 109.9(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 105.5 . . ?
C35 C34 Si4 112.7(2) . . ?
C35 C34 H34 105.5 . . ?
C36 C34 Si4 117.70(18) . . ?
C36 C34 H34 105.5 . . ?
C36 C34 C35 109.0(2) . . ?
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 odpm65_a.res in P2(1)/c
odpm65.res
created by SHELXL-2018/1 at 10:34:01 on 28-Mar-2018
REM Old TITL odpm65 in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.074, Rweak 0.022, Alpha 0.027, Orientation as input
REM Formula found by SHELXT: C35 N3 Si4 Cl Sm
CELL 0.71073 15.872592 13.178208 22.601188 90 109.2986 90
ZERR 4 0.000393 0.000308 0.000566 0 0.0029 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl N Si Sm
UNIT 144 336 4 8 16 4
L.S. 4
PLAN 20
TEMP -123.14(1)
CONN 20 Sm1
FREE Sm1 Si1
FREE Sm1 Si3
FREE Sm1 Si4
BOND $H
list 4
fmap 2
acta
SHEL 100 0.83
REM
REM
REM
WGHT 0.028800 0.309500
FVAR 2.68706
SM1 6 0.668925 0.530509 0.275158 11.00000 0.01807 0.01625 =
0.01682 -0.00014 0.00679 0.00279
CL1 3 0.496700 0.524291 0.237044 11.00000 0.02068 0.02819 =
0.02573 -0.00181 0.00596 0.00035
SI1 5 0.770899 0.713745 0.372000 11.00000 0.01816 0.01427 =
0.01891 0.00183 0.00758 0.00027
SI2 5 0.709697 0.531037 0.437978 11.00000 0.01535 0.01640 =
0.01596 0.00214 0.00663 0.00003
SI3 5 0.774921 0.314327 0.261355 11.00000 0.02068 0.01631 =
0.01787 0.00046 0.00652 0.00347
SI4 5 0.730089 0.469931 0.147837 11.00000 0.01885 0.01572 =
0.01673 0.00056 0.00799 0.00000
N1 4 0.725004 0.595527 0.374755 11.00000 0.01632 0.01313 =
0.01766 0.00062 0.00724 0.00096
N2 4 0.740561 0.429139 0.222846 11.00000 0.01766 0.01391 =
0.01507 -0.00025 0.00443 0.00063
C1 1 0.743229 0.739818 0.283220 11.00000 0.02641 0.01360 =
0.02079 0.00207 0.00967 0.00199
AFIX 13
H1 2 0.757109 0.676145 0.264200 11.00000 -1.20000
AFIX 0
C2 1 0.643731 0.762891 0.249637 11.00000 0.03317 0.01758 =
0.02417 0.00123 0.00668 0.00481
AFIX 137
H2A 2 0.607287 0.709458 0.259232 11.00000 -1.50000
H2B 2 0.631897 0.765466 0.204272 11.00000 -1.50000
H2C 2 0.628678 0.828436 0.264031 11.00000 -1.50000
AFIX 0
C3 1 0.798531 0.825462 0.267227 11.00000 0.04170 0.01698 =
0.02845 0.00349 0.01747 -0.00550
AFIX 137
H3A 2 0.782949 0.830798 0.221613 11.00000 -1.50000
H3B 2 0.862258 0.810033 0.285887 11.00000 -1.50000
H3C 2 0.785480 0.889906 0.284031 11.00000 -1.50000
AFIX 0
C4 1 0.723919 0.820780 0.408362 11.00000 0.02630 0.01682 =
0.01960 0.00179 0.00771 0.00375
AFIX 13
H4 2 0.753505 0.814334 0.454713 11.00000 -1.20000
AFIX 0
C5 1 0.623349 0.816467 0.397084 11.00000 0.02937 0.02658 =
0.02765 0.00146 0.01161 0.00783
AFIX 137
H5A 2 0.590702 0.832113 0.353055 11.00000 -1.50000
H5B 2 0.607863 0.866222 0.424037 11.00000 -1.50000
H5C 2 0.607154 0.748309 0.406944 11.00000 -1.50000
AFIX 0
C6 1 0.745771 0.928699 0.391279 11.00000 0.04068 0.01935 =
0.02929 -0.00383 0.01258 -0.00031
AFIX 137
H6A 2 0.809651 0.933491 0.397186 11.00000 -1.50000
H6B 2 0.730328 0.978177 0.418404 11.00000 -1.50000
H6C 2 0.711214 0.942977 0.347395 11.00000 -1.50000
AFIX 0
C7 1 0.896759 0.707641 0.410108 11.00000 0.01979 0.01978 =
0.02413 0.00527 0.00759 -0.00192
AFIX 13
H7 2 0.906493 0.665131 0.448445 11.00000 -1.20000
AFIX 0
C8 1 0.940998 0.647466 0.369675 11.00000 0.02006 0.03271 =
0.02853 0.00409 0.00922 0.00120
AFIX 137
H8A 2 0.905574 0.586676 0.352939 11.00000 -1.50000
H8B 2 1.001431 0.627423 0.395493 11.00000 -1.50000
H8C 2 0.944085 0.690080 0.334916 11.00000 -1.50000
AFIX 0
C9 1 0.948799 0.805552 0.434052 11.00000 0.02453 0.03132 =
0.04595 0.00446 0.00563 -0.00587
AFIX 137
H9A 2 0.942330 0.851473 0.398716 11.00000 -1.50000
H9B 2 1.012067 0.789452 0.454516 11.00000 -1.50000
H9C 2 0.925308 0.838395 0.464250 11.00000 -1.50000
AFIX 0
C10 1 0.793169 0.422768 0.462705 11.00000 0.01934 0.01685 =
0.01857 0.00015 0.00738 0.00004
AFIX 13
H10 2 0.775940 0.374070 0.426753 11.00000 -1.20000
AFIX 0
C11 1 0.890682 0.452429 0.471993 11.00000 0.01760 0.02231 =
0.02087 0.00105 0.00415 0.00158
AFIX 137
H11A 2 0.893135 0.490593 0.435383 11.00000 -1.50000
H11B 2 0.927070 0.390931 0.476889 11.00000 -1.50000
H11C 2 0.913815 0.494616 0.509611 11.00000 -1.50000
AFIX 0
C12 1 0.792616 0.360363 0.520107 11.00000 0.02988 0.02704 =
0.03170 0.01172 0.01104 0.00417
AFIX 137
H12A 2 0.820948 0.399593 0.558373 11.00000 -1.50000
H12B 2 0.825664 0.297046 0.521669 11.00000 -1.50000
H12C 2 0.730883 0.344698 0.516843 11.00000 -1.50000
AFIX 0
C13 1 0.592659 0.474279 0.403528 11.00000 0.01808 0.02189 =
0.02014 0.00265 0.00841 -0.00064
AFIX 13
H13 2 0.588457 0.453056 0.360164 11.00000 -1.20000
AFIX 0
C14 1 0.518326 0.553210 0.393739 11.00000 0.01858 0.03246 =
0.02869 0.00163 0.00914 0.00298
AFIX 137
H14A 2 0.517142 0.576872 0.434564 11.00000 -1.50000
H14B 2 0.460711 0.522397 0.370420 11.00000 -1.50000
H14C 2 0.529611 0.610817 0.369977 11.00000 -1.50000
AFIX 0
C15 1 0.568785 0.378448 0.432996 11.00000 0.02492 0.03137 =
0.03861 0.00603 0.01262 -0.00201
AFIX 137
H15A 2 0.612856 0.325334 0.434996 11.00000 -1.50000
H15B 2 0.509366 0.354818 0.407408 11.00000 -1.50000
H15C 2 0.568867 0.393914 0.475428 11.00000 -1.50000
AFIX 0
C16 1 0.716353 0.611615 0.509340 11.00000 0.02322 0.02293 =
0.01874 0.00248 0.00931 0.00421
AFIX 13
H16 2 0.682569 0.675508 0.493232 11.00000 -1.20000
AFIX 0
C17 1 0.671505 0.561447 0.553246 11.00000 0.03322 0.03283 =
0.02294 0.00269 0.01561 0.00304
AFIX 137
H17A 2 0.608879 0.546713 0.529588 11.00000 -1.50000
H17B 2 0.674625 0.607714 0.587854 11.00000 -1.50000
H17C 2 0.702614 0.498148 0.570097 11.00000 -1.50000
AFIX 0
C18 1 0.811658 0.643414 0.548956 11.00000 0.02993 0.03200 =
0.02398 -0.00766 0.00965 -0.00117
AFIX 137
H18A 2 0.846224 0.583075 0.567814 11.00000 -1.50000
H18B 2 0.809047 0.689888 0.582157 11.00000 -1.50000
H18C 2 0.840366 0.677521 0.522115 11.00000 -1.50000
AFIX 0
C19 1 0.683729 0.289385 0.298228 11.00000 0.02690 0.00971 =
0.02697 -0.00024 0.01105 0.00078
AFIX 13
H19 2 0.679003 0.354188 0.319938 11.00000 -1.20000
AFIX 0
C20 1 0.591703 0.275894 0.247718 11.00000 0.02659 0.02889 =
0.03685 0.00515 0.01377 -0.00275
AFIX 137
H20A 2 0.581632 0.330868 0.216953 11.00000 -1.50000
H20B 2 0.545194 0.277703 0.267397 11.00000 -1.50000
H20C 2 0.589656 0.210516 0.226624 11.00000 -1.50000
AFIX 0
C21 1 0.696113 0.206686 0.348343 11.00000 0.03911 0.01970 =
0.02950 0.00195 0.01720 -0.00238
AFIX 137
H21A 2 0.703449 0.140652 0.330705 11.00000 -1.50000
H21B 2 0.643528 0.204851 0.361908 11.00000 -1.50000
H21C 2 0.749259 0.221821 0.384371 11.00000 -1.50000
AFIX 0
C22 1 0.883746 0.333426 0.328217 11.00000 0.02323 0.02954 =
0.02108 -0.00160 0.00446 0.00791
AFIX 13
H22 2 0.868632 0.381167 0.357609 11.00000 -1.20000
AFIX 0
C23 1 0.957253 0.387978 0.309586 11.00000 0.02107 0.04201 =
0.03406 -0.00527 0.00390 -0.00008
AFIX 137
H23A 2 0.980936 0.341862 0.284905 11.00000 -1.50000
H23B 2 1.005501 0.408562 0.347493 11.00000 -1.50000
H23C 2 0.932015 0.448164 0.284525 11.00000 -1.50000
AFIX 0
C24 1 0.924421 0.240050 0.368381 11.00000 0.03358 0.04749 =
0.02995 0.01020 0.00565 0.01492
AFIX 137
H24A 2 0.880449 0.210525 0.385272 11.00000 -1.50000
H24B 2 0.977523 0.260551 0.403031 11.00000 -1.50000
H24C 2 0.941197 0.189604 0.342420 11.00000 -1.50000
AFIX 0
C25 1 0.782783 0.202021 0.210323 11.00000 0.03320 0.02098 =
0.02377 -0.00055 0.01060 0.00855
AFIX 13
H25 2 0.734426 0.211443 0.169097 11.00000 -1.20000
AFIX 0
C26 1 0.767089 0.097989 0.235059 11.00000 0.06516 0.01685 =
0.03145 -0.00280 0.01873 0.00892
AFIX 137
H26A 2 0.810558 0.087336 0.276950 11.00000 -1.50000
H26B 2 0.774125 0.044865 0.206710 11.00000 -1.50000
H26C 2 0.706541 0.095205 0.237342 11.00000 -1.50000
AFIX 0
C27 1 0.871399 0.199731 0.196412 11.00000 0.04267 0.03346 =
0.02776 -0.00485 0.01299 0.01269
AFIX 137
H27A 2 0.881043 0.265542 0.179498 11.00000 -1.50000
H27B 2 0.868914 0.146375 0.165677 11.00000 -1.50000
H27C 2 0.920645 0.185819 0.235208 11.00000 -1.50000
AFIX 0
C28 1 0.639363 0.573940 0.127350 11.00000 0.02698 0.02016 =
0.01505 0.00305 0.00741 0.00441
AFIX 13
H28 2 0.643883 0.607454 0.167983 11.00000 -1.20000
AFIX 0
C29 1 0.544028 0.533401 0.101133 11.00000 0.02346 0.03406 =
0.02574 0.00037 0.00655 0.00775
AFIX 137
H29A 2 0.532714 0.508840 0.058273 11.00000 -1.50000
H29B 2 0.501853 0.587873 0.100826 11.00000 -1.50000
H29C 2 0.536357 0.477483 0.127482 11.00000 -1.50000
AFIX 0
C30 1 0.649929 0.659631 0.083871 11.00000 0.04431 0.02491 =
0.03160 0.01005 0.01252 0.00518
AFIX 137
H30A 2 0.707791 0.692999 0.102842 11.00000 -1.50000
H30B 2 0.601941 0.709369 0.077959 11.00000 -1.50000
H30C 2 0.646771 0.630984 0.043178 11.00000 -1.50000
AFIX 0
C31 1 0.833152 0.533304 0.139047 11.00000 0.02799 0.02810 =
0.02626 0.00199 0.01558 -0.00212
AFIX 13
H31 2 0.811935 0.567655 0.097261 11.00000 -1.20000
AFIX 0
C32 1 0.870290 0.618483 0.186776 11.00000 0.03058 0.03518 =
0.03486 -0.00633 0.01607 -0.01072
AFIX 137
H32A 2 0.822876 0.667614 0.184243 11.00000 -1.50000
H32B 2 0.919340 0.652615 0.177495 11.00000 -1.50000
H32C 2 0.892392 0.589663 0.229096 11.00000 -1.50000
AFIX 0
C33 1 0.908759 0.463587 0.136793 11.00000 0.03024 0.04326 =
0.04191 -0.00319 0.02071 -0.00246
AFIX 137
H33A 2 0.934952 0.430198 0.177509 11.00000 -1.50000
H33B 2 0.954664 0.503649 0.127232 11.00000 -1.50000
H33C 2 0.885230 0.412128 0.104191 11.00000 -1.50000
AFIX 0
C34 1 0.697575 0.367957 0.084938 11.00000 0.02855 0.01857 =
0.01834 0.00131 0.01021 0.00381
AFIX 13
H34 2 0.747620 0.317750 0.097164 11.00000 -1.20000
AFIX 0
C35 1 0.693784 0.408200 0.019649 11.00000 0.04011 0.02970 =
0.01999 -0.00003 0.01136 0.00271
AFIX 137
H35A 2 0.646968 0.459847 0.005571 11.00000 -1.50000
H35B 2 0.680485 0.351993 -0.010426 11.00000 -1.50000
H35C 2 0.751504 0.438197 0.022532 11.00000 -1.50000
AFIX 0
C36 1 0.612551 0.305999 0.077870 11.00000 0.03415 0.02181 =
0.02483 -0.00488 0.00719 -0.00141
AFIX 137
H36A 2 0.607816 0.293268 0.119376 11.00000 -1.50000
H36B 2 0.615576 0.241169 0.057425 11.00000 -1.50000
H36C 2 0.560147 0.344126 0.052312 11.00000 -1.50000
AFIX 0
HKLF 4
REM odpm65_a.res in P2(1)/c
REM R1 = 0.0286 for 6874 Fo > 4sig(Fo) and 0.0385 for all 8147 data
REM 421 parameters refined using 0 restraints
END
WGHT 0.0288 0.3095
REM Highest difference peak 0.842, deepest hole -0.489, 1-sigma level 0.080
Q1 1 0.6253 0.5237 0.2312 11.00000 0.05 0.84
Q2 1 0.7167 0.5305 0.3180 11.00000 0.05 0.80
Q3 1 0.9963 0.5265 0.1790 11.00000 0.05 0.47
Q4 1 0.6721 0.4045 0.2767 11.00000 0.05 0.45
Q5 1 0.8355 0.3212 0.2923 11.00000 0.05 0.45
Q6 1 0.7591 0.7172 0.3278 11.00000 0.05 0.42
Q7 1 0.7302 0.4208 0.1901 11.00000 0.05 0.41
Q8 1 0.5712 0.5226 0.2869 11.00000 0.05 0.40
Q9 1 0.6991 0.4350 0.1059 11.00000 0.05 0.40
Q10 1 0.6889 0.6045 0.3588 11.00000 0.05 0.39
Q11 1 0.7626 0.2147 0.3697 11.00000 0.05 0.36
Q12 1 0.7747 0.6229 0.2583 11.00000 0.05 0.36
Q13 1 0.8277 0.7196 0.4074 11.00000 0.05 0.35
Q14 1 0.7057 0.5836 0.4692 11.00000 0.05 0.35
Q15 1 0.7702 0.3931 0.2385 11.00000 0.05 0.34
Q16 1 0.5595 0.5169 0.4022 11.00000 0.05 0.34
Q17 1 0.7336 0.7845 0.3813 11.00000 0.05 0.34
Q18 1 0.7586 0.4629 0.1918 11.00000 0.05 0.34
Q19 1 0.7708 0.5393 0.3517 11.00000 0.05 0.33
Q20 1 0.5821 0.7189 0.2289 11.00000 0.05 0.33
;
_shelx_res_checksum 7571
_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 1.145
_oxdiff_exptl_absorpt_empirical_full_min 0.847
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_2-Br
_database_code_depnum_ccdc_archive 'CCDC 1833622'
_audit_update_record
;
2018-03-29 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;
_manchester_internal_coll_name odpm74
_manchester_internal_coll_client CAPG
_manchester_internal_coll_type custom
_manchester_internal_coll_frame_time 12.5
_manchester_internal_coll_frame_width 0.8
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user CAPG
_manchester_internal_coll_date 29/9/16
_manchester_internal_process_user CAPG
_manchester_internal_process_date 27/3/18
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 27/3/18
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 27/3/18
_manchester_internal_validation_user CAPG
_manchester_internal_validation_date 28/3/18
_manchester_internal_archive_date 28/3/18
_refine_special_details
;
Positional disorder was located at iPr groups C22-C24, and C25-C27. For
C22-C24, only C22 and C24 needed to be modelled as two components, which were
then refined competetively, converging at a ratio of 0.71(1)0.29(1). For
C25-C27, the whole group was modelled over two positions and refined
competetively, converging at a ratio of 0.518(6):0.482(6). Similarity
restraints (SIMU) were applied to every atom in the SiiPr3 group.
Additionally, equivalent Si-C and C-C distances in the whole structure were
refined to be approximately equal (SADI), and enhanced rigid bond restraints
(RIGU) were applied globally.
;
_audit_creation_date 2018-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2018/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H84 Br N2 Si4 Sm'
_chemical_formula_sum 'C36 H84 Br N2 Si4 Sm'
_chemical_formula_weight 887.67
_chemical_melting_point ?
_chemical_oxdiff_formula Sm(N(SiC9H21)2)2Br
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 61
_space_group_name_H-M_alt 'P b c a'
_space_group_name_Hall '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
_cell_length_a 20.6319(9)
_cell_length_b 20.1603(11)
_cell_length_c 21.9662(10)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 9136.7(8)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 7912
_cell_measurement_temperature 150.01(1)
_cell_measurement_theta_max 25.7600
_cell_measurement_theta_min 2.8970
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.289
_exptl_absorpt_correction_T_max 0.945
_exptl_absorpt_correction_T_min 0.913
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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_primary yellow
_exptl_crystal_density_diffrn 1.291
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 3736
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 -19 23 0.2256
-25 -2 17 0.4308
-3 18 -23 0.0746
-23 16 -11 0.1928
-9 -12 -27 0.0856
28 -10 1 0.0957
9 -7 -28 0.0696
-16 -23 -6 0.2082
-3 27 8 0.1683
9 27 1 0.0965
18 22 -6 0.0777
2 -23 -18 0.0747
25 2 -15 0.0508
11 12 25 0.1541
-25 -11 -12 0.2065
_exptl_crystal_preparation 'By Benjamin Reant and CAPG.'
_exptl_crystal_recrystallization_method 'From hexane.'
_exptl_crystal_size_max 0.494
_exptl_crystal_size_mid 0.356
_exptl_crystal_size_min 0.259
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
4.5007 -18.5118 22.9939 0.2720 -0.9185 -0.2855
-24.5053 -1.5034 17.0118 -0.0663 -0.0480 -1.0049
-3.0004 18.0116 -22.9947 -0.2625 0.8868 0.3288
-22.5044 15.5093 -10.9867 -0.2539 0.8682 -0.4513
-8.9986 -11.9897 -27.0137 0.7717 0.6524 0.1136
27.5054 -9.5054 0.9859 0.1706 -0.6122 0.7772
9.0041 -6.9912 -28.0162 0.5472 0.4552 0.6849
-15.5002 -23.4983 -6.0126 0.8942 0.0651 -0.4472
-3.0034 27.0006 8.0210 -0.9515 0.2378 -0.1269
8.9991 27.0016 1.0152 -0.9127 0.2173 0.3422
18.0016 22.0025 -5.9930 -0.7016 0.1738 0.7050
2.0036 -22.9960 -18.0213 0.9580 0.0876 0.2664
25.0052 2.0026 -15.0110 0.0223 -0.0033 0.9902
10.9991 11.9902 25.0125 -0.7545 -0.6349 -0.0224
-24.5024 -11.4933 -12.0040 0.6285 0.5363 -0.5838
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0675
_diffrn_reflns_av_unetI/netI 0.0743
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 32776
_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 2.404
_diffrn_ambient_temperature 150.01(1)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.1636
_diffrn_detector_type Atlas
_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 35.00 101.40 0.80 12.50 -- 11.54 178.00 120.00 83
2 \w -79.00 11.40 0.80 12.50 -- -12.00 -57.00-120.00 113
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0043460000
_diffrn_orient_matrix_UB_12 -0.0318670000
_diffrn_orient_matrix_UB_13 -0.0129763000
_diffrn_orient_matrix_UB_21 -0.0163630000
_diffrn_orient_matrix_UB_22 0.0144471000
_diffrn_orient_matrix_UB_23 -0.0251130000
_diffrn_orient_matrix_UB_31 0.0299499000
_diffrn_orient_matrix_UB_32 0.0032782000
_diffrn_orient_matrix_UB_33 -0.0156382000
_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'
_diffrn_special_details ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5518
_reflns_number_total 8310
_reflns_odcompleteness_completeness 98.62
_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 0.698
_refine_diff_density_min -1.119
_refine_diff_density_rms 0.105
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 467
_refine_ls_number_reflns 8310
_refine_ls_number_restraints 914
_refine_ls_R_factor_all 0.0857
_refine_ls_R_factor_gt 0.0459
_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^)+(0.0361P)^2^+3.7975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0889
_refine_ls_wR_factor_ref 0.1063
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
C26B-C25B \\sim C27B-C25B \\sim C26A-C25A \\sim C27A-C25A \\sim C20-C19 \\sim
C21-C19 \\sim C32-C31 ~
C33-C31 \\sim C29-C28 \\sim C30-C28 \\sim C35-C34 \\sim C36-C34 \\sim C2-C1
\\sim C3-C1 \\sim C9-C7 \\sim C8-
C7 \\sim C5-C4 \\sim C6-C4 \\sim C23-C22A \\sim C24A-C22A \\sim C14-C13 \\sim
C15-C13 \\sim C12-C10 \\sim C11-
C10 \\sim C17-C16 \\sim C18-C16
with sigma of 0.008
Si3-C22A \\sim Si3-C22B \\sim Si3-C25A \\sim Si3-C25B \\sim Si3-C19 \\sim
Si4-C31 \\sim Si4-C34 \\sim Si2-
C10 \\sim Si2-C16 \\sim Si2-C13 \\sim Si1-C1 \\sim Si1-C7 \\sim Si1-C4 \\sim
Si4-C28
with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
Si3 \\sim C19 \\sim C20 \\sim C21 \\sim C23 \\sim C25A \\sim C27A \\sim C26A
\\sim C22B \\sim C24B \\sim C22A \\sim C24A \\sim C25B \\sim C26B \\sim C27B:
within 2A with sigma of 0.008 and sigma for terminal atoms of 0.008
4. Rigid body (RIGU) restrains
All non-hydrogen atoms
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
Sof(C25B)=Sof(H25B)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27B)=
Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(1)
Sof(C25A)=Sof(H25A)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C26A)=
Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C22A)=Sof(H22A)=Sof(C24A)=Sof(H24D)=
Sof(H24E)=Sof(H24F)=1-FVAR(2)
Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C22B)=Sof(H22B)=Sof(C24B)=Sof(H24A)=
Sof(H24B)=Sof(H24C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16), C19(H19), C28(H28),
C31(H31), C34(H34), C25A(H25A), C22B(H22B), C22A(H22A), C25B(H25B)
6.b Me refined with riding coordinates:
C27A(H27A,H27B,H27C), C26A(H26A,H26B,H26C), C26B(H26D,H26E,H26F), C27B(H27D,
H27E,H27F)
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(H23D,H23E,H23F), C23(H23A,H23B,
H23C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C24B(H24A,H24B,H24C),
C24A(H24D,H24E,H24F)
;
_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
Sm1 Sm 0.30532(2) 0.34297(2) 0.61487(2) 0.03782(10) Uani 1 1 d . U . . .
Br1 Br 0.23637(3) 0.25878(3) 0.68854(3) 0.06024(19) Uani 1 1 d . U . . .
Si1 Si 0.27916(6) 0.32993(7) 0.46279(6) 0.0333(3) Uani 1 1 d D U . . .
Si2 Si 0.17933(6) 0.41966(7) 0.52867(6) 0.0335(3) Uani 1 1 d D U . . .
Si3 Si 0.38571(7) 0.46571(8) 0.68844(7) 0.0437(4) Uani 1 1 d D U . . .
Si4 Si 0.46269(6) 0.33086(7) 0.66971(6) 0.0360(4) Uani 1 1 d D U . . .
N1 N 0.24908(16) 0.37013(19) 0.52731(16) 0.0285(9) Uani 1 1 d . U . . .
N2 N 0.39759(17) 0.3857(2) 0.66145(17) 0.0323(9) Uani 1 1 d . U . . .
C1 C 0.3383(2) 0.2669(2) 0.4974(2) 0.0413(13) Uani 1 1 d D U . . .
H1 H 0.363912 0.292211 0.528320 0.050 Uiso 1 1 calc R . . . .
C2 C 0.3027(3) 0.2122(3) 0.5334(2) 0.0542(15) Uani 1 1 d D U . . .
H2A H 0.273324 0.232632 0.563039 0.081 Uiso 1 1 calc GR . . . .
H2B H 0.334446 0.184576 0.554872 0.081 Uiso 1 1 calc GR . . . .
H2C H 0.277665 0.184514 0.505239 0.081 Uiso 1 1 calc GR . . . .
C3 C 0.3890(3) 0.2345(3) 0.4552(2) 0.0652(18) Uani 1 1 d D U . . .
H3A H 0.366726 0.209675 0.423003 0.098 Uiso 1 1 calc GR . . . .
H3B H 0.416209 0.204213 0.478883 0.098 Uiso 1 1 calc GR . . . .
H3C H 0.416086 0.269028 0.436822 0.098 Uiso 1 1 calc GR . . . .
C4 C 0.3260(2) 0.3879(2) 0.41050(19) 0.0457(14) Uani 1 1 d D U . . .
H4 H 0.295882 0.425627 0.401691 0.055 Uiso 1 1 calc R . . . .
C5 C 0.3844(2) 0.4190(3) 0.4435(3) 0.0631(17) Uani 1 1 d D U . . .
H5A H 0.370450 0.436365 0.483027 0.095 Uiso 1 1 calc GR . . . .
H5B H 0.402048 0.455165 0.418768 0.095 Uiso 1 1 calc GR . . . .
H5C H 0.417814 0.385098 0.449641 0.095 Uiso 1 1 calc GR . . . .
C6 C 0.3476(3) 0.3616(3) 0.3479(2) 0.0674(19) Uani 1 1 d D U . . .
H6A H 0.378912 0.325624 0.353556 0.101 Uiso 1 1 calc GR . . . .
H6B H 0.367756 0.397595 0.324663 0.101 Uiso 1 1 calc GR . . . .
H6C H 0.309763 0.344893 0.325687 0.101 Uiso 1 1 calc GR . . . .
C7 C 0.2159(2) 0.2832(2) 0.4157(2) 0.0439(13) Uani 1 1 d D U . . .
H7 H 0.182941 0.266490 0.445357 0.053 Uiso 1 1 calc R . . . .
C8 C 0.1785(3) 0.3274(3) 0.3702(2) 0.0562(16) Uani 1 1 d D U . . .
H8A H 0.160919 0.366017 0.391697 0.084 Uiso 1 1 calc GR . . . .
H8B H 0.142937 0.301929 0.352165 0.084 Uiso 1 1 calc GR . . . .
H8C H 0.208017 0.342293 0.338062 0.084 Uiso 1 1 calc GR . . . .
C9 C 0.2400(3) 0.2219(3) 0.3807(3) 0.0691(19) Uani 1 1 d D U . . .
H9A H 0.274621 0.235068 0.352626 0.104 Uiso 1 1 calc GR . . . .
H9B H 0.204064 0.202545 0.357616 0.104 Uiso 1 1 calc GR . . . .
H9C H 0.256789 0.189092 0.409605 0.104 Uiso 1 1 calc GR . . . .
C10 C 0.1761(2) 0.4630(2) 0.60642(18) 0.0392(13) Uani 1 1 d D U . . .
H10 H 0.221964 0.473701 0.617225 0.047 Uiso 1 1 calc R . . . .
C11 C 0.1500(3) 0.4194(3) 0.6587(2) 0.0599(16) Uani 1 1 d D U . . .
H11A H 0.103672 0.411120 0.652479 0.090 Uiso 1 1 calc GR . . . .
H11B H 0.156424 0.442302 0.697576 0.090 Uiso 1 1 calc GR . . . .
H11C H 0.173379 0.377085 0.659216 0.090 Uiso 1 1 calc GR . . . .
C12 C 0.1390(3) 0.5292(3) 0.6083(3) 0.0686(19) Uani 1 1 d D U . . .
H12A H 0.158999 0.560579 0.579854 0.103 Uiso 1 1 calc GR . . . .
H12B H 0.140792 0.547512 0.649650 0.103 Uiso 1 1 calc GR . . . .
H12C H 0.093750 0.521804 0.596747 0.103 Uiso 1 1 calc GR . . . .
C13 C 0.1859(2) 0.4849(2) 0.4662(2) 0.0463(14) Uani 1 1 d D U . . .
H13 H 0.196738 0.459853 0.428279 0.056 Uiso 1 1 calc R . . . .
C14 C 0.2431(2) 0.5327(3) 0.4763(3) 0.0613(17) Uani 1 1 d D U . . .
H14A H 0.233747 0.561575 0.511160 0.092 Uiso 1 1 calc GR . . . .
H14B H 0.249379 0.559921 0.439816 0.092 Uiso 1 1 calc GR . . . .
H14C H 0.282549 0.507166 0.484457 0.092 Uiso 1 1 calc GR . . . .
C15 C 0.1251(3) 0.5258(3) 0.4506(3) 0.071(2) Uani 1 1 d D U . . .
H15A H 0.090641 0.496054 0.436511 0.106 Uiso 1 1 calc GR . . . .
H15B H 0.135478 0.557744 0.418382 0.106 Uiso 1 1 calc GR . . . .
H15C H 0.110367 0.549696 0.486917 0.106 Uiso 1 1 calc GR . . . .
C16 C 0.10253(18) 0.3681(2) 0.5171(2) 0.0456(14) Uani 1 1 d D U . . .
H16 H 0.101139 0.356970 0.472808 0.055 Uiso 1 1 calc R . . . .
C17 C 0.1029(2) 0.3015(3) 0.5509(3) 0.0589(16) Uani 1 1 d D U . . .
H17A H 0.144656 0.279466 0.544645 0.088 Uiso 1 1 calc GR . . . .
H17B H 0.067978 0.273361 0.535183 0.088 Uiso 1 1 calc GR . . . .
H17C H 0.096183 0.309249 0.594522 0.088 Uiso 1 1 calc GR . . . .
C18 C 0.0385(2) 0.4050(3) 0.5310(3) 0.0648(18) Uani 1 1 d D U . . .
H18A H 0.036571 0.415831 0.574425 0.097 Uiso 1 1 calc GR . . . .
H18B H 0.001712 0.376590 0.520215 0.097 Uiso 1 1 calc GR . . . .
H18C H 0.036670 0.445981 0.507030 0.097 Uiso 1 1 calc GR . . . .
C19 C 0.3037(2) 0.4628(3) 0.7288(3) 0.0641(15) Uani 1 1 d D U . . .
H19 H 0.273571 0.445330 0.696935 0.077 Uiso 1 1 calc R . . . .
C20 C 0.2982(3) 0.4117(3) 0.7805(3) 0.0729(18) Uani 1 1 d D U . . .
H20A H 0.315551 0.369049 0.766642 0.109 Uiso 1 1 calc GR . . . .
H20B H 0.252642 0.406409 0.791954 0.109 Uiso 1 1 calc GR . . . .
H20C H 0.323089 0.427168 0.815758 0.109 Uiso 1 1 calc GR . . . .
C21 C 0.2720(3) 0.5281(4) 0.7485(4) 0.120(3) Uani 1 1 d D U . . .
H21A H 0.278956 0.534885 0.792145 0.179 Uiso 1 1 calc GR . . . .
H21B H 0.225352 0.526236 0.740089 0.179 Uiso 1 1 calc GR . . . .
H21C H 0.291333 0.564919 0.725716 0.179 Uiso 1 1 calc GR . . . .
C23 C 0.4305(3) 0.5208(3) 0.5761(3) 0.0828(19) Uani 1 1 d D U . . .
H23D H 0.455035 0.560159 0.588491 0.124 Uiso 0.702(11) 1 calc GR . P A 2
H23E H 0.418435 0.524742 0.533089 0.124 Uiso 0.702(11) 1 calc GR . P A 2
H23F H 0.457317 0.481148 0.581804 0.124 Uiso 0.702(11) 1 calc GR . P A 2
H23A H 0.472057 0.534182 0.593866 0.124 Uiso 0.298(11) 1 calc GR . P A 1
H23B H 0.419941 0.550135 0.541932 0.124 Uiso 0.298(11) 1 calc GR . P A 1
H23C H 0.433588 0.474957 0.561498 0.124 Uiso 0.298(11) 1 calc GR . P A 1
C28 C 0.4299(2) 0.24415(19) 0.6507(2) 0.0410(13) Uani 1 1 d D U . . .
H28 H 0.393404 0.251627 0.621523 0.049 Uiso 1 1 calc R . . . .
C29 C 0.3999(3) 0.2066(3) 0.7051(2) 0.0592(16) Uani 1 1 d D U . . .
H29A H 0.434444 0.191200 0.732213 0.089 Uiso 1 1 calc GR . . . .
H29B H 0.375163 0.168442 0.690126 0.089 Uiso 1 1 calc GR . . . .
H29C H 0.370891 0.236423 0.727528 0.089 Uiso 1 1 calc GR . . . .
C30 C 0.4765(3) 0.1957(3) 0.6181(3) 0.0644(17) Uani 1 1 d D U . . .
H30A H 0.494710 0.217173 0.581938 0.097 Uiso 1 1 calc GR . . . .
H30B H 0.452745 0.155749 0.605941 0.097 Uiso 1 1 calc GR . . . .
H30C H 0.511740 0.183358 0.645882 0.097 Uiso 1 1 calc GR . . . .
C31 C 0.5023(2) 0.3289(3) 0.74835(18) 0.0451(14) Uani 1 1 d D U . . .
H31 H 0.522062 0.373786 0.754056 0.054 Uiso 1 1 calc R . . . .
C32 C 0.4579(3) 0.3184(4) 0.8036(2) 0.0673(19) Uani 1 1 d D U . . .
H32A H 0.416587 0.341141 0.796817 0.101 Uiso 1 1 calc GR . . . .
H32B H 0.478797 0.336462 0.840120 0.101 Uiso 1 1 calc GR . . . .
H32C H 0.450081 0.270837 0.809254 0.101 Uiso 1 1 calc GR . . . .
C33 C 0.5593(2) 0.2793(3) 0.7519(3) 0.0616(17) Uani 1 1 d D U . . .
H33A H 0.543736 0.234710 0.741825 0.092 Uiso 1 1 calc GR . . . .
H33B H 0.577141 0.279306 0.793285 0.092 Uiso 1 1 calc GR . . . .
H33C H 0.593077 0.292426 0.723009 0.092 Uiso 1 1 calc GR . . . .
C34 C 0.5325(2) 0.3436(3) 0.6139(2) 0.0616(17) Uani 1 1 d D U . . .
H34 H 0.558711 0.301994 0.616467 0.074 Uiso 1 1 calc R . . . .
C35 C 0.5801(3) 0.3995(3) 0.6285(3) 0.091(2) Uani 1 1 d D U . . .
H35A H 0.560104 0.442328 0.618901 0.136 Uiso 1 1 calc GR . . . .
H35B H 0.619509 0.393894 0.604118 0.136 Uiso 1 1 calc GR . . . .
H35C H 0.591253 0.398102 0.671856 0.136 Uiso 1 1 calc GR . . . .
C36 C 0.5106(3) 0.3478(4) 0.5473(2) 0.075(2) Uani 1 1 d D U . . .
H36A H 0.482035 0.310287 0.538030 0.113 Uiso 1 1 calc GR . . . .
H36B H 0.548641 0.346272 0.520617 0.113 Uiso 1 1 calc GR . . . .
H36C H 0.487163 0.389440 0.540710 0.113 Uiso 1 1 calc GR . . . .
C25A C 0.4438(4) 0.4972(7) 0.7502(4) 0.066(2) Uani 0.518(6) 1 d D U P A 1
H25A H 0.453911 0.457419 0.775708 0.079 Uiso 0.518(6) 1 calc R . P A 1
C27A C 0.5098(5) 0.5221(7) 0.7271(6) 0.078(3) Uani 0.518(6) 1 d D U P A 1
H27A H 0.527639 0.490237 0.697885 0.118 Uiso 0.518(6) 1 calc R . P A 1
H27B H 0.504240 0.565238 0.707183 0.118 Uiso 0.518(6) 1 calc R . P A 1
H27C H 0.539650 0.526797 0.761560 0.118 Uiso 0.518(6) 1 calc R . P A 1
C26A C 0.4203(4) 0.5504(6) 0.7953(5) 0.075(2) Uani 0.518(6) 1 d D U P A 1
H26A H 0.378078 0.537432 0.811910 0.113 Uiso 0.518(6) 1 calc R . P A 1
H26B H 0.451690 0.554577 0.828635 0.113 Uiso 0.518(6) 1 calc R . P A 1
H26C H 0.416280 0.593018 0.774258 0.113 Uiso 0.518(6) 1 calc R . P A 1
C22B C 0.3816(14) 0.5252(12) 0.6206(9) 0.070(2) Uani 0.298(11) 1 d D U P A 1
H22B H 0.339138 0.517601 0.599688 0.085 Uiso 0.298(11) 1 calc R . P A 1
C24B C 0.3840(13) 0.6068(11) 0.6421(11) 0.078(3) Uani 0.298(11) 1 d . U P A 1
H24A H 0.342262 0.619297 0.660010 0.117 Uiso 0.298(11) 1 calc GR . P A 1
H24B H 0.392565 0.634530 0.606345 0.117 Uiso 0.298(11) 1 calc GR . P A 1
H24C H 0.418508 0.613130 0.672135 0.117 Uiso 0.298(11) 1 calc GR . P A 1
C22A C 0.3690(4) 0.5150(5) 0.6151(3) 0.069(2) Uani 0.702(11) 1 d D U P A 2
H22A H 0.338489 0.486895 0.590829 0.082 Uiso 0.702(11) 1 calc R . P A 2
C24A C 0.3366(5) 0.5836(4) 0.6189(5) 0.081(2) Uani 0.702(11) 1 d D U P A 2
H24D H 0.290398 0.578226 0.628009 0.121 Uiso 0.702(11) 1 calc GR . P A 2
H24E H 0.341590 0.606710 0.579922 0.121 Uiso 0.702(11) 1 calc GR . P A 2
H24F H 0.357187 0.609673 0.651236 0.121 Uiso 0.702(11) 1 calc GR . P A 2
C25B C 0.4564(5) 0.5050(6) 0.7313(5) 0.067(2) Uani 0.482(6) 1 d D U P A 2
H25B H 0.497016 0.484442 0.715043 0.080 Uiso 0.482(6) 1 calc R . P A 2
C26B C 0.4535(6) 0.4885(7) 0.7995(5) 0.071(3) Uani 0.482(6) 1 d D U P A 2
H26D H 0.449320 0.440380 0.804782 0.107 Uiso 0.482(6) 1 calc R . P A 2
H26E H 0.493218 0.503847 0.819436 0.107 Uiso 0.482(6) 1 calc R . P A 2
H26F H 0.415953 0.510614 0.817840 0.107 Uiso 0.482(6) 1 calc R . P A 2
C27B C 0.4630(7) 0.5805(6) 0.7225(6) 0.078(2) Uani 0.482(6) 1 d D U P A 2
H27D H 0.464836 0.590693 0.678941 0.117 Uiso 0.482(6) 1 calc R . P A 2
H27E H 0.425466 0.602781 0.740725 0.117 Uiso 0.482(6) 1 calc R . P A 2
H27F H 0.502731 0.596014 0.742321 0.117 Uiso 0.482(6) 1 calc R . P A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sm1 0.03437(15) 0.04453(19) 0.03458(18) 0.00326(13) -0.00286(12) -0.00659(12)
Br1 0.0502(3) 0.0694(5) 0.0611(4) 0.0187(3) 0.0088(3) -0.0061(3)
Si1 0.0384(7) 0.0310(8) 0.0304(8) -0.0008(6) 0.0023(6) 0.0061(6)
Si2 0.0304(7) 0.0314(8) 0.0389(8) -0.0007(7) 0.0036(6) 0.0038(6)
Si3 0.0429(8) 0.0367(9) 0.0514(10) -0.0063(7) 0.0005(7) -0.0021(7)
Si4 0.0307(7) 0.0414(9) 0.0360(8) 0.0028(7) -0.0003(6) -0.0014(6)
N1 0.030(2) 0.022(2) 0.033(2) -0.0026(18) 0.0024(18) 0.0013(16)
N2 0.031(2) 0.036(3) 0.030(2) 0.0019(19) 0.0005(18) -0.0018(17)
C1 0.052(3) 0.039(3) 0.033(3) -0.006(3) -0.002(3) 0.015(3)
C2 0.083(4) 0.035(3) 0.044(3) 0.002(3) -0.014(3) 0.007(3)
C3 0.071(4) 0.068(5) 0.058(4) -0.013(3) 0.001(3) 0.039(3)
C4 0.043(3) 0.046(4) 0.048(3) 0.012(3) 0.010(3) 0.010(3)
C5 0.049(3) 0.067(5) 0.074(4) 0.007(3) 0.019(3) -0.006(3)
C6 0.072(4) 0.084(5) 0.046(4) 0.011(3) 0.025(3) 0.019(4)
C7 0.056(3) 0.045(4) 0.031(3) -0.004(3) -0.001(3) 0.001(3)
C8 0.062(4) 0.064(5) 0.042(3) -0.005(3) -0.017(3) 0.003(3)
C9 0.097(5) 0.050(4) 0.061(4) -0.021(3) -0.023(4) 0.008(4)
C10 0.037(3) 0.038(3) 0.043(3) -0.001(2) 0.012(2) 0.009(2)
C11 0.064(4) 0.067(4) 0.049(4) -0.002(3) 0.013(3) -0.001(3)
C12 0.085(5) 0.048(4) 0.073(5) -0.012(3) 0.021(4) 0.007(3)
C13 0.055(3) 0.033(3) 0.050(3) 0.008(3) 0.006(3) 0.015(3)
C14 0.069(4) 0.038(4) 0.077(5) 0.015(3) 0.022(3) 0.002(3)
C15 0.068(4) 0.078(5) 0.065(4) 0.022(4) 0.005(3) 0.035(4)
C16 0.033(3) 0.058(4) 0.046(3) -0.004(3) 0.000(3) -0.002(2)
C17 0.044(3) 0.056(4) 0.077(4) -0.005(3) 0.007(3) -0.016(3)
C18 0.030(3) 0.071(5) 0.093(5) 0.002(4) -0.001(3) 0.005(3)
C19 0.058(3) 0.070(4) 0.064(3) -0.024(3) 0.005(3) 0.008(3)
C20 0.063(4) 0.095(5) 0.061(4) -0.010(4) 0.011(3) -0.017(3)
C21 0.123(5) 0.109(6) 0.127(6) -0.033(5) 0.042(5) 0.034(5)
C23 0.085(4) 0.059(4) 0.105(4) 0.013(4) 0.012(4) -0.007(3)
C28 0.042(3) 0.034(3) 0.047(3) -0.006(3) -0.012(3) 0.007(2)
C29 0.055(3) 0.049(4) 0.074(4) 0.014(3) -0.012(3) -0.011(3)
C30 0.076(4) 0.048(4) 0.069(4) -0.007(3) -0.002(3) 0.013(3)
C31 0.039(3) 0.056(4) 0.040(3) -0.001(3) -0.007(3) -0.003(2)
C32 0.071(4) 0.092(6) 0.040(4) 0.002(3) -0.011(3) -0.005(4)
C33 0.055(4) 0.073(5) 0.057(4) 0.000(3) -0.019(3) 0.008(3)
C34 0.043(3) 0.074(5) 0.068(4) 0.009(4) 0.007(3) -0.002(3)
C35 0.060(4) 0.089(6) 0.124(6) 0.017(5) 0.012(4) -0.027(4)
C36 0.075(4) 0.090(6) 0.061(4) 0.021(4) 0.023(4) 0.003(4)
C25A 0.059(4) 0.058(4) 0.082(4) -0.018(4) -0.004(4) -0.012(3)
C27A 0.069(5) 0.070(5) 0.097(5) -0.019(5) 0.000(5) -0.018(4)
C26A 0.072(4) 0.068(5) 0.086(5) -0.022(4) -0.005(4) -0.014(4)
C22B 0.072(4) 0.044(4) 0.095(4) 0.010(4) 0.014(4) 0.003(4)
C24B 0.084(6) 0.047(5) 0.104(6) 0.009(5) 0.013(5) 0.004(5)
C22A 0.067(4) 0.043(4) 0.097(4) 0.009(3) 0.013(3) 0.001(3)
C24A 0.082(5) 0.048(4) 0.112(5) 0.016(4) 0.014(4) 0.008(4)
C25B 0.060(4) 0.058(4) 0.083(4) -0.018(4) -0.006(4) -0.014(3)
C26B 0.066(5) 0.066(5) 0.082(5) -0.023(5) -0.010(5) -0.011(4)
C27B 0.074(5) 0.065(5) 0.094(5) -0.019(5) -0.007(4) -0.020(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 Br1 2.7428(6) . ?
Sm1 N1 2.312(4) . ?
Sm1 N2 2.327(4) . ?
Si1 N1 1.747(4) . ?
Si1 C1 1.919(4) . ?
Si1 C4 1.903(4) . ?
Si1 C7 1.915(4) . ?
Si2 N1 1.752(4) . ?
Si2 C10 1.919(4) . ?
Si2 C13 1.906(4) . ?
Si2 C16 1.912(4) . ?
Si3 N2 1.736(4) . ?
Si3 C19 1.912(4) . ?
Si3 C25A 1.917(6) . ?
Si3 C22B 1.916(6) . ?
Si3 C22A 1.925(5) . ?
Si3 C25B 1.909(6) . ?
Si4 N2 1.749(4) . ?
Si4 C28 1.920(4) . ?
Si4 C31 1.911(4) . ?
Si4 C34 1.909(4) . ?
C1 H1 1.0000 . ?
C1 C2 1.545(5) . ?
C1 C3 1.542(4) . ?
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 1.539(5) . ?
C4 C6 1.540(5) . ?
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 1.544(5) . ?
C7 C9 1.537(5) . ?
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 1.543(5) . ?
C10 C12 1.539(5) . ?
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 1.539(5) . ?
C13 C15 1.541(5) . ?
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 1.533(5) . ?
C16 C18 1.546(5) . ?
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 1.537(5) . ?
C19 C21 1.531(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 H23D 0.9800 . ?
C23 H23E 0.9800 . ?
C23 H23F 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C23 C22B 1.41(2) . ?
C23 C22A 1.536(6) . ?
C28 H28 1.0000 . ?
C28 C29 1.545(5) . ?
C28 C30 1.547(5) . ?
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 1.536(5) . ?
C31 C33 1.545(5) . ?
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 1.529(5) . ?
C34 C36 1.533(5) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C25A H25A 1.0000 . ?
C25A C27A 1.538(6) . ?
C25A C26A 1.540(6) . ?
C27A H27A 0.9800 . ?
C27A H27B 0.9800 . ?
C27A H27C 0.9800 . ?
C26A H26A 0.9800 . ?
C26A H26B 0.9800 . ?
C26A H26C 0.9800 . ?
C22B H22B 1.0000 . ?
C22B C24B 1.71(3) . ?
C24B H24A 0.9800 . ?
C24B H24B 0.9800 . ?
C24B H24C 0.9800 . ?
C22A H22A 1.0000 . ?
C22A C24A 1.538(6) . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C25B H25B 1.0000 . ?
C25B C26B 1.536(6) . ?
C25B C27B 1.540(6) . ?
C26B H26D 0.9800 . ?
C26B H26E 0.9800 . ?
C26B H26F 0.9800 . ?
C27B H27D 0.9800 . ?
C27B H27E 0.9800 . ?
C27B H27F 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Sm1 Br1 112.15(9) . . ?
N1 Sm1 N2 133.55(13) . . ?
N2 Sm1 Br1 113.20(9) . . ?
N1 Si1 C1 102.23(19) . . ?
N1 Si1 C4 112.6(2) . . ?
N1 Si1 C7 115.2(2) . . ?
C4 Si1 C1 108.8(2) . . ?
C4 Si1 C7 108.8(2) . . ?
C7 Si1 C1 108.8(2) . . ?
N1 Si2 C10 107.66(19) . . ?
N1 Si2 C13 108.82(19) . . ?
N1 Si2 C16 111.64(19) . . ?
C13 Si2 C10 109.2(2) . . ?
C13 Si2 C16 109.8(2) . . ?
C16 Si2 C10 109.6(2) . . ?
N2 Si3 C19 104.8(2) . . ?
N2 Si3 C25A 117.4(4) . . ?
N2 Si3 C22B 108.8(9) . . ?
N2 Si3 C22A 102.7(3) . . ?
N2 Si3 C25B 116.5(5) . . ?
C19 Si3 C25A 103.6(3) . . ?
C19 Si3 C22B 109.9(8) . . ?
C19 Si3 C22A 104.2(3) . . ?
C22B Si3 C25A 111.8(11) . . ?
C25B Si3 C19 117.4(5) . . ?
C25B Si3 C22A 109.6(5) . . ?
N2 Si4 C28 106.38(19) . . ?
N2 Si4 C31 115.8(2) . . ?
N2 Si4 C34 115.3(2) . . ?
C31 Si4 C28 109.2(2) . . ?
C34 Si4 C28 104.4(2) . . ?
C34 Si4 C31 105.1(2) . . ?
Si1 N1 Sm1 112.76(18) . . ?
Si1 N1 Si2 124.8(2) . . ?
Si2 N1 Sm1 122.22(19) . . ?
Si3 N2 Sm1 112.24(18) . . ?
Si3 N2 Si4 131.3(2) . . ?
Si4 N2 Sm1 116.1(2) . . ?
Si1 C1 H1 105.5 . . ?
C2 C1 Si1 111.9(3) . . ?
C2 C1 H1 105.5 . . ?
C3 C1 Si1 118.3(3) . . ?
C3 C1 H1 105.5 . . ?
C3 C1 C2 109.1(4) . . ?
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 105.6 . . ?
C5 C4 Si1 111.3(3) . . ?
C5 C4 H4 105.6 . . ?
C5 C4 C6 109.5(4) . . ?
C6 C4 Si1 118.3(4) . . ?
C6 C4 H4 105.6 . . ?
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 106.0 . . ?
C8 C7 Si1 113.9(3) . . ?
C8 C7 H7 106.0 . . ?
C9 C7 Si1 116.4(3) . . ?
C9 C7 H7 106.0 . . ?
C9 C7 C8 107.6(4) . . ?
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 106.0 . . ?
C11 C10 Si2 114.5(3) . . ?
C11 C10 H10 106.0 . . ?
C12 C10 Si2 115.9(3) . . ?
C12 C10 H10 106.0 . . ?
C12 C10 C11 107.5(4) . . ?
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 105.5 . . ?
C14 C13 Si2 112.5(3) . . ?
C14 C13 H13 105.5 . . ?
C14 C13 C15 108.8(5) . . ?
C15 C13 Si2 118.1(3) . . ?
C15 C13 H13 105.5 . . ?
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 105.9 . . ?
C17 C16 Si2 114.1(3) . . ?
C17 C16 H16 105.9 . . ?
C17 C16 C18 109.3(4) . . ?
C18 C16 Si2 114.9(3) . . ?
C18 C16 H16 105.9 . . ?
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 103.6 . . ?
C20 C19 Si3 115.3(4) . . ?
C20 C19 H19 103.6 . . ?
C21 C19 Si3 118.9(4) . . ?
C21 C19 H19 103.6 . . ?
C21 C19 C20 109.7(5) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 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 . . ?
H23D C23 H23E 109.5 . . ?
H23D C23 H23F 109.5 . . ?
H23E C23 H23F 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22B C23 H23A 109.5 . . ?
C22B C23 H23B 109.5 . . ?
C22B C23 H23C 109.5 . . ?
C22A C23 H23D 109.5 . . ?
C22A C23 H23E 109.5 . . ?
C22A C23 H23F 109.5 . . ?
Si4 C28 H28 105.5 . . ?
C29 C28 Si4 114.8(3) . . ?
C29 C28 H28 105.5 . . ?
C29 C28 C30 107.3(4) . . ?
C30 C28 Si4 117.2(4) . . ?
C30 C28 H28 105.5 . . ?
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 105.6 . . ?
C32 C31 Si4 117.6(3) . . ?
C32 C31 H31 105.6 . . ?
C32 C31 C33 108.9(4) . . ?
C33 C31 Si4 112.6(3) . . ?
C33 C31 H31 105.6 . . ?
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 105.0 . . ?
C35 C34 Si4 116.7(4) . . ?
C35 C34 H34 105.0 . . ?
C35 C34 C36 110.4(5) . . ?
C36 C34 Si4 113.5(4) . . ?
C36 C34 H34 105.0 . . ?
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 . . ?
Si3 C25A H25A 105.2 . . ?
C27A C25A Si3 115.4(7) . . ?
C27A C25A H25A 105.2 . . ?
C27A C25A C26A 105.2(9) . . ?
C26A C25A Si3 119.3(7) . . ?
C26A C25A H25A 105.2 . . ?
C25A C27A H27A 109.5 . . ?
C25A C27A H27B 109.5 . . ?
C25A C27A H27C 109.5 . . ?
H27A C27A H27B 109.5 . . ?
H27A C27A H27C 109.5 . . ?
H27B C27A H27C 109.5 . . ?
C25A C26A H26A 109.5 . . ?
C25A C26A H26B 109.5 . . ?
C25A C26A H26C 109.5 . . ?
H26A C26A H26B 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
Si3 C22B H22B 107.4 . . ?
C23 C22B Si3 117.9(13) . . ?
C23 C22B H22B 107.4 . . ?
C23 C22B C24B 103.4(16) . . ?
C24B C22B Si3 112.7(16) . . ?
C24B C22B H22B 107.4 . . ?
C22B C24B H24A 109.5 . . ?
C22B C24B H24B 109.5 . . ?
C22B C24B H24C 109.5 . . ?
H24A C24B H24B 109.5 . . ?
H24A C24B H24C 109.5 . . ?
H24B C24B H24C 109.5 . . ?
Si3 C22A H22A 105.4 . . ?
C23 C22A Si3 110.9(5) . . ?
C23 C22A H22A 105.4 . . ?
C23 C22A C24A 108.7(6) . . ?
C24A C22A Si3 119.8(6) . . ?
C24A C22A H22A 105.4 . . ?
C22A C24A H24D 109.5 . . ?
C22A C24A H24E 109.5 . . ?
C22A C24A H24F 109.5 . . ?
H24D C24A H24E 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
Si3 C25B H25B 107.0 . . ?
C26B C25B Si3 111.1(7) . . ?
C26B C25B H25B 107.0 . . ?
C26B C25B C27B 109.9(10) . . ?
C27B C25B Si3 114.5(7) . . ?
C27B C25B H25B 107.0 . . ?
C25B C26B H26D 109.5 . . ?
C25B C26B H26E 109.5 . . ?
C25B C26B H26F 109.5 . . ?
H26D C26B H26E 109.5 . . ?
H26D C26B H26F 109.5 . . ?
H26E C26B H26F 109.5 . . ?
C25B C27B H27D 109.5 . . ?
C25B C27B H27E 109.5 . . ?
C25B C27B H27F 109.5 . . ?
H27D C27B H27E 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 109.5 . . ?
_shelx_res_file
;
TITL odpm74_a.res in Pbca
odpm74.res
created by SHELXL-2018/1 at 13:14:44 on 28-Mar-2018
REM Old TITL odpm74 in Pbca
REM SHELXT solution in Pbca
REM R1 0.154, Rweak 0.011, Alpha 0.069, Orientation as input
REM Formula found by SHELXT: C34 N2 Si4 Br Sm
CELL 0.71073 20.6319 20.1603 21.9662 90 90 90
ZERR 8 0.0009 0.0011 0.001 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Br N Si Sm
UNIT 288 672 8 16 32 8
SADI 0.008 C26B C25B C27B C25B C26A C25A C27A C25A C20 C19 C21 C19 C32 C31 =
C33 C31 C29 C28 C30 C28 C35 C34 C36 C34 C2 C1 C3 C1 C9 C7 C8 C7 C5 C4 C6 C4 =
C23 C22A C24A C22A C14 C13 C15 C13 C12 C10 C11 C10 C17 C16 C18 C16
SADI 0.008 Si3 C22A Si3 C22B Si3 C25A Si3 C25B Si3 C19 Si4 C31 Si4 C34 Si2 =
C10 SI2 C16 SI2 C13 SI1 C1 SI1 C7 SI1 C4 SI4 C28
SIMU 0.008 0.008 2 Si3 C19 > C23 C25A > C27B
RIGU 0.01 0.01
L.S. 10
PLAN 20
TEMP -123.14(1)
CONN 20 Sm1
FREE Sm1 Si1
FREE Sm1 Si3
BOND $H
list 4
bump 0.01
fmap 2
acta
SHEL 100 0.83
REM
REM
REM
WGHT 0.036100 3.797500
FVAR 0.56995 0.51811 0.29825
SM1 6 0.305319 0.342975 0.614868 11.00000 0.03437 0.04453 =
0.03458 0.00326 -0.00286 -0.00659
BR1 3 0.236373 0.258781 0.688536 11.00000 0.05020 0.06940 =
0.06112 0.01867 0.00881 -0.00611
SI1 5 0.279160 0.329930 0.462788 11.00000 0.03840 0.03104 =
0.03039 -0.00083 0.00229 0.00611
SI2 5 0.179329 0.419664 0.528667 11.00000 0.03038 0.03140 =
0.03886 -0.00069 0.00362 0.00375
SI3 5 0.385713 0.465713 0.688440 11.00000 0.04291 0.03669 =
0.05141 -0.00630 0.00049 -0.00207
SI4 5 0.462695 0.330855 0.669709 11.00000 0.03072 0.04138 =
0.03598 0.00277 -0.00029 -0.00141
N1 4 0.249085 0.370129 0.527313 11.00000 0.03022 0.02233 =
0.03305 -0.00262 0.00236 0.00131
N2 4 0.397594 0.385676 0.661451 11.00000 0.03146 0.03588 =
0.02970 0.00190 0.00054 -0.00181
C1 1 0.338339 0.266923 0.497386 11.00000 0.05156 0.03912 =
0.03334 -0.00578 -0.00177 0.01504
AFIX 13
H1 2 0.363912 0.292211 0.528320 11.00000 -1.20000
AFIX 0
C2 1 0.302684 0.212154 0.533429 11.00000 0.08342 0.03540 =
0.04371 0.00183 -0.01382 0.00689
AFIX 137
H2A 2 0.273324 0.232632 0.563039 11.00000 -1.50000
H2B 2 0.334446 0.184576 0.554872 11.00000 -1.50000
H2C 2 0.277665 0.184514 0.505239 11.00000 -1.50000
AFIX 0
C3 1 0.388950 0.234507 0.455179 11.00000 0.07058 0.06754 =
0.05757 -0.01279 0.00134 0.03872
AFIX 137
H3A 2 0.366726 0.209675 0.423003 11.00000 -1.50000
H3B 2 0.416209 0.204213 0.478883 11.00000 -1.50000
H3C 2 0.416086 0.269028 0.436822 11.00000 -1.50000
AFIX 0
C4 1 0.325975 0.387947 0.410502 11.00000 0.04333 0.04556 =
0.04831 0.01196 0.00973 0.00993
AFIX 13
H4 2 0.295882 0.425627 0.401691 11.00000 -1.20000
AFIX 0
C5 1 0.384372 0.418958 0.443478 11.00000 0.04905 0.06655 =
0.07365 0.00690 0.01943 -0.00612
AFIX 137
H5A 2 0.370450 0.436365 0.483027 11.00000 -1.50000
H5B 2 0.402048 0.455165 0.418768 11.00000 -1.50000
H5C 2 0.417814 0.385098 0.449641 11.00000 -1.50000
AFIX 0
C6 1 0.347563 0.361623 0.347916 11.00000 0.07190 0.08398 =
0.04625 0.01090 0.02499 0.01857
AFIX 137
H6A 2 0.378912 0.325624 0.353556 11.00000 -1.50000
H6B 2 0.367756 0.397595 0.324663 11.00000 -1.50000
H6C 2 0.309763 0.344893 0.325687 11.00000 -1.50000
AFIX 0
C7 1 0.215876 0.283154 0.415666 11.00000 0.05648 0.04454 =
0.03068 -0.00357 -0.00129 0.00104
AFIX 13
H7 2 0.182941 0.266490 0.445357 11.00000 -1.20000
AFIX 0
C8 1 0.178526 0.327389 0.370250 11.00000 0.06219 0.06424 =
0.04220 -0.00527 -0.01686 0.00307
AFIX 137
H8A 2 0.160919 0.366017 0.391697 11.00000 -1.50000
H8B 2 0.142937 0.301929 0.352165 11.00000 -1.50000
H8C 2 0.208017 0.342293 0.338062 11.00000 -1.50000
AFIX 0
C9 1 0.240025 0.221918 0.380712 11.00000 0.09667 0.04958 =
0.06117 -0.02055 -0.02290 0.00812
AFIX 137
H9A 2 0.274621 0.235068 0.352626 11.00000 -1.50000
H9B 2 0.204064 0.202545 0.357616 11.00000 -1.50000
H9C 2 0.256789 0.189092 0.409605 11.00000 -1.50000
AFIX 0
C10 1 0.176059 0.462995 0.606415 11.00000 0.03733 0.03758 =
0.04258 -0.00065 0.01158 0.00866
AFIX 13
H10 2 0.221964 0.473701 0.617225 11.00000 -1.20000
AFIX 0
C11 1 0.150008 0.419401 0.658688 11.00000 0.06360 0.06709 =
0.04905 -0.00201 0.01291 -0.00075
AFIX 137
H11A 2 0.103672 0.411120 0.652479 11.00000 -1.50000
H11B 2 0.156424 0.442302 0.697576 11.00000 -1.50000
H11C 2 0.173379 0.377085 0.659216 11.00000 -1.50000
AFIX 0
C12 1 0.139038 0.529238 0.608341 11.00000 0.08451 0.04799 =
0.07342 -0.01154 0.02117 0.00709
AFIX 137
H12A 2 0.158999 0.560579 0.579854 11.00000 -1.50000
H12B 2 0.140792 0.547512 0.649650 11.00000 -1.50000
H12C 2 0.093750 0.521804 0.596747 11.00000 -1.50000
AFIX 0
C13 1 0.185942 0.484946 0.466217 11.00000 0.05511 0.03329 =
0.05045 0.00807 0.00606 0.01537
AFIX 13
H13 2 0.196738 0.459853 0.428279 11.00000 -1.20000
AFIX 0
C14 1 0.243094 0.532742 0.476331 11.00000 0.06884 0.03792 =
0.07706 0.01538 0.02217 0.00194
AFIX 137
H14A 2 0.233747 0.561575 0.511160 11.00000 -1.50000
H14B 2 0.249379 0.559921 0.439816 11.00000 -1.50000
H14C 2 0.282549 0.507166 0.484457 11.00000 -1.50000
AFIX 0
C15 1 0.125066 0.525831 0.450584 11.00000 0.06819 0.07843 =
0.06537 0.02196 0.00499 0.03543
AFIX 137
H15A 2 0.090641 0.496054 0.436511 11.00000 -1.50000
H15B 2 0.135478 0.557744 0.418382 11.00000 -1.50000
H15C 2 0.110367 0.549696 0.486917 11.00000 -1.50000
AFIX 0
C16 1 0.102531 0.368110 0.517150 11.00000 0.03304 0.05770 =
0.04594 -0.00364 -0.00027 -0.00214
AFIX 13
H16 2 0.101139 0.356970 0.472808 11.00000 -1.20000
AFIX 0
C17 1 0.102867 0.301540 0.550922 11.00000 0.04440 0.05555 =
0.07663 -0.00450 0.00688 -0.01601
AFIX 137
H17A 2 0.144656 0.279466 0.544645 11.00000 -1.50000
H17B 2 0.067978 0.273361 0.535183 11.00000 -1.50000
H17C 2 0.096183 0.309249 0.594522 11.00000 -1.50000
AFIX 0
C18 1 0.038512 0.405005 0.530970 11.00000 0.03021 0.07135 =
0.09275 0.00165 -0.00059 0.00483
AFIX 137
H18A 2 0.036571 0.415831 0.574425 11.00000 -1.50000
H18B 2 0.001712 0.376590 0.520215 11.00000 -1.50000
H18C 2 0.036670 0.445981 0.507030 11.00000 -1.50000
AFIX 0
C19 1 0.303654 0.462829 0.728812 11.00000 0.05811 0.07042 =
0.06391 -0.02423 0.00462 0.00795
AFIX 13
H19 2 0.273571 0.445330 0.696935 11.00000 -1.20000
AFIX 0
C20 1 0.298244 0.411738 0.780469 11.00000 0.06295 0.09505 =
0.06058 -0.00953 0.01074 -0.01688
AFIX 137
H20A 2 0.315551 0.369049 0.766642 11.00000 -1.50000
H20B 2 0.252642 0.406409 0.791954 11.00000 -1.50000
H20C 2 0.323089 0.427168 0.815758 11.00000 -1.50000
AFIX 0
C21 1 0.271973 0.528090 0.748459 11.00000 0.12346 0.10884 =
0.12650 -0.03303 0.04233 0.03387
AFIX 137
H21A 2 0.278956 0.534885 0.792145 11.00000 -1.50000
H21B 2 0.225352 0.526236 0.740089 11.00000 -1.50000
H21C 2 0.291333 0.564919 0.725716 11.00000 -1.50000
AFIX 0
C23 1 0.430506 0.520788 0.576085 11.00000 0.08473 0.05884 =
0.10487 0.01332 0.01237 -0.00651
PART 2
AFIX 137
H23D 2 0.455035 0.560159 0.588491 -31.00000 -1.50000
H23E 2 0.418435 0.524742 0.533089 -31.00000 -1.50000
H23F 2 0.457317 0.481148 0.581804 -31.00000 -1.50000
AFIX 137
PART 0
PART 1
H23A 2 0.472057 0.534182 0.593866 31.00000 -1.50000
H23B 2 0.419941 0.550135 0.541932 31.00000 -1.50000
H23C 2 0.433588 0.474957 0.561498 31.00000 -1.50000
AFIX 0
PART 0
C28 1 0.429897 0.244151 0.650687 11.00000 0.04165 0.03422 =
0.04705 -0.00621 -0.01227 0.00748
AFIX 13
H28 2 0.393404 0.251627 0.621523 11.00000 -1.20000
AFIX 0
C29 1 0.399853 0.206625 0.705112 11.00000 0.05455 0.04868 =
0.07435 0.01400 -0.01170 -0.01111
AFIX 137
H29A 2 0.434444 0.191200 0.732213 11.00000 -1.50000
H29B 2 0.375163 0.168442 0.690126 11.00000 -1.50000
H29C 2 0.370891 0.236423 0.727528 11.00000 -1.50000
AFIX 0
C30 1 0.476548 0.195665 0.618128 11.00000 0.07616 0.04835 =
0.06862 -0.00711 -0.00206 0.01293
AFIX 137
H30A 2 0.494710 0.217173 0.581938 11.00000 -1.50000
H30B 2 0.452745 0.155749 0.605941 11.00000 -1.50000
H30C 2 0.511740 0.183358 0.645882 11.00000 -1.50000
AFIX 0
C31 1 0.502305 0.328920 0.748353 11.00000 0.03889 0.05598 =
0.04044 -0.00143 -0.00653 -0.00315
AFIX 13
H31 2 0.522062 0.373786 0.754056 11.00000 -1.20000
AFIX 0
C32 1 0.457929 0.318387 0.803636 11.00000 0.07071 0.09161 =
0.03965 0.00176 -0.01056 -0.00546
AFIX 137
H32A 2 0.416587 0.341141 0.796817 11.00000 -1.50000
H32B 2 0.478797 0.336462 0.840120 11.00000 -1.50000
H32C 2 0.450081 0.270837 0.809254 11.00000 -1.50000
AFIX 0
C33 1 0.559276 0.279302 0.751947 11.00000 0.05467 0.07340 =
0.05681 -0.00048 -0.01856 0.00801
AFIX 137
H33A 2 0.543736 0.234710 0.741825 11.00000 -1.50000
H33B 2 0.577141 0.279306 0.793285 11.00000 -1.50000
H33C 2 0.593077 0.292426 0.723009 11.00000 -1.50000
AFIX 0
C34 1 0.532491 0.343618 0.613905 11.00000 0.04301 0.07408 =
0.06775 0.00853 0.00663 -0.00242
AFIX 13
H34 2 0.558711 0.301994 0.616467 11.00000 -1.20000
AFIX 0
C35 1 0.580114 0.399501 0.628506 11.00000 0.05980 0.08879 =
0.12382 0.01704 0.01191 -0.02684
AFIX 137
H35A 2 0.560104 0.442328 0.618901 11.00000 -1.50000
H35B 2 0.619509 0.393894 0.604118 11.00000 -1.50000
H35C 2 0.591253 0.398102 0.671856 11.00000 -1.50000
AFIX 0
C36 1 0.510609 0.347779 0.547308 11.00000 0.07469 0.08954 =
0.06088 0.02129 0.02255 0.00261
AFIX 137
H36A 2 0.482035 0.310287 0.538030 11.00000 -1.50000
H36B 2 0.548641 0.346272 0.520617 11.00000 -1.50000
H36C 2 0.487163 0.389440 0.540710 11.00000 -1.50000
AFIX 0
PART 1
C25A 1 0.443803 0.497155 0.750167 21.00000 0.05890 0.05766 =
0.08167 -0.01760 -0.00389 -0.01161
AFIX 13
H25A 2 0.453911 0.457419 0.775708 21.00000 -1.20000
AFIX 0
C27A 1 0.509820 0.522121 0.727108 21.00000 0.06867 0.06973 =
0.09706 -0.01877 0.00000 -0.01812
AFIX 33
H27A 2 0.527639 0.490237 0.697885 21.00000 -1.50000
H27B 2 0.504240 0.565238 0.707183 21.00000 -1.50000
H27C 2 0.539650 0.526797 0.761560 21.00000 -1.50000
AFIX 0
C26A 1 0.420329 0.550384 0.795349 21.00000 0.07177 0.06835 =
0.08584 -0.02200 -0.00468 -0.01382
AFIX 33
H26A 2 0.378078 0.537432 0.811910 21.00000 -1.50000
H26B 2 0.451690 0.554577 0.828635 21.00000 -1.50000
H26C 2 0.416280 0.593018 0.774258 21.00000 -1.50000
AFIX 0
C22B 1 0.381561 0.525225 0.620564 31.00000 0.07237 0.04402 =
0.09503 0.00989 0.01398 0.00298
AFIX 13
H22B 2 0.339138 0.517601 0.599688 31.00000 -1.20000
AFIX 0
C24B 1 0.383983 0.606752 0.642059 31.00000 0.08391 0.04703 =
0.10383 0.00912 0.01312 0.00416
AFIX 137
H24A 2 0.342262 0.619297 0.660010 31.00000 -1.50000
H24B 2 0.392565 0.634530 0.606345 31.00000 -1.50000
H24C 2 0.418508 0.613130 0.672135 31.00000 -1.50000
AFIX 0
PART 0
PART 2
C22A 1 0.368963 0.515010 0.615064 -31.00000 0.06669 0.04273 =
0.09665 0.00914 0.01312 0.00142
AFIX 13
H22A 2 0.338489 0.486895 0.590829 -31.00000 -1.20000
AFIX 0
C24A 1 0.336597 0.583632 0.618906 -31.00000 0.08178 0.04846 =
0.11230 0.01581 0.01400 0.00784
AFIX 137
H24D 2 0.290398 0.578226 0.628009 -31.00000 -1.50000
H24E 2 0.341590 0.606710 0.579922 -31.00000 -1.50000
H24F 2 0.357187 0.609673 0.651236 -31.00000 -1.50000
AFIX 0
C25B 1 0.456444 0.505002 0.731300 -21.00000 0.05991 0.05782 =
0.08256 -0.01798 -0.00576 -0.01369
AFIX 13
H25B 2 0.497016 0.484442 0.715043 -21.00000 -1.20000
AFIX 0
C26B 1 0.453464 0.488463 0.799515 -21.00000 0.06586 0.06601 =
0.08215 -0.02262 -0.01042 -0.01124
AFIX 33
H26D 2 0.449320 0.440380 0.804782 -21.00000 -1.50000
H26E 2 0.493218 0.503847 0.819436 -21.00000 -1.50000
H26F 2 0.415953 0.510614 0.817840 -21.00000 -1.50000
AFIX 0
C27B 1 0.462962 0.580482 0.722524 -21.00000 0.07447 0.06514 =
0.09366 -0.01915 -0.00749 -0.02008
AFIX 33
H27D 2 0.464836 0.590693 0.678941 -21.00000 -1.50000
H27E 2 0.425466 0.602781 0.740725 -21.00000 -1.50000
H27F 2 0.502731 0.596014 0.742321 -21.00000 -1.50000
AFIX 0
HKLF 4
REM odpm74_a.res in Pbca
REM R1 = 0.0459 for 5518 Fo > 4sig(Fo) and 0.0857 for all 8310 data
REM 467 parameters refined using 914 restraints
END
WGHT 0.0361 3.8038
REM Highest difference peak 0.698, deepest hole -1.119, 1-sigma level 0.105
Q1 1 0.2648 0.5573 0.6960 11.00000 0.05 0.70
Q2 1 0.3049 0.1590 0.6587 11.00000 0.05 0.69
Q3 1 0.2472 0.2971 0.7032 11.00000 0.05 0.69
Q4 1 0.3081 0.5364 0.7720 11.00000 0.05 0.67
Q5 1 0.2885 0.3791 0.6291 11.00000 0.05 0.67
Q6 1 0.2724 0.3665 0.6209 11.00000 0.05 0.62
Q7 1 0.0812 0.3399 0.6148 11.00000 0.05 0.52
Q8 1 0.4257 0.6128 0.6470 11.00000 0.05 0.50
Q9 1 0.1962 0.4773 0.6133 11.00000 0.05 0.50
Q10 1 0.3003 0.2792 0.5896 11.00000 0.05 0.46
Q11 1 0.6020 0.3461 0.6193 11.00000 0.05 0.44
Q12 1 0.3119 0.5787 0.7445 11.00000 0.05 0.43
Q13 1 0.2250 0.2996 0.6603 11.00000 0.05 0.41
Q14 1 0.3621 0.5255 0.5726 11.00000 0.05 0.40
Q15 1 0.1749 0.4406 0.6230 11.00000 0.05 0.40
Q16 1 0.2763 0.2917 0.6529 11.00000 0.05 0.39
Q17 1 0.6023 0.4140 0.5808 11.00000 0.05 0.39
Q18 1 0.1789 0.4494 0.5717 11.00000 0.05 0.39
Q19 1 0.4853 0.4448 0.5491 11.00000 0.05 0.37
Q20 1 0.2936 0.2827 0.6431 11.00000 0.05 0.36
;
_shelx_res_checksum 44402
_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 1.877
_oxdiff_exptl_absorpt_empirical_full_min 0.475