# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
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data_rm422
_database_code_depnum_ccdc_archive 'CCDC 1589407'
_audit_update_record
;
2017-12-05 deposited with the CCDC.
2018-01-23 downloaded from the CCDC.
;
_audit_creation_date 2016-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number 2014-1
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C19 H27 Fe N Si'
_chemical_formula_sum 'C19 H27 Fe N Si'
_chemical_formula_weight 353.3549
_chemical_absolute_configuration ?
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
_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 45
_space_group_name_H-M_alt 'I b a 2'
_space_group_name_Hall 'I 2 -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, z+1/2'
'x, -y, z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1'
'x+1/2, -y+1/2, z+1'
_cell_length_a 13.6524(4)
_cell_length_b 27.8481(10)
_cell_length_c 8.8550(3)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3366.6(2)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 5900
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.91
_cell_measurement_theta_min 2.65
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.964
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.6687
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0582 before and 0.0470 after correction.
The Ratio of minimum to maximum transmission is 0.8969.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour 'clear reddish orange'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier reddish
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.394
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 1504
_exptl_crystal_size_max 0.552
_exptl_crystal_size_mid 0.304
_exptl_crystal_size_min 0.114
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0310
_diffrn_reflns_av_unetI/netI 0.0336
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 34
_diffrn_reflns_limit_k_min -36
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 14677
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.924
_diffrn_reflns_theta_min 1.462
_diffrn_ambient_temperature 100.03
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'sealed tube'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.735
_reflns_Friedel_fraction_full 0.858
_reflns_Friedel_fraction_max 0.841
_reflns_number_gt 3539
_reflns_number_total 3733
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.344
_refine_diff_density_min -0.195
_refine_diff_density_rms 0.049
_refine_ls_abs_structure_details
;
Flack x determined using 1423 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.018(10)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.046
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 207
_refine_ls_number_reflns 3733
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0276
_refine_ls_R_factor_gt 0.0250
_refine_ls_restrained_S_all 1.046
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.2274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0581
_refine_ls_wR_factor_ref 0.0592
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Others
Fixed Uiso: H2(0.02) H3(0.022) H4(0.021) H5(0.018) H7(0.017) H8(0.02)
H9(0.019) H10(0.017) H12A(0.018) H12B(0.018) H13A(0.019) H13B(0.019)
H14A(0.018) H14B(0.018) H16A(0.025) H16B(0.025) H16C(0.025) H17A(0.025)
H17B(0.025) H17C(0.025) H18A(0.022) H18B(0.022) H18C(0.022) H19A(0.022)
H19B(0.022) H19C(0.022)
Fixed X: H2(0.3225) H3(0.3431) H4(0.3713) H5(0.3672) H7(0.111) H8(0.0662)
H9(0.0855) H10(0.1408) H12A(0.4124) H12B(0.3525) H13A(0.2685) H13B(0.2636)
H14A(0.1735) H14B(0.1149) H16A(0.4418) H16B(0.4928) H16C(0.4118) H17A(0.3335)
H17B(0.4458) H17C(0.3741) H18A(0.0658) H18B(0.1782) H18C(0.1222) H19A(0.0997)
H19B(0.0209) H19C(0.0587)
Fixed Y: H2(0.2157) H3(0.2696) H4(0.2169) H5(0.13) H7(0.1986) H8(0.2477)
H9(0.195) H10(0.1129) H12A(0.0449) H12B(0.0111) H13A(0.0166) H13B(0.0741)
H14A(0.0075) H14B(0.0396) H16A(0.0962) H16B(0.0629) H16C(0.0408) H17A(0.1376)
H17B(0.1291) H17C(0.1568) H18A(0.1208) H18B(0.1352) H18C(0.151) H19A(0.034)
H19B(0.0524) H19C(0.0877)
Fixed Z: H2(0.1362) H3(0.3636) H4(0.5947) H5(0.5075) H7(0.1483) H8(0.3792)
H9(0.6103) H10(0.5229) H12A(-0.2179) H12B(-0.1046) H13A(-0.3365) H13B(-0.3211)
H14A(-0.1167) H14B(-0.236) H16A(0.1449) H16B(0.0204) H16C(0.1311) H17A(-
0.1976) H17B(-0.1526) H17C(-0.0392) H18A(-0.1765) H18B(-0.2005) H18C(-0.0497)
H19A(0.1137) H19B(-0.007) H19C(0.123)
;
_atom_sites_solution_hydrogens mixed
_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
Fe1 Fe 0.22888(2) 0.18874(2) 0.38977(5) 0.01117(9) Uani 1 1 d . . . . .
Si1 Si 0.25150(4) 0.10672(2) 0.22351(9) 0.00992(13) Uani 1 1 d . . . . .
H1 H 0.2704(19) 0.0694(11) 0.320(4) 0.023(8) Uiso 1 1 d . . . . .
N1 N 0.25351(14) 0.08546(7) 0.0402(2) 0.0105(4) Uani 1 1 d . . . . .
C1 C 0.33957(18) 0.15560(10) 0.2838(3) 0.0129(5) Uani 1 1 d . . . . .
C2 C 0.33311(18) 0.20506(10) 0.2369(3) 0.0170(5) Uani 1 1 d . . . . .
H2 H 0.3225 0.2157 0.1362 0.020 Uiso 1 1 calc R . . . .
C3 C 0.34517(17) 0.23552(9) 0.3646(3) 0.0186(6) Uani 1 1 d . . . . .
H3 H 0.3431 0.2696 0.3636 0.022 Uiso 1 1 calc R . . . .
C4 C 0.36092(19) 0.20612(10) 0.4942(3) 0.0179(6) Uani 1 1 d . . . . .
H4 H 0.3713 0.2169 0.5947 0.021 Uiso 1 1 calc R . . . .
C5 C 0.35815(18) 0.15725(10) 0.4445(3) 0.0149(6) Uani 1 1 d . . . . .
H5 H 0.3672 0.1300 0.5075 0.018 Uiso 1 1 calc R . . . .
C6 C 0.14032(19) 0.13955(10) 0.2971(3) 0.0112(5) Uani 1 1 d . . . . .
C7 C 0.1122(2) 0.18745(9) 0.2496(3) 0.0141(6) Uani 1 1 d . . . . .
H7 H 0.1110 0.1986 0.1483 0.017 Uiso 1 1 calc R . . . .
C8 C 0.08677(15) 0.21511(8) 0.3794(4) 0.0170(5) Uani 1 1 d . . . . .
H8 H 0.0662 0.2477 0.3792 0.020 Uiso 1 1 calc R . . . .
C9 C 0.0974(2) 0.18569(10) 0.5087(3) 0.0157(6) Uani 1 1 d . . . . .
H9 H 0.0855 0.1950 0.6103 0.019 Uiso 1 1 calc R . . . .
C10 C 0.12894(19) 0.13966(10) 0.4589(3) 0.0140(5) Uani 1 1 d . . . . .
H10 H 0.1408 0.1129 0.5229 0.017 Uiso 1 1 calc R . . . .
C11 C 0.35091(17) 0.08288(8) -0.0393(3) 0.0122(5) Uani 1 1 d . . . . .
C12 C 0.35155(17) 0.04245(9) -0.1576(3) 0.0151(5) Uani 1 1 d . . . . .
H12A H 0.4124 0.0449 -0.2179 0.018 Uiso 1 1 calc R . . . .
H12B H 0.3525 0.0111 -0.1046 0.018 Uiso 1 1 calc R . . . .
C13 C 0.26449(16) 0.04354(9) -0.2637(3) 0.0158(5) Uani 1 1 d . . . . .
H13A H 0.2685 0.0166 -0.3365 0.019 Uiso 1 1 calc R . . . .
H13B H 0.2636 0.0741 -0.3211 0.019 Uiso 1 1 calc R . . . .
C14 C 0.17265(19) 0.03907(9) -0.1684(3) 0.0152(5) Uani 1 1 d . . . . .
H14A H 0.1735 0.0075 -0.1167 0.018 Uiso 1 1 calc R . . . .
H14B H 0.1149 0.0396 -0.2360 0.018 Uiso 1 1 calc R . . . .
C15 C 0.16079(17) 0.07876(8) -0.0490(3) 0.0119(5) Uani 1 1 d . . . . .
C16 C 0.43167(16) 0.06949(9) 0.0746(3) 0.0169(5) Uani 1 1 d . . . . .
H16A H 0.4418 0.0962 0.1449 0.025 Uiso 1 1 calc GR . . . .
H16B H 0.4928 0.0629 0.0204 0.025 Uiso 1 1 calc GR . . . .
H16C H 0.4118 0.0408 0.1311 0.025 Uiso 1 1 calc GR . . . .
C17 C 0.37860(16) 0.13095(8) -0.1140(4) 0.0167(4) Uani 1 1 d . . . . .
H17A H 0.3335 0.1376 -0.1976 0.025 Uiso 1 1 calc GR . . . .
H17B H 0.4458 0.1291 -0.1526 0.025 Uiso 1 1 calc GR . . . .
H17C H 0.3741 0.1568 -0.0392 0.025 Uiso 1 1 calc GR . . . .
C18 C 0.12889(17) 0.12571(8) -0.1259(4) 0.0150(5) Uani 1 1 d . . . . .
H18A H 0.0658 0.1208 -0.1765 0.022 Uiso 1 1 calc GR . . . .
H18B H 0.1782 0.1352 -0.2005 0.022 Uiso 1 1 calc GR . . . .
H18C H 0.1222 0.1510 -0.0497 0.022 Uiso 1 1 calc GR . . . .
C19 C 0.07746(16) 0.06166(9) 0.0545(3) 0.0145(5) Uani 1 1 d . . . . .
H19A H 0.0997 0.0340 0.1137 0.022 Uiso 1 1 calc GR . . . .
H19B H 0.0209 0.0524 -0.0070 0.022 Uiso 1 1 calc GR . . . .
H19C H 0.0587 0.0877 0.1230 0.022 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
Fe1 0.01161(15) 0.01095(15) 0.01094(16) -0.00137(17) 0.00062(18) -0.00067(11)
Si1 0.0109(3) 0.0100(3) 0.0088(3) -0.0005(3) -0.0005(2) -0.0003(2)
N1 0.0098(9) 0.0116(10) 0.0101(10) -0.0009(8) -0.0003(8) -0.0001(7)
C1 0.0086(12) 0.0158(13) 0.0142(13) -0.0034(10) 0.0014(9) -0.0003(9)
C2 0.0163(12) 0.0178(13) 0.0169(14) -0.0017(12) 0.0040(11) -0.0054(10)
C3 0.0196(11) 0.0162(11) 0.0200(17) -0.0042(12) 0.0045(10) -0.0072(9)
C4 0.0137(12) 0.0225(14) 0.0174(14) -0.0071(12) 0.0005(10) -0.0052(11)
C5 0.0109(11) 0.0184(13) 0.0154(13) -0.0028(10) -0.0016(10) -0.0002(10)
C6 0.0102(12) 0.0118(13) 0.0117(12) -0.0028(10) 0.0012(10) -0.0021(10)
C7 0.0131(12) 0.0170(14) 0.0123(14) 0.0006(11) -0.0020(10) 0.0031(9)
C8 0.0145(10) 0.0181(11) 0.0185(13) -0.0020(14) -0.0007(13) 0.0045(8)
C9 0.0106(13) 0.0226(15) 0.0139(14) -0.0052(11) 0.0017(10) -0.0027(10)
C10 0.0119(12) 0.0158(14) 0.0144(13) 0.0009(11) 0.0007(10) -0.0028(10)
C11 0.0108(11) 0.0145(12) 0.0114(12) -0.0018(10) 0.0014(9) 0.0002(9)
C12 0.0140(12) 0.0180(12) 0.0132(12) -0.0033(10) 0.0013(9) 0.0020(9)
C13 0.0174(12) 0.0180(13) 0.0120(12) -0.0048(11) -0.0013(10) 0.0027(9)
C14 0.0141(12) 0.0162(12) 0.0152(12) -0.0042(10) -0.0017(9) 0.0003(10)
C15 0.0118(11) 0.0126(12) 0.0112(11) -0.0014(9) -0.0024(9) 0.0003(9)
C16 0.0121(12) 0.0224(13) 0.0162(13) -0.0043(11) -0.0006(10) 0.0021(10)
C17 0.0171(10) 0.0174(10) 0.0155(11) -0.0018(14) 0.0047(13) -0.0046(8)
C18 0.0173(11) 0.0146(11) 0.0132(13) -0.0008(12) -0.0021(11) 0.0017(8)
C19 0.0124(11) 0.0162(12) 0.0150(13) -0.0008(10) 0.0008(9) -0.0026(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 Si1 2.7349(8) . ?
Fe1 C1 2.004(3) . ?
Fe1 C2 2.016(3) . ?
Fe1 C3 2.066(2) . ?
Fe1 C4 2.083(3) . ?
Fe1 C5 2.029(3) . ?
Fe1 C6 2.003(3) . ?
Fe1 C7 2.019(3) . ?
Fe1 C8 2.077(2) . ?
Fe1 C9 2.083(3) . ?
Fe1 C10 2.026(3) . ?
Si1 N1 1.728(2) . ?
Si1 C1 1.893(3) . ?
Si1 C6 1.888(3) . ?
N1 C11 1.506(3) . ?
N1 C15 1.504(3) . ?
C1 C2 1.441(4) . ?
C1 C5 1.446(4) . ?
C2 C3 1.423(4) . ?
C3 C4 1.426(4) . ?
C4 C5 1.431(4) . ?
C6 C7 1.450(4) . ?
C6 C10 1.442(3) . ?
C7 C8 1.427(4) . ?
C8 C9 1.415(4) . ?
C9 C10 1.422(4) . ?
C11 C12 1.537(3) . ?
C11 C16 1.541(3) . ?
C11 C17 1.540(3) . ?
C12 C13 1.516(3) . ?
C13 C14 1.516(3) . ?
C14 C15 1.538(3) . ?
C15 C18 1.537(3) . ?
C15 C19 1.537(3) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 Si1 43.79(7) . . ?
C1 Fe1 C2 42.02(11) . . ?
C1 Fe1 C3 70.15(10) . . ?
C1 Fe1 C4 70.27(10) . . ?
C1 Fe1 C5 42.02(11) . . ?
C1 Fe1 C7 107.38(11) . . ?
C1 Fe1 C8 147.86(12) . . ?
C1 Fe1 C9 150.21(11) . . ?
C1 Fe1 C10 109.80(11) . . ?
C2 Fe1 Si1 75.35(8) . . ?
C2 Fe1 C3 40.79(10) . . ?
C2 Fe1 C4 68.60(12) . . ?
C2 Fe1 C5 69.14(11) . . ?
C2 Fe1 C7 98.51(12) . . ?
C2 Fe1 C8 123.37(12) . . ?
C2 Fe1 C9 163.13(11) . . ?
C2 Fe1 C10 146.14(11) . . ?
C3 Fe1 Si1 112.45(7) . . ?
C3 Fe1 C4 40.21(11) . . ?
C3 Fe1 C8 119.35(9) . . ?
C3 Fe1 C9 137.96(11) . . ?
C4 Fe1 Si1 109.60(8) . . ?
C4 Fe1 C9 122.07(12) . . ?
C5 Fe1 Si1 70.70(8) . . ?
C5 Fe1 C3 68.28(11) . . ?
C5 Fe1 C4 40.70(11) . . ?
C5 Fe1 C8 167.39(12) . . ?
C5 Fe1 C9 127.68(11) . . ?
C6 Fe1 Si1 43.65(8) . . ?
C6 Fe1 C1 87.03(11) . . ?
C6 Fe1 C2 107.76(11) . . ?
C6 Fe1 C3 148.31(11) . . ?
C6 Fe1 C4 149.68(11) . . ?
C6 Fe1 C5 109.10(11) . . ?
C6 Fe1 C7 42.26(11) . . ?
C6 Fe1 C8 70.11(10) . . ?
C6 Fe1 C9 70.06(11) . . ?
C6 Fe1 C10 41.93(9) . . ?
C7 Fe1 Si1 75.13(8) . . ?
C7 Fe1 C3 123.44(11) . . ?
C7 Fe1 C4 163.64(11) . . ?
C7 Fe1 C5 145.58(11) . . ?
C7 Fe1 C8 40.74(12) . . ?
C7 Fe1 C9 68.29(10) . . ?
C7 Fe1 C10 69.06(11) . . ?
C8 Fe1 Si1 112.16(8) . . ?
C8 Fe1 C4 138.24(11) . . ?
C8 Fe1 C9 39.77(12) . . ?
C9 Fe1 Si1 109.59(8) . . ?
C10 Fe1 Si1 71.05(8) . . ?
C10 Fe1 C3 167.33(11) . . ?
C10 Fe1 C4 127.26(11) . . ?
C10 Fe1 C5 102.83(11) . . ?
C10 Fe1 C8 67.83(10) . . ?
C10 Fe1 C9 40.47(11) . . ?
N1 Si1 Fe1 142.52(7) . . ?
N1 Si1 C1 120.07(11) . . ?
N1 Si1 C6 120.18(11) . . ?
C1 Si1 Fe1 47.11(8) . . ?
C6 Si1 Fe1 47.08(8) . . ?
C6 Si1 C1 93.74(12) . . ?
C11 N1 Si1 118.00(15) . . ?
C15 N1 Si1 121.50(15) . . ?
C15 N1 C11 119.46(19) . . ?
Si1 C1 Fe1 89.10(11) . . ?
C2 C1 Fe1 69.44(14) . . ?
C2 C1 Si1 124.55(19) . . ?
C2 C1 C5 105.3(2) . . ?
C5 C1 Fe1 69.93(16) . . ?
C5 C1 Si1 114.3(2) . . ?
C1 C2 Fe1 68.54(14) . . ?
C3 C2 Fe1 71.48(15) . . ?
C3 C2 C1 109.5(2) . . ?
C2 C3 Fe1 67.73(13) . . ?
C2 C3 C4 108.4(2) . . ?
C4 C3 Fe1 70.55(14) . . ?
C3 C4 Fe1 69.24(15) . . ?
C3 C4 C5 107.1(2) . . ?
C5 C4 Fe1 67.63(14) . . ?
C1 C5 Fe1 68.05(16) . . ?
C4 C5 Fe1 71.67(15) . . ?
C4 C5 C1 109.7(3) . . ?
Si1 C6 Fe1 89.27(11) . . ?
C7 C6 Fe1 69.47(15) . . ?
C7 C6 Si1 123.9(2) . . ?
C10 C6 Fe1 69.89(17) . . ?
C10 C6 Si1 115.5(2) . . ?
C10 C6 C7 104.9(3) . . ?
C6 C7 Fe1 68.27(15) . . ?
C8 C7 Fe1 71.79(15) . . ?
C8 C7 C6 109.1(2) . . ?
C7 C8 Fe1 67.47(14) . . ?
C9 C8 Fe1 70.37(15) . . ?
C9 C8 C7 108.30(19) . . ?
C8 C9 Fe1 69.86(15) . . ?
C8 C9 C10 107.6(3) . . ?
C10 C9 Fe1 67.60(15) . . ?
C6 C10 Fe1 68.19(18) . . ?
C9 C10 Fe1 71.93(16) . . ?
C9 C10 C6 110.0(3) . . ?
N1 C11 C12 110.99(19) . . ?
N1 C11 C16 109.69(19) . . ?
N1 C11 C17 112.07(19) . . ?
C12 C11 C16 105.36(19) . . ?
C12 C11 C17 110.1(2) . . ?
C17 C11 C16 108.4(2) . . ?
C13 C12 C11 113.8(2) . . ?
C12 C13 C14 107.6(2) . . ?
C13 C14 C15 114.2(2) . . ?
N1 C15 C14 111.20(19) . . ?
N1 C15 C18 111.45(19) . . ?
N1 C15 C19 110.39(19) . . ?
C18 C15 C14 109.7(2) . . ?
C19 C15 C14 105.39(19) . . ?
C19 C15 C18 108.54(19) . . ?
_shelx_res_file
;
TITL RM422 in Iba2 #45
REM reset to Iba2 #45
CELL 0.71073 13.6524 27.84812 8.855 90 90 90
ZERR 38 0.0004 0.00104 0.0003 0 0 0
LATT -2
SYMM -X,-Y,+Z
SYMM -X,+Y,0.5+Z
SYMM +X,-Y,0.5+Z
SFAC C H Fe N Si
UNIT 152 216 8 8 8
L.S. 10
PLAN 20
TEMP -173.12
BOND
fmap 2
acta
REM
REM
REM
WGHT 0.031100 0.227400
FVAR 0.06236
FE1 3 0.228884 0.188739 0.389772 11.00000 0.01161 0.01095 =
0.01094 -0.00137 0.00062 -0.00067
SI1 5 0.251501 0.106719 0.223515 11.00000 0.01089 0.01003 =
0.00884 -0.00050 -0.00047 -0.00028
H1 2 0.270434 0.069430 0.320433 11.00000 0.02284
N1 4 0.253514 0.085456 0.040172 11.00000 0.00976 0.01159 =
0.01012 -0.00092 -0.00030 -0.00010
C1 1 0.339566 0.155598 0.283772 11.00000 0.00861 0.01578 =
0.01422 -0.00339 0.00142 -0.00025
C2 1 0.333114 0.205060 0.236857 11.00000 0.01633 0.01780 =
0.01689 -0.00171 0.00400 -0.00537
AFIX 43
H2 2 0.322461 0.215685 0.136241 11.00000 -1.20000
AFIX 0
C3 1 0.345171 0.235522 0.364584 11.00000 0.01963 0.01615 =
0.02004 -0.00416 0.00447 -0.00724
AFIX 43
H3 2 0.343085 0.269619 0.363649 11.00000 -1.20000
AFIX 0
C4 1 0.360921 0.206120 0.494223 11.00000 0.01375 0.02254 =
0.01742 -0.00705 0.00047 -0.00521
AFIX 43
H4 2 0.371297 0.216947 0.594695 11.00000 -1.20000
AFIX 0
C5 1 0.358153 0.157251 0.444492 11.00000 0.01087 0.01841 =
0.01545 -0.00284 -0.00155 -0.00021
AFIX 43
H5 2 0.367164 0.130003 0.507528 11.00000 -1.20000
AFIX 0
C6 1 0.140324 0.139550 0.297067 11.00000 0.01017 0.01185 =
0.01171 -0.00281 0.00120 -0.00210
C7 1 0.112224 0.187450 0.249637 11.00000 0.01311 0.01702 =
0.01230 0.00056 -0.00198 0.00306
AFIX 43
H7 2 0.110967 0.198626 0.148292 11.00000 -1.20000
AFIX 0
C8 1 0.086766 0.215115 0.379440 11.00000 0.01449 0.01810 =
0.01855 -0.00201 -0.00069 0.00452
AFIX 43
H8 2 0.066221 0.247708 0.379150 11.00000 -1.20000
AFIX 0
C9 1 0.097360 0.185687 0.508689 11.00000 0.01062 0.02257 =
0.01395 -0.00520 0.00170 -0.00274
AFIX 43
H9 2 0.085524 0.194987 0.610284 11.00000 -1.20000
AFIX 0
C10 1 0.128944 0.139660 0.458918 11.00000 0.01187 0.01579 =
0.01442 0.00092 0.00065 -0.00277
AFIX 43
H10 2 0.140802 0.112912 0.522947 11.00000 -1.20000
AFIX 0
C11 1 0.350912 0.082878 -0.039347 11.00000 0.01083 0.01448 =
0.01141 -0.00179 0.00143 0.00016
C12 1 0.351546 0.042449 -0.157565 11.00000 0.01396 0.01804 =
0.01321 -0.00332 0.00126 0.00198
AFIX 23
H12A 2 0.412412 0.044859 -0.217864 11.00000 -1.20000
H12B 2 0.352547 0.011146 -0.104596 11.00000 -1.20000
AFIX 0
C13 1 0.264490 0.043539 -0.263728 11.00000 0.01743 0.01799 =
0.01205 -0.00479 -0.00132 0.00268
AFIX 23
H13A 2 0.268474 0.016614 -0.336471 11.00000 -1.20000
H13B 2 0.263565 0.074054 -0.321067 11.00000 -1.20000
AFIX 0
C14 1 0.172650 0.039069 -0.168430 11.00000 0.01408 0.01625 =
0.01515 -0.00422 -0.00174 0.00034
AFIX 23
H14A 2 0.173479 0.007547 -0.116750 11.00000 -1.20000
H14B 2 0.114908 0.039631 -0.236040 11.00000 -1.20000
AFIX 0
C15 1 0.160794 0.078760 -0.049009 11.00000 0.01179 0.01258 =
0.01119 -0.00142 -0.00237 0.00029
C16 1 0.431669 0.069490 0.074649 11.00000 0.01214 0.02236 =
0.01616 -0.00432 -0.00061 0.00207
AFIX 137
H16A 2 0.441794 0.096213 0.144943 11.00000 -1.50000
H16B 2 0.492777 0.062906 0.020400 11.00000 -1.50000
H16C 2 0.411804 0.040834 0.131117 11.00000 -1.50000
AFIX 0
C17 1 0.378596 0.130952 -0.114000 11.00000 0.01714 0.01743 =
0.01553 -0.00185 0.00474 -0.00462
AFIX 137
H17A 2 0.333544 0.137553 -0.197622 11.00000 -1.50000
H17B 2 0.445753 0.129085 -0.152639 11.00000 -1.50000
H17C 2 0.374105 0.156806 -0.039240 11.00000 -1.50000
AFIX 0
C18 1 0.128889 0.125712 -0.125879 11.00000 0.01727 0.01456 =
0.01316 -0.00076 -0.00205 0.00175
AFIX 137
H18A 2 0.065834 0.120827 -0.176488 11.00000 -1.50000
H18B 2 0.178249 0.135216 -0.200468 11.00000 -1.50000
H18C 2 0.122243 0.151028 -0.049692 11.00000 -1.50000
AFIX 0
C19 1 0.077462 0.061664 0.054516 11.00000 0.01243 0.01618 =
0.01501 -0.00079 0.00085 -0.00261
AFIX 137
H19A 2 0.099680 0.033985 0.113657 11.00000 -1.50000
H19B 2 0.020905 0.052367 -0.007046 11.00000 -1.50000
H19C 2 0.058658 0.087736 0.122960 11.00000 -1.50000
AFIX 0
HKLF 4
REM RM422 in Iba2 #45
REM R1 = 0.0250 for 3539 Fo > 4sig(Fo) and 0.0276 for all 3733 data
REM 207 parameters refined using 1 restraints
END
WGHT 0.0311 0.2274
REM Highest difference peak 0.344, deepest hole -0.195, 1-sigma level 0.049
Q1 1 0.2180 0.2205 0.3773 11.00000 0.05 0.34
Q2 1 0.2934 0.1893 0.3907 11.00000 0.05 0.28
Q3 1 0.1667 0.0596 -0.1097 11.00000 0.05 0.28
Q4 1 0.2293 0.1544 0.3925 11.00000 0.05 0.28
Q5 1 0.1424 0.0995 -0.0906 11.00000 0.05 0.27
Q6 1 0.1022 0.1616 0.4856 11.00000 0.05 0.26
Q7 1 0.2274 0.2114 0.3154 11.00000 0.05 0.26
Q8 1 0.2380 0.1602 0.4350 11.00000 0.05 0.25
Q9 1 0.3634 0.1812 0.4835 11.00000 0.05 0.25
Q10 1 0.3701 0.1044 -0.0932 11.00000 0.05 0.25
Q11 1 0.3506 0.0677 -0.1108 11.00000 0.05 0.25
Q12 1 0.1514 0.1982 0.3880 11.00000 0.05 0.25
Q13 1 0.0973 0.1999 0.4433 11.00000 0.05 0.24
Q14 1 0.1791 0.1141 0.2522 11.00000 0.05 0.24
Q15 1 0.3579 0.1795 0.2627 11.00000 0.05 0.23
Q16 1 0.2875 0.1342 0.2577 11.00000 0.05 0.23
Q17 1 0.1670 0.1264 0.2537 11.00000 0.05 0.23
Q18 1 0.2166 0.0411 -0.2208 11.00000 0.05 0.22
Q19 1 0.1238 0.1596 0.2708 11.00000 0.05 0.22
Q20 1 0.3002 0.0804 -0.0031 11.00000 0.05 0.22
;
_shelx_res_checksum 10092
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_testr1
_database_code_depnum_ccdc_archive 'CCDC 1589411'
_audit_update_record
;
2017-12-05 deposited with the CCDC.
2018-01-23 downloaded from the CCDC.
;
_audit_creation_date 2016-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number 2013-4
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C12 H18 Fe1 N6, B12 Cl12'
_chemical_formula_sum 'C12 H18 B12 Cl12 Fe N6'
_chemical_formula_weight 857.29
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
_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 trigonal
_space_group_IT_number 166
_space_group_name_H-M_alt 'R -3 m'
_space_group_name_Hall '-R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
_cell_length_a 11.3371(2)
_cell_length_b 11.3371(2)
_cell_length_c 23.9716(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 2668.28(10)
_cell_formula_units_Z 3
_cell_measurement_reflns_used 2377
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 26.63
_cell_measurement_theta_min 2.24
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.346
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.6468
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0508 before and 0.0403 after correction.
The Ratio of minimum to maximum transmission is 0.8675.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour orange
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.601
_exptl_crystal_density_meas .
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1266
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.21
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0390
_diffrn_reflns_av_unetI/netI 0.0175
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 7988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 27.574
_diffrn_reflns_theta_min 2.242
_diffrn_ambient_temperature 100(2)
_diffrn_detector 'Bruker area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type 'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 720
_reflns_number_total 800
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.27A (Bruker, 2012)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max 0.435
_refine_diff_density_min -0.453
_refine_diff_density_rms 0.061
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.143
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 46
_refine_ls_number_reflns 800
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0281
_refine_ls_R_factor_gt 0.0238
_refine_ls_restrained_S_all 1.143
_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^)+(0.0316P)^2^+2.7832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0616
_refine_ls_wR_factor_ref 0.0632
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.5 times of:
All C(H,H,H) groups
2. Others
Fixed Sof: H2A(0.5) H2B(0.5) H2C(0.5)
3.a Idealised Me refined as rotating group:
C2(H2A,H2B,H2C)
;
_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
Fe1 Fe 1.0000 1.0000 0.5000 0.0246(2) Uani 1 12 d S T P . .
N1 N 0.90790(11) 0.8158(2) 0.54815(9) 0.0288(5) Uani 1 2 d S T P . .
C1 C 0.85311(13) 0.7062(3) 0.56405(9) 0.0244(5) Uani 1 2 d S T P . .
C2 C 0.78456(13) 0.5691(3) 0.58435(10) 0.0282(5) Uani 1 2 d S T P . .
H2A H 0.7865 0.5097 0.5563 0.042 Uiso 0.5 1 calc GR . . A -1
H2B H 0.6918 0.5421 0.5930 0.042 Uiso 0.5 1 calc GR . . A -1
H2C H 0.8295 0.5636 0.6174 0.042 Uiso 0.5 1 calc GR . . A -1
Cl1 Cl 0.44139(3) 0.55861(3) 0.55104(2) 0.02124(15) Uani 1 2 d S T P . .
Cl2 Cl 0.68188(5) 0.84094(2) 0.63894(2) 0.02085(15) Uani 1 2 d S T P . .
B1 B 0.38591(12) 0.61409(12) 0.61044(9) 0.0147(4) Uani 1 2 d S T P . .
B2 B 0.5031(2) 0.75157(11) 0.65336(9) 0.0143(4) Uani 1 2 d S T P . .
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
Fe1 0.0202(3) 0.0202(3) 0.0333(5) 0.000 0.000 0.01012(14)
N1 0.0235(7) 0.0289(11) 0.0360(11) 0.0024(9) 0.0012(4) 0.0145(6)
C1 0.0181(8) 0.0335(13) 0.0268(11) -0.0012(10) -0.0006(5) 0.0168(7)
C2 0.0249(9) 0.0285(13) 0.0325(12) 0.0015(10) 0.0008(5) 0.0143(6)
Cl1 0.0267(2) 0.0267(2) 0.0142(2) -0.00325(9) 0.00325(9) 0.0162(2)
Cl2 0.0135(3) 0.0226(2) 0.0234(3) 0.00141(9) 0.00283(19) 0.00674(13)
B1 0.0168(8) 0.0168(8) 0.0111(9) -0.0016(4) 0.0016(4) 0.0088(9)
B2 0.0136(10) 0.0154(8) 0.0135(10) 0.0008(4) 0.0015(8) 0.0068(5)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 2.145(2) 20_566 ?
Fe1 N1 2.145(2) 2_765 ?
Fe1 N1 2.145(2) 21_656 ?
Fe1 N1 2.145(2) 3_675 ?
Fe1 N1 2.145(2) 19_776 ?
Fe1 N1 2.145(2) . ?
N1 C1 1.141(3) . ?
C1 C2 1.431(3) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
Cl1 B1 1.793(2) . ?
Cl2 B2 1.789(2) . ?
B1 B1 1.788(4) 3_565 ?
B1 B1 1.788(4) 2_665 ?
B1 B2 1.784(2) 3_565 ?
B1 B2 1.784(2) . ?
B1 B2 1.784(3) 26_456 ?
B2 B1 1.784(2) 2_665 ?
B2 B1 1.784(3) 27_556 ?
B2 B2 1.785(3) 26_456 ?
B2 B2 1.785(3) 27_556 ?
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 Fe1 N1 180.0 20_566 2_765 ?
N1 Fe1 N1 86.23(8) 21_656 . ?
N1 Fe1 N1 93.77(8) 21_656 19_776 ?
N1 Fe1 N1 93.77(8) 2_765 . ?
N1 Fe1 N1 93.77(8) 3_675 . ?
N1 Fe1 N1 93.77(8) 20_566 19_776 ?
N1 Fe1 N1 86.23(8) 20_566 . ?
N1 Fe1 N1 93.77(8) 2_765 3_675 ?
N1 Fe1 N1 180.00(9) 21_656 3_675 ?
N1 Fe1 N1 86.23(8) 2_765 21_656 ?
N1 Fe1 N1 180.0 19_776 . ?
N1 Fe1 N1 86.23(8) 2_765 19_776 ?
N1 Fe1 N1 86.23(8) 20_566 3_675 ?
N1 Fe1 N1 86.23(8) 3_675 19_776 ?
N1 Fe1 N1 93.77(8) 20_566 21_656 ?
C1 N1 Fe1 166.9(2) . . ?
N1 C1 C2 179.6(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
B1 B1 Cl1 121.75(6) 3_565 . ?
B1 B1 Cl1 121.75(6) 2_665 . ?
B1 B1 B1 60.000(1) 2_665 3_565 ?
B2 B1 Cl1 121.73(15) 26_456 . ?
B2 B1 Cl1 121.72(10) . . ?
B2 B1 Cl1 121.72(10) 3_565 . ?
B2 B1 B1 107.95(9) . 3_565 ?
B2 B1 B1 59.92(8) . 2_665 ?
B2 B1 B1 59.92(8) 3_565 3_565 ?
B2 B1 B1 107.95(9) 3_565 2_665 ?
B2 B1 B1 107.95(9) 26_456 3_565 ?
B2 B1 B1 107.95(9) 26_456 2_665 ?
B2 B1 B2 60.05(8) 26_456 . ?
B2 B1 B2 60.05(8) 26_456 3_565 ?
B2 B1 B2 108.06(18) . 3_565 ?
B1 B2 Cl2 121.44(12) . . ?
B1 B2 Cl2 121.99(15) 27_556 . ?
B1 B2 Cl2 121.44(12) 2_665 . ?
B1 B2 B1 108.02(14) 27_556 . ?
B1 B2 B1 108.01(14) 27_556 2_665 ?
B1 B2 B1 60.15(16) 2_665 . ?
B1 B2 B2 108.07(11) 2_665 26_456 ?
B1 B2 B2 59.98(12) 27_556 27_556 ?
B1 B2 B2 108.07(11) . 27_556 ?
B1 B2 B2 59.97(10) 2_665 27_556 ?
B1 B2 B2 59.98(12) 27_556 26_456 ?
B1 B2 B2 59.97(10) . 26_456 ?
B2 B2 Cl2 121.82(2) 27_556 . ?
B2 B2 Cl2 121.82(2) 26_456 . ?
B2 B2 B2 107.96(14) 26_456 27_556 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl1 B1 B2 Cl2 0.2(2) . . . . ?
Cl1 B1 B2 B1 -148.23(10) . . . 27_556 ?
Cl1 B1 B2 B1 110.91(13) . . . 2_665 ?
Cl1 B1 B2 B2 148.34(16) . . . 27_556 ?
Cl1 B1 B2 B2 -110.95(17) . . . 26_456 ?
B1 B1 B2 Cl2 -110.74(12) 2_665 . . . ?
B1 B1 B2 Cl2 -148.09(7) 3_565 . . . ?
B1 B1 B2 B1 -37.35(8) 3_565 . . 2_665 ?
B1 B1 B2 B1 63.51(9) 3_565 . . 27_556 ?
B1 B1 B2 B1 100.85(11) 2_665 . . 27_556 ?
B1 B1 B2 B2 37.42(12) 2_665 . . 27_556 ?
B1 B1 B2 B2 138.14(8) 2_665 . . 26_456 ?
B1 B1 B2 B2 0.07(16) 3_565 . . 27_556 ?
B1 B1 B2 B2 100.79(7) 3_565 . . 26_456 ?
B2 B1 B2 Cl2 148.56(9) 3_565 . . . ?
B2 B1 B2 Cl2 111.12(6) 26_456 . . . ?
B2 B1 B2 B1 -37.28(15) 26_456 . . 27_556 ?
B2 B1 B2 B1 -100.70(11) 3_565 . . 2_665 ?
B2 B1 B2 B1 -138.14(8) 26_456 . . 2_665 ?
B2 B1 B2 B1 0.15(19) 3_565 . . 27_556 ?
B2 B1 B2 B2 -100.72(19) 26_456 . . 27_556 ?
B2 B1 B2 B2 37.44(7) 3_565 . . 26_456 ?
B2 B1 B2 B2 -63.3(2) 3_565 . . 27_556 ?
_shelx_res_file
;
TITL
CELL 0.71073 11.3371 11.3371 23.9716 90 90 120
ZERR 3 0.0002 0.0002 0.0004 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SYMM +Y,+X,-Z
SFAC C H B Cl Fe N
UNIT 36 54 36 36 3 18
L.S. 4
PLAN 5
MORE -1
BOND $H
CONF
fmap 2 53
acta 52
REM
REM
REM
WGHT 0.031600 2.783200
FVAR 0.06403
FE1 5 1.000000 1.000000 0.500000 10.08333 0.02024 0.02024 =
0.03329 0.00000 0.00000 0.01012
N1 6 0.907903 0.815805 0.548155 10.50000 0.02346 0.02891 =
0.03597 0.00237 0.00119 0.01445
C1 1 0.853110 0.706220 0.564048 10.50000 0.01806 0.03354 =
0.02677 -0.00120 -0.00060 0.01677
C2 1 0.784564 0.569129 0.584349 10.50000 0.02487 0.02852 =
0.03246 0.00151 0.00075 0.01426
PART -1
AFIX 137
H2A 2 0.786463 0.509696 0.556284 10.50000 -1.50000
H2B 2 0.691765 0.542120 0.593013 10.50000 -1.50000
H2C 2 0.829489 0.563619 0.617368 10.50000 -1.50000
AFIX 0
PART 0
CL1 4 0.441387 0.558613 0.551037 10.50000 0.02667 0.02667 =
0.01419 -0.00325 0.00325 0.01620
CL2 4 0.681884 0.840942 0.638940 10.50000 0.01348 0.02262 =
0.02341 0.00141 0.00283 0.00674
B1 3 0.385909 0.614091 0.610438 10.50000 0.01682 0.01682 =
0.01111 -0.00155 0.00155 0.00881
B2 3 0.503144 0.751572 0.653357 10.50000 0.01359 0.01536 =
0.01351 0.00077 0.00155 0.00679
HKLF 4
REM
REM R1 = 0.0238 for 720 Fo > 4sig(Fo) and 0.0281 for all 800 data
REM 46 parameters refined using 0 restraints
END
WGHT 0.0316 2.7832
REM Highest difference peak 0.435, deepest hole -0.453, 1-sigma level 0.061
Q1 1 0.8121 0.6241 0.5608 10.50000 0.05 0.43
Q2 1 1.0181 1.0362 0.4579 10.50000 0.05 0.39
Q3 1 0.4191 0.5809 0.5816 10.50000 0.05 0.31
Q4 1 0.8540 0.7081 0.5423 10.50000 0.05 0.29
Q5 1 0.4836 0.7732 0.6867 11.00000 0.05 0.25
;
_shelx_res_checksum 39663
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_test
_database_code_depnum_ccdc_archive 'CCDC 1589409'
_audit_update_record
;
2017-12-05 deposited with the CCDC.
2018-01-23 downloaded from the CCDC.
;
_audit_creation_date 2016-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number 2013-4
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C15 H23 Au Cl Fe P Si'
_chemical_formula_sum 'C15 H23 Au Cl Fe P Si'
_chemical_formula_weight 550.66
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
_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 7.473(5)
_cell_length_b 9.660(7)
_cell_length_c 12.930(9)
_cell_angle_alpha 76.909(16)
_cell_angle_beta 81.91(2)
_cell_angle_gamma 80.681(14)
_cell_volume 891.9(11)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9942
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 29.48
_cell_measurement_theta_min 2.44
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 9.323
_exptl_absorpt_correction_T_max 0.7459
_exptl_absorpt_correction_T_min 0.5558
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0950 before and 0.0380 after correction.
The Ratio of minimum to maximum transmission is 0.7451.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour orange
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 2.050
_exptl_crystal_density_meas .
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 528
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.07
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0281
_diffrn_reflns_av_unetI/netI 0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 29657
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.495
_diffrn_reflns_theta_min 2.184
_diffrn_ambient_temperature 100(2)
_diffrn_detector 'Bruker area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device 'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type 'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4632
_reflns_number_total 4960
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 1.024
_refine_diff_density_min -0.459
_refine_diff_density_rms 0.107
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 186
_refine_ls_number_reflns 4960
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0185
_refine_ls_R_factor_gt 0.0154
_refine_ls_restrained_S_all 1.062
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+0.2283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0330
_refine_ls_wR_factor_ref 0.0338
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10)
2.b Idealised Me refined as rotating group:
C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
H14C), C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.68602(2) -0.02372(2) 0.17658(2) 0.01280(3) Uani 1 1 d . . . . .
Fe1 Fe 0.46038(4) 0.32869(3) 0.20776(2) 0.01003(6) Uani 1 1 d . . . . .
Cl1 Cl 0.85619(8) 0.35445(6) 0.49800(4) 0.02012(11) Uani 1 1 d . . . . .
P1 P 0.94942(8) -0.18005(6) 0.17199(4) 0.01340(11) Uani 1 1 d . . . . .
Si1 Si 0.67332(8) 0.26087(6) 0.43444(5) 0.01376(12) Uani 1 1 d . . . . .
C1 C 0.4562(3) 0.1195(2) 0.18910(17) 0.0136(4) Uani 1 1 d . . . . .
C2 C 0.3710(3) 0.2245(2) 0.10686(17) 0.0148(4) Uani 1 1 d . . . . .
H2 H 0.4077 0.2347 0.0324 0.018 Uiso 1 1 calc R . . . .
C3 C 0.2233(3) 0.3113(2) 0.15363(18) 0.0161(4) Uani 1 1 d . . . . .
H3 H 0.1457 0.3886 0.1162 0.019 Uiso 1 1 calc R . . . .
C4 C 0.2125(3) 0.2622(2) 0.26564(18) 0.0159(4) Uani 1 1 d . . . . .
H4 H 0.1261 0.2999 0.3170 0.019 Uiso 1 1 calc R . . . .
C5 C 0.3550(3) 0.1457(2) 0.28755(17) 0.0144(4) Uani 1 1 d . . . . .
H5 H 0.3794 0.0932 0.3568 0.017 Uiso 1 1 calc R . . . .
C6 C 0.6322(3) 0.3732(2) 0.30308(16) 0.0121(4) Uani 1 1 d . . . . .
C7 C 0.7283(3) 0.3530(2) 0.20144(16) 0.0122(4) Uani 1 1 d . . . . .
H7 H 0.8301 0.2827 0.1914 0.015 Uiso 1 1 calc R . . . .
C8 C 0.6448(3) 0.4562(2) 0.11887(17) 0.0137(4) Uani 1 1 d . . . . .
H8 H 0.6808 0.4662 0.0444 0.016 Uiso 1 1 calc R . . . .
C9 C 0.4982(3) 0.5415(2) 0.16732(17) 0.0145(4) Uani 1 1 d . . . . .
H9 H 0.4199 0.6191 0.1308 0.017 Uiso 1 1 calc R . . . .
C10 C 0.4887(3) 0.4910(2) 0.27948(16) 0.0134(4) Uani 1 1 d . . . . .
H10 H 0.4021 0.5286 0.3307 0.016 Uiso 1 1 calc R . . . .
C11 C 1.1386(3) -0.1160(3) 0.2115(2) 0.0229(5) Uani 1 1 d . . . . .
H11A H 1.1635 -0.0262 0.1623 0.034 Uiso 1 1 calc GR . . . .
H11B H 1.2470 -0.1880 0.2092 0.034 Uiso 1 1 calc GR . . . .
H11C H 1.1079 -0.0992 0.2842 0.034 Uiso 1 1 calc GR . . . .
C12 C 0.9370(3) -0.3540(2) 0.25926(19) 0.0218(5) Uani 1 1 d . . . . .
H12A H 0.8971 -0.3419 0.3326 0.033 Uiso 1 1 calc GR . . . .
H12B H 1.0576 -0.4115 0.2567 0.033 Uiso 1 1 calc GR . . . .
H12C H 0.8496 -0.4027 0.2358 0.033 Uiso 1 1 calc GR . . . .
C13 C 1.0344(3) -0.2218(3) 0.04284(18) 0.0269(6) Uani 1 1 d . . . . .
H13A H 1.1386 -0.2980 0.0506 0.040 Uiso 1 1 calc GR . . . .
H13B H 1.0729 -0.1359 -0.0061 0.040 Uiso 1 1 calc GR . . . .
H13C H 0.9376 -0.2543 0.0141 0.040 Uiso 1 1 calc GR . . . .
C14 C 0.4640(3) 0.2619(3) 0.53068(17) 0.0201(5) Uani 1 1 d . . . . .
H14A H 0.3702 0.2231 0.5042 0.030 Uiso 1 1 calc GR . . . .
H14B H 0.4190 0.3605 0.5385 0.030 Uiso 1 1 calc GR . . . .
H14C H 0.4923 0.2027 0.6001 0.030 Uiso 1 1 calc GR . . . .
C15 C 0.7928(3) 0.0807(2) 0.42254(18) 0.0197(5) Uani 1 1 d . . . . .
H15A H 0.9069 0.0905 0.3755 0.030 Uiso 1 1 calc GR . . . .
H15B H 0.7149 0.0310 0.3925 0.030 Uiso 1 1 calc GR . . . .
H15C H 0.8198 0.0253 0.4933 0.030 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
Au1 0.01120(4) 0.01143(4) 0.01633(4) -0.00484(3) -0.00112(3) -0.00066(3)
Fe1 0.00798(13) 0.01095(14) 0.01184(13) -0.00365(11) -0.00068(10) -0.00176(11)
Cl1 0.0209(3) 0.0258(3) 0.0166(2) -0.0066(2) -0.0049(2) -0.0062(2)
P1 0.0120(3) 0.0126(3) 0.0164(3) -0.0050(2) -0.0021(2) -0.0008(2)
Si1 0.0147(3) 0.0150(3) 0.0118(3) -0.0023(2) -0.0012(2) -0.0033(2)
C1 0.0112(10) 0.0142(10) 0.0168(10) -0.0061(8) 0.0007(8) -0.0035(8)
C2 0.0127(10) 0.0161(11) 0.0176(10) -0.0060(8) -0.0023(8) -0.0037(8)
C3 0.0096(10) 0.0173(11) 0.0236(11) -0.0064(9) -0.0049(8) -0.0020(8)
C4 0.0094(10) 0.0170(11) 0.0221(11) -0.0065(9) 0.0022(8) -0.0040(8)
C5 0.0125(10) 0.0145(10) 0.0167(10) -0.0030(8) 0.0009(8) -0.0060(8)
C6 0.0119(10) 0.0118(10) 0.0139(9) -0.0030(8) -0.0021(7) -0.0042(8)
C7 0.0099(9) 0.0120(10) 0.0157(9) -0.0034(8) -0.0010(7) -0.0038(8)
C8 0.0132(10) 0.0144(10) 0.0139(9) -0.0025(8) -0.0009(8) -0.0042(8)
C9 0.0143(10) 0.0111(10) 0.0180(10) -0.0020(8) -0.0034(8) -0.0020(8)
C10 0.0125(10) 0.0139(10) 0.0152(9) -0.0060(8) 0.0005(8) -0.0037(8)
C11 0.0163(11) 0.0202(12) 0.0364(13) -0.0115(10) -0.0067(10) -0.0036(9)
C12 0.0225(12) 0.0145(11) 0.0284(12) -0.0018(9) -0.0043(10) -0.0051(9)
C13 0.0242(13) 0.0374(15) 0.0183(11) -0.0118(11) -0.0024(9) 0.0074(11)
C14 0.0216(12) 0.0236(12) 0.0149(10) -0.0043(9) 0.0034(9) -0.0067(9)
C15 0.0226(12) 0.0161(11) 0.0190(10) -0.0010(9) -0.0036(9) -0.0011(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 P1 2.2812(13) . ?
Au1 C1 2.035(2) . ?
Fe1 C1 2.095(3) . ?
Fe1 C2 2.054(2) . ?
Fe1 C3 2.039(2) . ?
Fe1 C4 2.045(2) . ?
Fe1 C5 2.051(2) . ?
Fe1 C6 2.054(2) . ?
Fe1 C7 2.042(2) . ?
Fe1 C8 2.049(2) . ?
Fe1 C9 2.059(3) . ?
Fe1 C10 2.045(2) . ?
Cl1 Si1 2.1008(12) . ?
P1 C11 1.809(2) . ?
P1 C12 1.807(3) . ?
P1 C13 1.811(3) . ?
Si1 C6 1.833(2) . ?
Si1 C14 1.857(2) . ?
Si1 C15 1.852(3) . ?
C1 C2 1.435(3) . ?
C1 C5 1.439(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.425(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.413(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.426(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.444(3) . ?
C6 C10 1.441(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.423(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.422(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.417(3) . ?
C10 H10 0.9500 . ?
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 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 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
C1 Au1 P1 176.22(6) . . ?
C2 Fe1 C1 40.45(9) . . ?
C2 Fe1 C9 123.51(9) . . ?
C3 Fe1 C1 68.91(9) . . ?
C3 Fe1 C2 40.75(8) . . ?
C3 Fe1 C4 40.50(9) . . ?
C3 Fe1 C5 68.10(9) . . ?
C3 Fe1 C6 159.33(8) . . ?
C3 Fe1 C7 158.13(9) . . ?
C3 Fe1 C8 122.35(10) . . ?
C3 Fe1 C9 107.75(9) . . ?
C3 Fe1 C10 123.12(9) . . ?
C4 Fe1 C1 68.97(9) . . ?
C4 Fe1 C2 68.09(9) . . ?
C4 Fe1 C5 40.75(9) . . ?
C4 Fe1 C6 123.01(9) . . ?
C4 Fe1 C8 158.40(9) . . ?
C4 Fe1 C9 122.95(9) . . ?
C4 Fe1 C10 107.91(9) . . ?
C5 Fe1 C1 40.60(8) . . ?
C5 Fe1 C2 67.48(10) . . ?
C5 Fe1 C6 107.48(9) . . ?
C5 Fe1 C9 159.32(8) . . ?
C6 Fe1 C1 121.78(9) . . ?
C6 Fe1 C2 158.10(9) . . ?
C6 Fe1 C9 68.84(9) . . ?
C7 Fe1 C1 106.54(8) . . ?
C7 Fe1 C2 122.12(9) . . ?
C7 Fe1 C4 159.71(9) . . ?
C7 Fe1 C5 123.20(9) . . ?
C7 Fe1 C6 41.30(8) . . ?
C7 Fe1 C8 40.72(8) . . ?
C7 Fe1 C9 68.33(9) . . ?
C7 Fe1 C10 68.76(8) . . ?
C8 Fe1 C1 122.32(9) . . ?
C8 Fe1 C2 107.49(10) . . ?
C8 Fe1 C5 159.03(9) . . ?
C8 Fe1 C6 69.15(9) . . ?
C8 Fe1 C9 40.49(8) . . ?
C9 Fe1 C1 158.80(8) . . ?
C10 Fe1 C1 158.91(9) . . ?
C10 Fe1 C2 159.45(9) . . ?
C10 Fe1 C5 123.56(10) . . ?
C10 Fe1 C6 41.17(8) . . ?
C10 Fe1 C8 68.37(9) . . ?
C10 Fe1 C9 40.39(9) . . ?
C11 P1 Au1 113.07(9) . . ?
C11 P1 C13 104.14(13) . . ?
C12 P1 Au1 114.73(9) . . ?
C12 P1 C11 104.28(12) . . ?
C12 P1 C13 103.74(13) . . ?
C13 P1 Au1 115.58(9) . . ?
C6 Si1 Cl1 107.34(8) . . ?
C6 Si1 C14 112.01(11) . . ?
C6 Si1 C15 111.30(10) . . ?
C14 Si1 Cl1 105.13(9) . . ?
C15 Si1 Cl1 105.14(9) . . ?
C15 Si1 C14 115.19(11) . . ?
Au1 C1 Fe1 122.94(11) . . ?
C2 C1 Au1 129.22(15) . . ?
C2 C1 Fe1 68.24(12) . . ?
C2 C1 C5 105.02(19) . . ?
C5 C1 Au1 125.46(16) . . ?
C5 C1 Fe1 68.06(12) . . ?
Fe1 C2 H2 126.1 . . ?
C1 C2 Fe1 71.31(13) . . ?
C1 C2 H2 125.1 . . ?
C3 C2 Fe1 69.06(13) . . ?
C3 C2 C1 109.76(19) . . ?
C3 C2 H2 125.1 . . ?
Fe1 C3 H3 125.4 . . ?
C2 C3 Fe1 70.19(13) . . ?
C2 C3 H3 126.1 . . ?
C4 C3 Fe1 69.98(13) . . ?
C4 C3 C2 107.9(2) . . ?
C4 C3 H3 126.1 . . ?
Fe1 C4 H4 126.0 . . ?
C3 C4 Fe1 69.52(12) . . ?
C3 C4 H4 126.2 . . ?
C3 C4 C5 107.50(19) . . ?
C5 C4 Fe1 69.85(13) . . ?
C5 C4 H4 126.2 . . ?
Fe1 C5 H5 125.8 . . ?
C1 C5 Fe1 71.34(13) . . ?
C1 C5 H5 125.1 . . ?
C4 C5 Fe1 69.40(13) . . ?
C4 C5 C1 109.84(19) . . ?
C4 C5 H5 125.1 . . ?
Si1 C6 Fe1 122.81(11) . . ?
C7 C6 Fe1 68.90(12) . . ?
C7 C6 Si1 126.47(16) . . ?
C10 C6 Fe1 69.11(12) . . ?
C10 C6 Si1 127.11(15) . . ?
C10 C6 C7 106.23(18) . . ?
Fe1 C7 H7 126.1 . . ?
C6 C7 Fe1 69.80(12) . . ?
C6 C7 H7 125.7 . . ?
C8 C7 Fe1 69.93(12) . . ?
C8 C7 C6 108.57(19) . . ?
C8 C7 H7 125.7 . . ?
Fe1 C8 H8 126.1 . . ?
C7 C8 Fe1 69.35(12) . . ?
C7 C8 H8 126.0 . . ?
C9 C8 Fe1 70.12(13) . . ?
C9 C8 C7 108.08(19) . . ?
C9 C8 H8 126.0 . . ?
Fe1 C9 H9 127.0 . . ?
C8 C9 Fe1 69.39(13) . . ?
C8 C9 H9 125.9 . . ?
C10 C9 Fe1 69.29(12) . . ?
C10 C9 C8 108.28(19) . . ?
C10 C9 H9 125.9 . . ?
Fe1 C10 H10 126.0 . . ?
C6 C10 Fe1 69.72(12) . . ?
C6 C10 H10 125.6 . . ?
C9 C10 Fe1 70.32(13) . . ?
C9 C10 C6 108.84(18) . . ?
C9 C10 H10 125.6 . . ?
P1 C11 H11A 109.5 . . ?
P1 C11 H11B 109.5 . . ?
P1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
P1 C12 H12A 109.5 . . ?
P1 C12 H12B 109.5 . . ?
P1 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
P1 C13 H13A 109.5 . . ?
P1 C13 H13B 109.5 . . ?
P1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Au1 C1 C2 Fe1 -115.46(17) . . . . ?
Au1 C1 C2 C3 -173.96(15) . . . . ?
Au1 C1 C5 Fe1 115.64(16) . . . . ?
Au1 C1 C5 C4 174.54(15) . . . . ?
Fe1 C1 C2 C3 -58.50(15) . . . . ?
Fe1 C1 C5 C4 58.90(15) . . . . ?
Fe1 C2 C3 C4 -60.09(15) . . . . ?
Fe1 C3 C4 C5 -59.78(15) . . . . ?
Fe1 C4 C5 C1 -60.07(15) . . . . ?
Fe1 C6 C7 C8 59.38(15) . . . . ?
Fe1 C6 C10 C9 -59.65(15) . . . . ?
Fe1 C7 C8 C9 59.65(15) . . . . ?
Fe1 C8 C9 C10 58.52(15) . . . . ?
Fe1 C9 C10 C6 59.27(15) . . . . ?
Cl1 Si1 C6 Fe1 -179.50(9) . . . . ?
Cl1 Si1 C6 C7 93.71(19) . . . . ?
Cl1 Si1 C6 C10 -92.03(19) . . . . ?
Si1 C6 C7 Fe1 115.92(17) . . . . ?
Si1 C6 C7 C8 175.30(15) . . . . ?
Si1 C6 C10 Fe1 -116.01(17) . . . . ?
Si1 C6 C10 C9 -175.66(16) . . . . ?
C1 C2 C3 Fe1 59.86(16) . . . . ?
C1 C2 C3 C4 -0.2(2) . . . . ?
C2 C1 C5 Fe1 -58.54(15) . . . . ?
C2 C1 C5 C4 0.4(2) . . . . ?
C2 C3 C4 Fe1 60.22(15) . . . . ?
C2 C3 C4 C5 0.4(2) . . . . ?
C3 C4 C5 Fe1 59.57(15) . . . . ?
C3 C4 C5 C1 -0.5(2) . . . . ?
C5 C1 C2 Fe1 58.43(14) . . . . ?
C5 C1 C2 C3 -0.1(2) . . . . ?
C6 C7 C8 Fe1 -59.30(14) . . . . ?
C6 C7 C8 C9 0.4(2) . . . . ?
C7 C6 C10 Fe1 59.18(14) . . . . ?
C7 C6 C10 C9 -0.5(2) . . . . ?
C7 C8 C9 Fe1 -59.16(15) . . . . ?
C7 C8 C9 C10 -0.6(2) . . . . ?
C8 C9 C10 Fe1 -58.58(15) . . . . ?
C8 C9 C10 C6 0.7(2) . . . . ?
C10 C6 C7 Fe1 -59.31(14) . . . . ?
C10 C6 C7 C8 0.1(2) . . . . ?
C14 Si1 C6 Fe1 -64.59(16) . . . . ?
C14 Si1 C6 C7 -151.38(18) . . . . ?
C14 Si1 C6 C10 22.9(2) . . . . ?
C15 Si1 C6 Fe1 65.96(16) . . . . ?
C15 Si1 C6 C7 -20.8(2) . . . . ?
C15 Si1 C6 C10 153.43(18) . . . . ?
_shelx_res_file
;
TITL RM076 in P1 New: P-1
CELL 0.71073 7.473 9.66 12.93 76.909 81.91 80.681
ZERR 2 0.005 0.007 0.009 0.016 0.02 0.014
LATT 1
SFAC C H Au Cl Fe P Si
UNIT 30 46 2 2 2 2 2
L.S. 4
PLAN -5
TEMP -173(2)
BOND $H
CONF
fmap 2
acta
MORE -1
OMIT 0 0 1
REM
REM
REM
WGHT 0.016100 0.228300
FVAR 0.12175
AU1 3 0.686020 -0.023719 0.176579 11.00000 0.01120 0.01143 =
0.01633 -0.00484 -0.00112 -0.00066
FE1 5 0.460380 0.328688 0.207762 11.00000 0.00798 0.01095 =
0.01184 -0.00365 -0.00068 -0.00176
CL1 4 0.856192 0.354455 0.498004 11.00000 0.02095 0.02581 =
0.01658 -0.00662 -0.00494 -0.00623
P1 6 0.949419 -0.180054 0.171987 11.00000 0.01199 0.01264 =
0.01642 -0.00502 -0.00208 -0.00085
SI1 7 0.673321 0.260873 0.434435 11.00000 0.01469 0.01497 =
0.01175 -0.00231 -0.00119 -0.00329
C1 1 0.456202 0.119467 0.189104 11.00000 0.01122 0.01424 =
0.01678 -0.00609 0.00069 -0.00353
C2 1 0.371042 0.224530 0.106862 11.00000 0.01268 0.01613 =
0.01762 -0.00596 -0.00235 -0.00373
AFIX 43
H2 2 0.407659 0.234690 0.032431 11.00000 -1.20000
AFIX 0
C3 1 0.223267 0.311344 0.153633 11.00000 0.00956 0.01731 =
0.02356 -0.00636 -0.00489 -0.00200
AFIX 43
H3 2 0.145705 0.388572 0.116164 11.00000 -1.20000
AFIX 0
C4 1 0.212526 0.262201 0.265644 11.00000 0.00936 0.01705 =
0.02211 -0.00654 0.00222 -0.00397
AFIX 43
H4 2 0.126147 0.299910 0.316965 11.00000 -1.20000
AFIX 0
C5 1 0.354997 0.145703 0.287550 11.00000 0.01252 0.01450 =
0.01670 -0.00303 0.00085 -0.00596
AFIX 43
H5 2 0.379443 0.093245 0.356803 11.00000 -1.20000
AFIX 0
C6 1 0.632229 0.373185 0.303083 11.00000 0.01185 0.01181 =
0.01387 -0.00298 -0.00212 -0.00417
C7 1 0.728287 0.353033 0.201441 11.00000 0.00993 0.01196 =
0.01575 -0.00341 -0.00103 -0.00375
AFIX 43
H7 2 0.830140 0.282710 0.191369 11.00000 -1.20000
AFIX 0
C8 1 0.644800 0.456183 0.118875 11.00000 0.01323 0.01444 =
0.01387 -0.00249 -0.00085 -0.00421
AFIX 43
H8 2 0.680791 0.466241 0.044390 11.00000 -1.20000
AFIX 0
C9 1 0.498158 0.541532 0.167323 11.00000 0.01435 0.01111 =
0.01803 -0.00197 -0.00336 -0.00199
AFIX 43
H9 2 0.419911 0.619136 0.130780 11.00000 -1.20000
AFIX 0
C10 1 0.488744 0.490975 0.279475 11.00000 0.01246 0.01387 =
0.01524 -0.00601 0.00052 -0.00372
AFIX 43
H10 2 0.402051 0.528565 0.330715 11.00000 -1.20000
AFIX 0
C11 1 1.138649 -0.116014 0.211450 11.00000 0.01627 0.02023 =
0.03642 -0.01150 -0.00673 -0.00362
AFIX 137
H11A 2 1.163541 -0.026201 0.162302 11.00000 -1.50000
H11B 2 1.247048 -0.187978 0.209234 11.00000 -1.50000
H11C 2 1.107877 -0.099168 0.284194 11.00000 -1.50000
AFIX 0
C12 1 0.937007 -0.353950 0.259263 11.00000 0.02246 0.01453 =
0.02842 -0.00180 -0.00433 -0.00506
AFIX 137
H12A 2 0.897058 -0.341882 0.332574 11.00000 -1.50000
H12B 2 1.057621 -0.411520 0.256696 11.00000 -1.50000
H12C 2 0.849613 -0.402745 0.235845 11.00000 -1.50000
AFIX 0
C13 1 1.034389 -0.221847 0.042843 11.00000 0.02418 0.03739 =
0.01825 -0.01185 -0.00236 0.00743
AFIX 137
H13A 2 1.138618 -0.297952 0.050633 11.00000 -1.50000
H13B 2 1.072914 -0.135950 -0.006129 11.00000 -1.50000
H13C 2 0.937623 -0.254261 0.014125 11.00000 -1.50000
AFIX 0
C14 1 0.463968 0.261879 0.530676 11.00000 0.02157 0.02364 =
0.01493 -0.00426 0.00336 -0.00671
AFIX 137
H14A 2 0.370172 0.223056 0.504170 11.00000 -1.50000
H14B 2 0.418991 0.360457 0.538496 11.00000 -1.50000
H14C 2 0.492267 0.202655 0.600147 11.00000 -1.50000
AFIX 0
C15 1 0.792783 0.080729 0.422541 11.00000 0.02256 0.01608 =
0.01896 -0.00097 -0.00356 -0.00107
AFIX 137
H15A 2 0.906916 0.090546 0.375505 11.00000 -1.50000
H15B 2 0.714859 0.030962 0.392475 11.00000 -1.50000
H15C 2 0.819804 0.025334 0.493346 11.00000 -1.50000
AFIX 0
HKLF 4
REM RM076 in P1 New: P-1
REM R1 = 0.0154 for 4632 Fo > 4sig(Fo) and 0.0185 for all 4960 data
REM 186 parameters refined using 0 restraints
END
WGHT 0.0161 0.2283
REM Highest difference peak 1.024, deepest hole -0.459, 1-sigma level 0.107
Q1 1 0.7103 0.0061 0.1145 11.00000 0.05 1.02
Q2 1 0.6853 0.1623 -0.0025 11.00000 0.05 0.88
Q3 1 0.6898 -0.0686 0.2599 11.00000 0.05 0.64
Q4 1 0.5754 0.4344 0.2913 11.00000 0.05 0.63
Q5 1 0.6501 0.3661 0.3626 11.00000 0.05 0.61
;
_shelx_res_checksum 73372
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_testm1
_database_code_depnum_ccdc_archive 'CCDC 1589408'
_audit_update_record
;
2017-12-05 deposited with the CCDC.
2018-01-23 downloaded from the CCDC.
;
_audit_creation_date 2016-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number 2013-4
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'B C24 F20, C38 H53 Fe2 N2 Si2'
_chemical_formula_sum 'C62 H53 B F20 Fe2 N2 Si2'
_chemical_formula_weight 1384.75
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 11.5252(5)
_cell_length_b 26.6215(10)
_cell_length_c 18.4948(7)
_cell_angle_alpha 90
_cell_angle_beta 91.736(3)
_cell_angle_gamma 90
_cell_volume 5671.9(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 4434
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 19.142
_cell_measurement_theta_min 2.204
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.664
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.6390
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0767 before and 0.0677 after correction. The Ratio of minimum to maximum transmission is 0.8570. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour red
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.622
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2816
_exptl_crystal_size_max 0.02
_exptl_crystal_size_mid 0.02
_exptl_crystal_size_min 0.02
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1593
_diffrn_reflns_av_unetI/netI 0.0919
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 32
_diffrn_reflns_limit_k_min -32
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 85664
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 25.681
_diffrn_reflns_theta_min 1.341
_diffrn_ambient_temperature 100(2)
_diffrn_detector 'Bruker area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type 'Bruker P4'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6230
_reflns_number_total 10766
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.27A (Bruker, 2012)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max 1.322
_refine_diff_density_min -0.745
_refine_diff_density_rms 0.087
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.011
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 810
_refine_ls_number_reflns 10766
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1208
_refine_ls_R_factor_gt 0.0555
_refine_ls_restrained_S_all 1.011
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+5.4887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1201
_refine_ls_wR_factor_ref 0.1506
_refine_special_details
;
Weak data and not a brilliant crystal hence high Rint of 15.9% but refinement stable without restraints.
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups, All Si(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
Si2(H2), N1(H1), C5(H5), C7(H7), C9(H9), C10(H10), C21(H21), C23(H23),
C24(H24), C25(H25), C26(H26), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C31(H31A,H31B), C32(H32A,
H32B), C33(H33A,H33B)
2.c Aromatic/amide H refined with riding coordinates:
C2(H2A), C3(H3), C4(H4), C8(H8), C27(H27)
2.d Idealised Me refined as rotating group:
C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
H19C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,
H38B,H38C)
;
_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
F1 F 0.0283(2) 0.59139(10) 0.16194(14) 0.0364(7) Uani 1 1 d . . . . .
F2 F -0.0699(3) 0.50215(12) 0.13865(17) 0.0559(9) Uani 1 1 d . . . . .
F3 F 0.0348(3) 0.43312(11) 0.05261(19) 0.0637(10) Uani 1 1 d . . . . .
F4 F 0.2405(3) 0.45589(10) -0.00726(17) 0.0520(9) Uani 1 1 d . . . . .
F5 F 0.3424(2) 0.54319(10) 0.01675(14) 0.0365(7) Uani 1 1 d . . . . .
F6 F 0.4336(2) 0.57178(9) 0.15466(14) 0.0316(7) Uani 1 1 d . . . . .
F7 F 0.6564(2) 0.58221(11) 0.12567(16) 0.0410(7) Uani 1 1 d . . . . .
F8 F 0.7250(2) 0.65645(11) 0.03367(16) 0.0447(8) Uani 1 1 d . . . . .
F9 F 0.5636(3) 0.72088(10) -0.02420(16) 0.0413(8) Uani 1 1 d . . . . .
F10 F 0.3414(2) 0.71120(10) 0.00443(15) 0.0348(7) Uani 1 1 d . . . . .
F11 F 0.2105(2) 0.62324(10) -0.04843(14) 0.0330(7) Uani 1 1 d . . . . .
F12 F 0.0334(3) 0.65559(11) -0.13117(14) 0.0441(8) Uani 1 1 d . . . . .
F13 F -0.1382(3) 0.71184(12) -0.07401(16) 0.0497(8) Uani 1 1 d . . . . .
F14 F -0.1231(2) 0.73759(10) 0.06913(15) 0.0369(7) Uani 1 1 d . . . . .
F15 F 0.0483(2) 0.70423(10) 0.15351(14) 0.0321(7) Uani 1 1 d . . . . .
F16 F 0.2756(2) 0.73074(9) 0.15936(14) 0.0312(6) Uani 1 1 d . . . . .
F17 F 0.2797(3) 0.76269(10) 0.29476(15) 0.0431(8) Uani 1 1 d . . . . .
F18 F 0.2614(3) 0.69495(12) 0.40752(15) 0.0492(8) Uani 1 1 d . . . . .
F19 F 0.2421(3) 0.59572(11) 0.37712(14) 0.0425(8) Uani 1 1 d . . . . .
F20 F 0.2320(2) 0.56313(10) 0.24281(14) 0.0345(7) Uani 1 1 d . . . . .
C39 C 0.1926(4) 0.57214(17) 0.0933(2) 0.0253(11) Uani 1 1 d . . . . .
C40 C 0.0863(4) 0.55808(18) 0.1205(2) 0.0302(12) Uani 1 1 d . . . . .
C41 C 0.0326(5) 0.5127(2) 0.1094(3) 0.0376(13) Uani 1 1 d . . . . .
C42 C 0.0853(5) 0.47809(19) 0.0665(3) 0.0414(14) Uani 1 1 d . . . . .
C43 C 0.1888(5) 0.48918(18) 0.0363(3) 0.0385(14) Uani 1 1 d . . . . .
C44 C 0.2397(4) 0.53554(18) 0.0495(2) 0.0294(11) Uani 1 1 d . . . . .
C45 C 0.3743(4) 0.63970(17) 0.0798(2) 0.0250(11) Uani 1 1 d . . . . .
C46 C 0.4616(4) 0.60981(17) 0.1087(2) 0.0274(11) Uani 1 1 d . . . . .
C47 C 0.5782(4) 0.61419(18) 0.0950(3) 0.0295(11) Uani 1 1 d . . . . .
C48 C 0.6128(4) 0.65125(19) 0.0499(3) 0.0323(12) Uani 1 1 d . . . . .
C49 C 0.5314(4) 0.68336(18) 0.0207(3) 0.0303(12) Uani 1 1 d . . . . .
C50 C 0.4155(4) 0.67729(17) 0.0360(3) 0.0281(11) Uani 1 1 d . . . . .
C51 C 0.1414(4) 0.66177(17) 0.0573(2) 0.0245(11) Uani 1 1 d . . . . .
C52 C 0.1300(4) 0.65200(17) -0.0162(3) 0.0263(11) Uani 1 1 d . . . . .
C53 C 0.0398(4) 0.66831(18) -0.0605(2) 0.0305(12) Uani 1 1 d . . . . .
C54 C -0.0467(4) 0.69665(18) -0.0320(3) 0.0327(12) Uani 1 1 d . . . . .
C55 C -0.0393(4) 0.70898(17) 0.0396(3) 0.0297(11) Uani 1 1 d . . . . .
C56 C 0.0523(4) 0.69134(17) 0.0823(2) 0.0255(11) Uani 1 1 d . . . . .
C57 C 0.2469(4) 0.64569(17) 0.1926(2) 0.0252(11) Uani 1 1 d . . . . .
C58 C 0.2639(4) 0.69559(17) 0.2117(3) 0.0271(11) Uani 1 1 d . . . . .
C59 C 0.2675(4) 0.71321(19) 0.2816(3) 0.0306(12) Uani 1 1 d . . . . .
C60 C 0.2579(4) 0.6794(2) 0.3380(3) 0.0339(12) Uani 1 1 d . . . . .
C61 C 0.2479(4) 0.62951(19) 0.3226(3) 0.0323(12) Uani 1 1 d . . . . .
C62 C 0.2420(4) 0.61369(18) 0.2516(3) 0.0279(11) Uani 1 1 d . . . . .
B1 B 0.2395(5) 0.63010(19) 0.1060(3) 0.0238(12) Uani 1 1 d . . . . .
Fe1 Fe 0.89233(6) 0.38691(3) 0.36845(4) 0.02973(19) Uani 1 1 d . . . . .
Fe2 Fe 0.39780(6) 0.40642(3) 0.43873(4) 0.03095(19) Uani 1 1 d . . . . .
Si1 Si 0.66470(11) 0.39195(5) 0.34299(7) 0.0249(3) Uani 1 1 d . . . . .
Si2 Si 0.31103(12) 0.33986(5) 0.54027(8) 0.0321(3) Uani 1 1 d . . . . .
H2 H 0.3063 0.3050 0.5203 0.038 Uiso 1 1 calc R . . . .
N1 N 0.5505(3) 0.39792(13) 0.26534(19) 0.0251(9) Uani 1 1 d . . . . .
H1 H 0.4785 0.4023 0.2935 0.030 Uiso 1 1 calc R . . . .
N2 N 0.2643(3) 0.33869(15) 0.6272(2) 0.0314(10) Uani 1 1 d . . . . .
C1 C 0.7680(4) 0.33828(17) 0.3375(3) 0.0274(11) Uani 1 1 d . . . . .
C2 C 0.8195(4) 0.32300(17) 0.4065(3) 0.0324(12) Uani 1 1 d . . . . .
H2A H 0.7795 0.3195 0.4504 0.039 Uiso 1 1 calc R . . . .
C3 C 0.9393(4) 0.31407(19) 0.3974(3) 0.0388(13) Uani 1 1 d . . . . .
H3 H 0.9928 0.3034 0.4344 0.047 Uiso 1 1 calc R . . . .
C4 C 0.9668(5) 0.3234(2) 0.3251(3) 0.0409(14) Uani 1 1 d . . . . .
H4 H 1.0414 0.3205 0.3051 0.049 Uiso 1 1 calc R . . . .
C5 C 0.8632(4) 0.33791(19) 0.2872(3) 0.0344(12) Uani 1 1 d . . . . .
H5 H 0.8566 0.3467 0.2347 0.041 Uiso 1 1 calc R . . . .
C6 C 0.7754(4) 0.44245(17) 0.3587(3) 0.0300(11) Uani 1 1 d . . . . .
C7 C 0.8267(4) 0.44121(18) 0.4321(3) 0.0358(13) Uani 1 1 d . . . . .
H7 H 0.7829 0.4352 0.4772 0.043 Uiso 1 1 calc R . . . .
C8 C 0.9493(5) 0.44846(19) 0.4292(3) 0.0411(14) Uani 1 1 d . . . . .
H8 H 1.0028 0.4484 0.4692 0.049 Uiso 1 1 calc R . . . .
C9 C 0.9764(5) 0.4557(2) 0.3568(3) 0.0435(14) Uani 1 1 d . . . . .
H9 H 1.0563 0.4603 0.3383 0.052 Uiso 1 1 calc R . . . .
C10 C 0.8739(4) 0.45215(19) 0.3136(3) 0.0402(14) Uani 1 1 d . . . . .
H10 H 0.8698 0.4553 0.2597 0.048 Uiso 1 1 calc R . . . .
C11 C 0.5493(5) 0.44815(17) 0.2211(3) 0.0316(12) Uani 1 1 d . . . . .
C12 C 0.4371(5) 0.45048(18) 0.1739(3) 0.0378(13) Uani 1 1 d . . . . .
H12A H 0.3708 0.4558 0.2058 0.045 Uiso 1 1 calc R . . . .
H12B H 0.4414 0.4800 0.1416 0.045 Uiso 1 1 calc R . . . .
C13 C 0.4128(5) 0.40454(18) 0.1281(3) 0.0398(13) Uani 1 1 d . . . . .
H13A H 0.4752 0.4001 0.0930 0.048 Uiso 1 1 calc R . . . .
H13B H 0.3383 0.4087 0.1007 0.048 Uiso 1 1 calc R . . . .
C14 C 0.4068(4) 0.35854(18) 0.1768(3) 0.0334(12) Uani 1 1 d . . . . .
H14A H 0.3896 0.3287 0.1465 0.040 Uiso 1 1 calc R . . . .
H14B H 0.3418 0.3629 0.2101 0.040 Uiso 1 1 calc R . . . .
C15 C 0.5188(4) 0.34891(17) 0.2218(3) 0.0288(11) Uani 1 1 d . . . . .
C16 C 0.5454(5) 0.49112(17) 0.2765(3) 0.0351(13) Uani 1 1 d . . . . .
H16A H 0.4856 0.4840 0.3117 0.053 Uiso 1 1 calc GR . . . .
H16B H 0.5270 0.5227 0.2515 0.053 Uiso 1 1 calc GR . . . .
H16C H 0.6210 0.4940 0.3018 0.053 Uiso 1 1 calc GR . . . .
C17 C 0.6560(5) 0.4523(2) 0.1758(3) 0.0443(14) Uani 1 1 d . . . . .
H17A H 0.7213 0.4352 0.2004 0.066 Uiso 1 1 calc GR . . . .
H17B H 0.6753 0.4878 0.1690 0.066 Uiso 1 1 calc GR . . . .
H17C H 0.6405 0.4366 0.1285 0.066 Uiso 1 1 calc GR . . . .
C18 C 0.6165(4) 0.33212(19) 0.1740(3) 0.0357(13) Uani 1 1 d . . . . .
H18A H 0.6352 0.3592 0.1404 0.054 Uiso 1 1 calc GR . . . .
H18B H 0.5920 0.3023 0.1465 0.054 Uiso 1 1 calc GR . . . .
H18C H 0.6853 0.3241 0.2042 0.054 Uiso 1 1 calc GR . . . .
C19 C 0.4942(4) 0.30808(18) 0.2774(3) 0.0327(12) Uani 1 1 d . . . . .
H19A H 0.5664 0.2992 0.3037 0.049 Uiso 1 1 calc GR . . . .
H19B H 0.4627 0.2783 0.2526 0.049 Uiso 1 1 calc GR . . . .
H19C H 0.4376 0.3206 0.3116 0.049 Uiso 1 1 calc GR . . . .
C20 C 0.5733(4) 0.39090(17) 0.4243(2) 0.0273(11) Uani 1 1 d . . . . .
C21 C 0.5139(4) 0.35008(18) 0.4568(2) 0.0285(11) Uani 1 1 d . . . . .
H21 H 0.5069 0.3156 0.4356 0.034 Uiso 1 1 calc R . . . .
C22 C 0.4614(4) 0.36583(18) 0.5228(3) 0.0293(11) Uani 1 1 d . . . . .
C23 C 0.4923(4) 0.41775(19) 0.5312(3) 0.0341(12) Uani 1 1 d . . . . .
H23 H 0.4691 0.4398 0.5720 0.041 Uiso 1 1 calc R . . . .
C24 C 0.5582(4) 0.43349(19) 0.4708(3) 0.0308(12) Uani 1 1 d . . . . .
H24 H 0.5878 0.4682 0.4622 0.037 Uiso 1 1 calc R . . . .
C25 C 0.2513(4) 0.4382(2) 0.4736(3) 0.0385(13) Uani 1 1 d . . . . .
H25 H 0.2456 0.4594 0.5180 0.046 Uiso 1 1 calc R . . . .
C26 C 0.2707(4) 0.4564(2) 0.4034(3) 0.0414(14) Uani 1 1 d . . . . .
H26 H 0.2834 0.4924 0.3899 0.050 Uiso 1 1 calc R . . . .
C27 C 0.2726(4) 0.4143(2) 0.3549(3) 0.0381(13) Uani 1 1 d . . . . .
H27 H 0.2843 0.4154 0.3043 0.046 Uiso 1 1 calc R . . . .
C28 C 0.2538(4) 0.3712(2) 0.3966(3) 0.0378(13) Uani 1 1 d . . . . .
H28 H 0.2525 0.3361 0.3774 0.045 Uiso 1 1 calc R . . . .
C29 C 0.2405(4) 0.38438(19) 0.4715(3) 0.0324(12) Uani 1 1 d . . . . .
C30 C 0.1472(4) 0.35917(19) 0.6477(3) 0.0357(13) Uani 1 1 d . . . . .
C31 C 0.1033(5) 0.3317(2) 0.7142(3) 0.0387(13) Uani 1 1 d . . . . .
H31A H 0.0331 0.3491 0.7308 0.046 Uiso 1 1 calc R . . . .
H31B H 0.0803 0.2972 0.6998 0.046 Uiso 1 1 calc R . . . .
C32 C 0.1913(5) 0.3285(2) 0.7771(3) 0.0428(14) Uani 1 1 d . . . . .
H32A H 0.2166 0.3625 0.7922 0.051 Uiso 1 1 calc R . . . .
H32B H 0.1567 0.3115 0.8189 0.051 Uiso 1 1 calc R . . . .
C33 C 0.2937(5) 0.2984(2) 0.7504(3) 0.0406(14) Uani 1 1 d . . . . .
H33A H 0.2668 0.2643 0.7370 0.049 Uiso 1 1 calc R . . . .
H33B H 0.3523 0.2950 0.7903 0.049 Uiso 1 1 calc R . . . .
C34 C 0.3514(4) 0.32228(18) 0.6851(3) 0.0332(12) Uani 1 1 d . . . . .
C35 C 0.0583(5) 0.3476(2) 0.5868(3) 0.0508(16) Uani 1 1 d . . . . .
H35A H 0.0761 0.3676 0.5440 0.076 Uiso 1 1 calc GR . . . .
H35B H -0.0197 0.3560 0.6026 0.076 Uiso 1 1 calc GR . . . .
H35C H 0.0617 0.3118 0.5747 0.076 Uiso 1 1 calc GR . . . .
C36 C 0.1521(6) 0.4150(2) 0.6627(3) 0.0560(18) Uani 1 1 d . . . . .
H36A H 0.1984 0.4211 0.7072 0.084 Uiso 1 1 calc GR . . . .
H36B H 0.0732 0.4278 0.6685 0.084 Uiso 1 1 calc GR . . . .
H36C H 0.1878 0.4322 0.6222 0.084 Uiso 1 1 calc GR . . . .
C37 C 0.4291(5) 0.3654(2) 0.7108(3) 0.0413(14) Uani 1 1 d . . . . .
H37A H 0.4686 0.3797 0.6694 0.062 Uiso 1 1 calc GR . . . .
H37B H 0.4870 0.3528 0.7463 0.062 Uiso 1 1 calc GR . . . .
H37C H 0.3818 0.3913 0.7332 0.062 Uiso 1 1 calc GR . . . .
C38 C 0.4282(5) 0.2803(2) 0.6541(3) 0.0435(14) Uani 1 1 d . . . . .
H38A H 0.3786 0.2537 0.6335 0.065 Uiso 1 1 calc GR . . . .
H38B H 0.4783 0.2663 0.6928 0.065 Uiso 1 1 calc GR . . . .
H38C H 0.4763 0.2943 0.6162 0.065 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
F1 0.0353(17) 0.0449(17) 0.0291(16) -0.0025(13) 0.0050(13) -0.0083(14)
F2 0.055(2) 0.063(2) 0.050(2) 0.0107(17) 0.0003(17) -0.0290(18)
F3 0.095(3) 0.0311(18) 0.064(2) 0.0009(16) -0.021(2) -0.0278(18)
F4 0.083(3) 0.0295(17) 0.0424(19) -0.0135(14) -0.0128(17) 0.0083(17)
F5 0.0416(18) 0.0383(17) 0.0295(16) -0.0085(13) 0.0012(14) 0.0063(14)
F6 0.0353(16) 0.0294(15) 0.0298(16) 0.0038(12) -0.0030(13) 0.0013(13)
F7 0.0328(17) 0.0467(18) 0.0431(19) -0.0064(14) -0.0037(14) 0.0099(14)
F8 0.0288(17) 0.058(2) 0.0474(19) -0.0099(16) 0.0106(14) -0.0100(15)
F9 0.0456(19) 0.0389(17) 0.0401(18) 0.0022(14) 0.0125(15) -0.0114(14)
F10 0.0400(17) 0.0299(15) 0.0345(17) 0.0074(13) 0.0022(13) -0.0009(13)
F11 0.0380(17) 0.0374(16) 0.0238(15) -0.0045(12) 0.0052(13) 0.0007(13)
F12 0.060(2) 0.0526(19) 0.0193(16) 0.0044(13) -0.0008(14) -0.0005(16)
F13 0.051(2) 0.061(2) 0.0355(18) 0.0146(16) -0.0119(15) 0.0114(17)
F14 0.0319(16) 0.0366(16) 0.0420(18) 0.0012(14) -0.0010(14) 0.0093(13)
F15 0.0305(16) 0.0415(17) 0.0241(15) -0.0094(12) 0.0002(12) 0.0039(13)
F16 0.0384(17) 0.0272(15) 0.0279(16) 0.0000(12) -0.0002(13) -0.0016(13)
F17 0.058(2) 0.0347(17) 0.0362(18) -0.0143(14) -0.0087(15) -0.0021(15)
F18 0.064(2) 0.063(2) 0.0198(16) -0.0117(14) -0.0011(15) -0.0050(17)
F19 0.0521(19) 0.0537(19) 0.0215(16) 0.0075(14) -0.0007(14) -0.0055(16)
F20 0.0469(18) 0.0299(16) 0.0265(16) 0.0040(12) -0.0024(13) -0.0030(13)
C39 0.028(3) 0.025(3) 0.022(3) 0.001(2) -0.004(2) 0.001(2)
C40 0.040(3) 0.030(3) 0.020(3) -0.001(2) -0.003(2) -0.004(2)
C41 0.043(3) 0.044(3) 0.025(3) 0.005(3) -0.006(2) -0.012(3)
C42 0.062(4) 0.027(3) 0.033(3) 0.009(2) -0.018(3) -0.015(3)
C43 0.067(4) 0.022(3) 0.026(3) -0.007(2) -0.014(3) 0.004(3)
C44 0.037(3) 0.030(3) 0.020(3) 0.002(2) -0.002(2) 0.002(2)
C45 0.031(3) 0.025(3) 0.020(3) -0.003(2) 0.004(2) 0.000(2)
C46 0.034(3) 0.026(3) 0.023(3) -0.005(2) 0.004(2) -0.003(2)
C47 0.032(3) 0.032(3) 0.024(3) -0.009(2) -0.004(2) 0.004(2)
C48 0.032(3) 0.036(3) 0.030(3) -0.011(2) 0.005(2) -0.005(2)
C49 0.038(3) 0.028(3) 0.026(3) -0.008(2) 0.004(2) -0.010(2)
C50 0.034(3) 0.026(3) 0.025(3) -0.005(2) -0.003(2) 0.003(2)
C51 0.025(3) 0.023(2) 0.025(3) -0.004(2) 0.002(2) -0.004(2)
C52 0.032(3) 0.022(3) 0.025(3) 0.000(2) 0.002(2) -0.003(2)
C53 0.040(3) 0.035(3) 0.016(3) 0.003(2) 0.001(2) -0.008(2)
C54 0.038(3) 0.034(3) 0.025(3) 0.012(2) -0.007(2) -0.004(2)
C55 0.029(3) 0.023(3) 0.037(3) 0.001(2) 0.003(2) 0.002(2)
C56 0.032(3) 0.025(3) 0.019(3) 0.000(2) -0.001(2) -0.005(2)
C57 0.020(3) 0.032(3) 0.024(3) -0.002(2) 0.000(2) 0.002(2)
C58 0.024(3) 0.032(3) 0.025(3) -0.004(2) -0.003(2) -0.001(2)
C59 0.031(3) 0.033(3) 0.028(3) -0.006(2) -0.003(2) -0.001(2)
C60 0.031(3) 0.052(4) 0.018(3) -0.014(2) -0.002(2) 0.001(3)
C61 0.030(3) 0.042(3) 0.025(3) 0.004(2) -0.001(2) -0.004(2)
C62 0.026(3) 0.030(3) 0.028(3) -0.002(2) 0.000(2) 0.001(2)
B1 0.031(3) 0.023(3) 0.018(3) -0.003(2) 0.003(2) 0.003(2)
Fe1 0.0278(4) 0.0312(4) 0.0302(4) 0.0012(3) 0.0017(3) 0.0014(3)
Fe2 0.0269(4) 0.0384(4) 0.0275(4) 0.0010(3) 0.0014(3) 0.0038(3)
Si1 0.0257(7) 0.0274(7) 0.0219(7) 0.0024(6) 0.0029(6) 0.0008(6)
Si2 0.0338(8) 0.0334(8) 0.0291(8) -0.0039(6) 0.0030(6) -0.0018(6)
N1 0.032(2) 0.023(2) 0.021(2) 0.0054(16) -0.0002(17) -0.0008(17)
N2 0.029(2) 0.041(3) 0.024(2) 0.0000(19) 0.0041(18) 0.003(2)
C1 0.029(3) 0.028(3) 0.025(3) 0.000(2) -0.001(2) 0.004(2)
C2 0.038(3) 0.029(3) 0.030(3) 0.003(2) -0.005(2) -0.005(2)
C3 0.032(3) 0.034(3) 0.050(4) 0.002(3) -0.010(3) 0.003(2)
C4 0.031(3) 0.046(3) 0.047(4) -0.013(3) 0.001(3) 0.002(3)
C5 0.034(3) 0.041(3) 0.029(3) -0.007(2) 0.002(2) 0.005(2)
C6 0.029(3) 0.024(3) 0.037(3) 0.003(2) 0.000(2) 0.005(2)
C7 0.032(3) 0.038(3) 0.037(3) -0.003(2) -0.004(2) 0.000(2)
C8 0.035(3) 0.034(3) 0.054(4) -0.006(3) -0.013(3) -0.002(2)
C9 0.030(3) 0.041(3) 0.059(4) 0.004(3) 0.002(3) -0.002(3)
C10 0.035(3) 0.038(3) 0.047(3) 0.012(3) 0.001(3) -0.006(3)
C11 0.049(3) 0.021(3) 0.025(3) 0.002(2) -0.004(2) -0.004(2)
C12 0.061(4) 0.026(3) 0.026(3) 0.006(2) -0.013(3) -0.002(3)
C13 0.053(4) 0.036(3) 0.030(3) 0.002(2) -0.013(3) 0.003(3)
C14 0.039(3) 0.032(3) 0.029(3) -0.004(2) -0.008(2) -0.003(2)
C15 0.034(3) 0.024(3) 0.028(3) -0.001(2) -0.001(2) -0.004(2)
C16 0.052(4) 0.021(3) 0.031(3) -0.001(2) -0.013(3) 0.004(2)
C17 0.065(4) 0.037(3) 0.031(3) 0.009(2) 0.007(3) -0.005(3)
C18 0.045(3) 0.035(3) 0.028(3) -0.004(2) 0.002(2) 0.000(2)
C19 0.035(3) 0.033(3) 0.030(3) 0.001(2) -0.001(2) -0.002(2)
C20 0.027(3) 0.033(3) 0.022(3) 0.004(2) -0.004(2) 0.003(2)
C21 0.030(3) 0.033(3) 0.022(3) 0.004(2) -0.001(2) 0.002(2)
C22 0.029(3) 0.036(3) 0.023(3) 0.001(2) 0.002(2) 0.001(2)
C23 0.031(3) 0.045(3) 0.027(3) -0.007(2) 0.003(2) 0.002(2)
C24 0.028(3) 0.036(3) 0.028(3) -0.001(2) -0.003(2) 0.004(2)
C25 0.028(3) 0.053(4) 0.035(3) 0.002(3) 0.004(2) 0.009(3)
C26 0.030(3) 0.053(4) 0.042(3) 0.007(3) 0.003(3) 0.006(3)
C27 0.028(3) 0.053(4) 0.033(3) 0.012(3) -0.004(2) 0.009(3)
C28 0.030(3) 0.052(3) 0.032(3) 0.001(3) -0.002(2) 0.001(3)
C29 0.022(3) 0.042(3) 0.033(3) 0.000(2) -0.004(2) 0.002(2)
C30 0.038(3) 0.038(3) 0.032(3) -0.003(2) 0.007(2) 0.000(2)
C31 0.035(3) 0.050(3) 0.031(3) 0.003(3) 0.007(2) -0.003(3)
C32 0.042(3) 0.055(4) 0.031(3) 0.000(3) 0.008(3) 0.000(3)
C33 0.042(3) 0.046(3) 0.034(3) 0.008(3) 0.000(3) -0.004(3)
C34 0.038(3) 0.036(3) 0.025(3) -0.005(2) 0.002(2) -0.001(2)
C35 0.030(3) 0.089(5) 0.034(3) 0.002(3) 0.002(3) 0.001(3)
C36 0.063(4) 0.048(4) 0.058(4) 0.000(3) 0.028(3) 0.007(3)
C37 0.044(3) 0.048(3) 0.032(3) 0.001(3) -0.002(3) -0.004(3)
C38 0.049(4) 0.042(3) 0.040(3) 0.006(3) 0.004(3) 0.007(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C40 1.361(5) . ?
F2 C41 1.343(6) . ?
F3 C42 1.352(6) . ?
F4 C43 1.349(6) . ?
F5 C44 1.360(5) . ?
F6 C46 1.367(5) . ?
F7 C47 1.351(5) . ?
F8 C48 1.343(5) . ?
F9 C49 1.358(5) . ?
F10 C50 1.362(5) . ?
F11 C52 1.355(5) . ?
F12 C53 1.350(5) . ?
F13 C54 1.353(6) . ?
F14 C55 1.357(5) . ?
F15 C56 1.363(5) . ?
F16 C58 1.356(5) . ?
F17 C59 1.346(5) . ?
F18 C60 1.350(5) . ?
F19 C61 1.354(5) . ?
F20 C62 1.360(5) . ?
C39 C40 1.389(6) . ?
C39 C44 1.388(6) . ?
C39 B1 1.650(7) . ?
C40 C41 1.370(7) . ?
C41 C42 1.370(8) . ?
C42 C43 1.365(8) . ?
C43 C44 1.385(7) . ?
C45 C46 1.379(7) . ?
C45 C50 1.380(6) . ?
C45 B1 1.661(7) . ?
C46 C47 1.380(7) . ?
C47 C48 1.360(7) . ?
C48 C49 1.368(7) . ?
C49 C50 1.383(7) . ?
C51 C52 1.387(6) . ?
C51 C56 1.384(6) . ?
C51 B1 1.655(7) . ?
C52 C53 1.374(7) . ?
C53 C54 1.368(7) . ?
C54 C55 1.365(7) . ?
C55 C56 1.382(7) . ?
C57 C58 1.387(6) . ?
C57 C62 1.387(6) . ?
C57 B1 1.655(7) . ?
C58 C59 1.374(6) . ?
C59 C60 1.386(7) . ?
C60 C61 1.362(7) . ?
C61 C62 1.379(7) . ?
Fe1 Si1 2.6547(15) . ?
Fe1 C1 2.002(5) . ?
Fe1 C2 2.032(5) . ?
Fe1 C3 2.079(5) . ?
Fe1 C4 2.069(5) . ?
Fe1 C5 2.010(5) . ?
Fe1 C6 2.005(5) . ?
Fe1 C7 2.026(5) . ?
Fe1 C8 2.081(5) . ?
Fe1 C9 2.085(5) . ?
Fe1 C10 2.019(5) . ?
Fe2 Si2 2.7894(16) . ?
Fe2 C20 2.090(5) . ?
Fe2 C21 2.031(5) . ?
Fe2 C22 2.014(5) . ?
Fe2 C23 2.022(5) . ?
Fe2 C24 2.055(5) . ?
Fe2 C25 2.012(5) . ?
Fe2 C26 2.071(5) . ?
Fe2 C27 2.096(5) . ?
Fe2 C28 2.040(5) . ?
Fe2 C29 2.016(5) . ?
Si1 N1 1.925(4) . ?
Si1 C1 1.865(5) . ?
Si1 C6 1.870(5) . ?
Si1 C20 1.862(5) . ?
Si2 H2 1.0000 . ?
Si2 N2 1.710(4) . ?
Si2 C22 1.903(5) . ?
Si2 C29 1.903(5) . ?
N1 H1 1.0000 . ?
N1 C11 1.568(6) . ?
N1 C15 1.571(6) . ?
N2 C30 1.515(6) . ?
N2 C34 1.511(6) . ?
C1 C2 1.449(7) . ?
C1 C5 1.458(6) . ?
C2 H2A 0.9500 . ?
C2 C3 1.417(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.406(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.419(7) . ?
C5 H5 1.0000 . ?
C6 C7 1.464(7) . ?
C6 C10 1.452(7) . ?
C7 H7 1.0000 . ?
C7 C8 1.429(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.397(8) . ?
C9 H9 1.0000 . ?
C9 C10 1.408(7) . ?
C10 H10 1.0000 . ?
C11 C12 1.539(7) . ?
C11 C16 1.538(6) . ?
C11 C17 1.513(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.509(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.524(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.536(7) . ?
C15 C18 1.520(6) . ?
C15 C19 1.529(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
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 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.427(6) . ?
C20 C24 1.437(7) . ?
C21 H21 1.0000 . ?
C21 C22 1.441(6) . ?
C22 C23 1.434(7) . ?
C23 H23 1.0000 . ?
C23 C24 1.432(7) . ?
C24 H24 1.0000 . ?
C25 H25 1.0000 . ?
C25 C26 1.411(7) . ?
C25 C29 1.439(7) . ?
C26 H26 1.0000 . ?
C26 C27 1.436(7) . ?
C27 H27 0.9500 . ?
C27 C28 1.403(7) . ?
C28 H28 1.0000 . ?
C28 C29 1.440(7) . ?
C30 C31 1.529(7) . ?
C30 C35 1.530(7) . ?
C30 C36 1.512(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.522(7) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.522(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.532(7) . ?
C34 C37 1.523(7) . ?
C34 C38 1.547(7) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 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
C40 C39 B1 119.3(4) . . ?
C44 C39 C40 112.8(4) . . ?
C44 C39 B1 127.4(4) . . ?
F1 C40 C39 118.8(4) . . ?
F1 C40 C41 115.5(4) . . ?
C41 C40 C39 125.6(5) . . ?
F2 C41 C40 121.5(5) . . ?
F2 C41 C42 120.2(5) . . ?
C42 C41 C40 118.2(5) . . ?
F3 C42 C41 120.6(5) . . ?
F3 C42 C43 119.4(5) . . ?
C43 C42 C41 120.0(5) . . ?
F4 C43 C42 120.6(5) . . ?
F4 C43 C44 119.9(5) . . ?
C42 C43 C44 119.5(5) . . ?
F5 C44 C39 121.0(4) . . ?
F5 C44 C43 115.1(4) . . ?
C43 C44 C39 123.8(5) . . ?
C46 C45 C50 112.7(4) . . ?
C46 C45 B1 118.4(4) . . ?
C50 C45 B1 128.6(4) . . ?
F6 C46 C45 119.0(4) . . ?
F6 C46 C47 115.3(4) . . ?
C45 C46 C47 125.7(4) . . ?
F7 C47 C46 120.7(4) . . ?
F7 C47 C48 120.7(4) . . ?
C48 C47 C46 118.6(5) . . ?
F8 C48 C47 120.9(5) . . ?
F8 C48 C49 120.1(5) . . ?
C47 C48 C49 119.0(5) . . ?
F9 C49 C48 120.2(4) . . ?
F9 C49 C50 119.7(5) . . ?
C48 C49 C50 120.1(5) . . ?
F10 C50 C45 120.7(4) . . ?
F10 C50 C49 115.6(4) . . ?
C45 C50 C49 123.8(5) . . ?
C52 C51 B1 118.7(4) . . ?
C56 C51 C52 112.6(4) . . ?
C56 C51 B1 127.6(4) . . ?
F11 C52 C51 119.4(4) . . ?
F11 C52 C53 115.6(4) . . ?
C53 C52 C51 125.0(4) . . ?
F12 C53 C52 121.1(4) . . ?
F12 C53 C54 119.5(5) . . ?
C54 C53 C52 119.4(4) . . ?
F13 C54 C53 120.5(4) . . ?
F13 C54 C55 120.7(5) . . ?
C55 C54 C53 118.8(5) . . ?
F14 C55 C54 120.0(5) . . ?
F14 C55 C56 120.1(4) . . ?
C54 C55 C56 119.8(5) . . ?
F15 C56 C51 120.9(4) . . ?
F15 C56 C55 114.7(4) . . ?
C55 C56 C51 124.4(4) . . ?
C58 C57 B1 119.3(4) . . ?
C62 C57 C58 113.4(4) . . ?
C62 C57 B1 127.3(4) . . ?
F16 C58 C57 119.7(4) . . ?
F16 C58 C59 115.8(4) . . ?
C59 C58 C57 124.5(5) . . ?
F17 C59 C58 120.3(4) . . ?
F17 C59 C60 120.7(4) . . ?
C58 C59 C60 119.1(5) . . ?
F18 C60 C59 121.1(5) . . ?
F18 C60 C61 119.9(5) . . ?
C61 C60 C59 118.9(4) . . ?
F19 C61 C60 119.8(4) . . ?
F19 C61 C62 120.3(4) . . ?
C60 C61 C62 119.9(5) . . ?
F20 C62 C57 121.2(4) . . ?
F20 C62 C61 114.7(4) . . ?
C61 C62 C57 124.0(5) . . ?
C39 B1 C45 114.1(4) . . ?
C39 B1 C51 100.6(4) . . ?
C39 B1 C57 112.3(4) . . ?
C51 B1 C45 113.1(4) . . ?
C51 B1 C57 114.4(4) . . ?
C57 B1 C45 102.9(4) . . ?
C1 Fe1 Si1 44.53(13) . . ?
C1 Fe1 C2 42.09(19) . . ?
C1 Fe1 C3 69.5(2) . . ?
C1 Fe1 C4 70.2(2) . . ?
C1 Fe1 C5 42.64(19) . . ?
C1 Fe1 C6 88.7(2) . . ?
C1 Fe1 C7 110.6(2) . . ?
C1 Fe1 C8 151.0(2) . . ?
C1 Fe1 C9 150.3(2) . . ?
C1 Fe1 C10 110.4(2) . . ?
C2 Fe1 Si1 71.77(15) . . ?
C2 Fe1 C3 40.29(19) . . ?
C2 Fe1 C4 68.3(2) . . ?
C2 Fe1 C8 126.8(2) . . ?
C2 Fe1 C9 165.7(2) . . ?
C3 Fe1 Si1 109.95(15) . . ?
C3 Fe1 C8 121.3(2) . . ?
C3 Fe1 C9 136.6(2) . . ?
C4 Fe1 Si1 113.06(15) . . ?
C4 Fe1 C3 39.6(2) . . ?
C4 Fe1 C8 136.5(2) . . ?
C4 Fe1 C9 118.5(2) . . ?
C5 Fe1 Si1 76.01(14) . . ?
C5 Fe1 C2 69.7(2) . . ?
C5 Fe1 C3 67.9(2) . . ?
C5 Fe1 C4 40.7(2) . . ?
C5 Fe1 C7 147.2(2) . . ?
C5 Fe1 C8 163.1(2) . . ?
C5 Fe1 C9 124.0(2) . . ?
C5 Fe1 C10 99.8(2) . . ?
C6 Fe1 Si1 44.68(14) . . ?
C6 Fe1 C2 111.4(2) . . ?
C6 Fe1 C3 151.7(2) . . ?
C6 Fe1 C4 148.6(2) . . ?
C6 Fe1 C5 108.4(2) . . ?
C6 Fe1 C7 42.61(19) . . ?
C6 Fe1 C8 70.6(2) . . ?
C6 Fe1 C9 69.9(2) . . ?
C6 Fe1 C10 42.29(19) . . ?
C7 Fe1 Si1 71.48(15) . . ?
C7 Fe1 C2 103.3(2) . . ?
C7 Fe1 C3 127.9(2) . . ?
C7 Fe1 C4 167.2(2) . . ?
C7 Fe1 C8 40.71(19) . . ?
C7 Fe1 C9 67.5(2) . . ?
C8 Fe1 Si1 110.48(15) . . ?
C8 Fe1 C9 39.2(2) . . ?
C9 Fe1 Si1 113.40(15) . . ?
C10 Fe1 Si1 77.24(15) . . ?
C10 Fe1 C2 148.8(2) . . ?
C10 Fe1 C3 162.6(2) . . ?
C10 Fe1 C4 123.2(2) . . ?
C10 Fe1 C7 69.1(2) . . ?
C10 Fe1 C8 67.7(2) . . ?
C10 Fe1 C9 40.1(2) . . ?
C20 Fe2 Si2 109.17(13) . . ?
C20 Fe2 C27 124.95(19) . . ?
C21 Fe2 Si2 70.60(13) . . ?
C21 Fe2 C20 40.49(18) . . ?
C21 Fe2 C24 68.2(2) . . ?
C21 Fe2 C26 169.4(2) . . ?
C21 Fe2 C27 129.1(2) . . ?
C21 Fe2 C28 104.4(2) . . ?
C22 Fe2 Si2 43.01(14) . . ?
C22 Fe2 C20 70.19(18) . . ?
C22 Fe2 C21 41.73(18) . . ?
C22 Fe2 C23 41.64(19) . . ?
C22 Fe2 C24 70.2(2) . . ?
C22 Fe2 C26 145.8(2) . . ?
C22 Fe2 C27 148.4(2) . . ?
C22 Fe2 C28 108.7(2) . . ?
C22 Fe2 C29 85.5(2) . . ?
C23 Fe2 Si2 73.76(15) . . ?
C23 Fe2 C20 68.82(19) . . ?
C23 Fe2 C21 68.6(2) . . ?
C23 Fe2 C24 41.11(19) . . ?
C23 Fe2 C26 121.9(2) . . ?
C23 Fe2 C27 162.1(2) . . ?
C23 Fe2 C28 143.4(2) . . ?
C24 Fe2 Si2 111.46(14) . . ?
C24 Fe2 C20 40.56(18) . . ?
C24 Fe2 C26 119.2(2) . . ?
C24 Fe2 C27 140.5(2) . . ?
C25 Fe2 Si2 74.34(15) . . ?
C25 Fe2 C20 161.6(2) . . ?
C25 Fe2 C21 144.4(2) . . ?
C25 Fe2 C22 105.5(2) . . ?
C25 Fe2 C23 95.8(2) . . ?
C25 Fe2 C24 121.1(2) . . ?
C25 Fe2 C26 40.4(2) . . ?
C25 Fe2 C27 68.2(2) . . ?
C25 Fe2 C28 68.6(2) . . ?
C25 Fe2 C29 41.9(2) . . ?
C26 Fe2 Si2 110.90(15) . . ?
C26 Fe2 C20 139.9(2) . . ?
C26 Fe2 C27 40.3(2) . . ?
C27 Fe2 Si2 107.99(15) . . ?
C28 Fe2 Si2 70.18(15) . . ?
C28 Fe2 C20 129.8(2) . . ?
C28 Fe2 C24 170.3(2) . . ?
C28 Fe2 C26 67.4(2) . . ?
C28 Fe2 C27 39.6(2) . . ?
C29 Fe2 Si2 43.02(14) . . ?
C29 Fe2 C20 149.72(19) . . ?
C29 Fe2 C21 109.2(2) . . ?
C29 Fe2 C23 104.8(2) . . ?
C29 Fe2 C24 145.6(2) . . ?
C29 Fe2 C26 69.4(2) . . ?
C29 Fe2 C27 69.3(2) . . ?
C29 Fe2 C28 41.59(19) . . ?
N1 Si1 Fe1 141.82(13) . . ?
C1 Si1 Fe1 48.83(15) . . ?
C1 Si1 N1 116.47(19) . . ?
C1 Si1 C6 97.2(2) . . ?
C6 Si1 Fe1 48.91(14) . . ?
C6 Si1 N1 120.29(19) . . ?
C20 Si1 Fe1 115.85(15) . . ?
C20 Si1 N1 102.31(19) . . ?
C20 Si1 C1 114.2(2) . . ?
C20 Si1 C6 106.6(2) . . ?
Fe2 Si2 H2 111.0 . . ?
N2 Si2 Fe2 140.68(15) . . ?
N2 Si2 H2 108.3 . . ?
N2 Si2 C22 118.7(2) . . ?
N2 Si2 C29 120.0(2) . . ?
C22 Si2 Fe2 46.21(15) . . ?
C22 Si2 H2 108.3 . . ?
C22 Si2 C29 91.9(2) . . ?
C29 Si2 Fe2 46.27(15) . . ?
C29 Si2 H2 108.3 . . ?
Si1 N1 H1 100.3 . . ?
C11 N1 Si1 117.1(3) . . ?
C11 N1 H1 100.3 . . ?
C11 N1 C15 116.3(3) . . ?
C15 N1 Si1 117.2(3) . . ?
C15 N1 H1 100.3 . . ?
C30 N2 Si2 122.5(3) . . ?
C34 N2 Si2 116.8(3) . . ?
C34 N2 C30 120.3(4) . . ?
Si1 C1 Fe1 86.65(19) . . ?
C2 C1 Fe1 70.1(3) . . ?
C2 C1 Si1 114.3(3) . . ?
C2 C1 C5 105.3(4) . . ?
C5 C1 Fe1 69.0(3) . . ?
C5 C1 Si1 122.3(4) . . ?
Fe1 C2 H2A 126.4 . . ?
C1 C2 Fe1 67.8(3) . . ?
C1 C2 H2A 125.8 . . ?
C3 C2 Fe1 71.6(3) . . ?
C3 C2 C1 108.5(5) . . ?
C3 C2 H2A 125.8 . . ?
Fe1 C3 H3 128.4 . . ?
C2 C3 Fe1 68.1(3) . . ?
C2 C3 H3 125.3 . . ?
C4 C3 Fe1 69.8(3) . . ?
C4 C3 C2 109.3(5) . . ?
C4 C3 H3 125.3 . . ?
Fe1 C4 H4 127.5 . . ?
C3 C4 Fe1 70.6(3) . . ?
C3 C4 H4 126.0 . . ?
C3 C4 C5 107.9(5) . . ?
C5 C4 Fe1 67.4(3) . . ?
C5 C4 H4 126.0 . . ?
Fe1 C5 H5 125.5 . . ?
C1 C5 Fe1 68.4(3) . . ?
C1 C5 H5 125.5 . . ?
C4 C5 Fe1 71.9(3) . . ?
C4 C5 C1 109.0(5) . . ?
C4 C5 H5 125.5 . . ?
Si1 C6 Fe1 86.41(19) . . ?
C7 C6 Fe1 69.5(3) . . ?
C7 C6 Si1 112.5(3) . . ?
C10 C6 Fe1 69.4(3) . . ?
C10 C6 Si1 125.5(4) . . ?
C10 C6 C7 103.7(4) . . ?
Fe1 C7 H7 125.3 . . ?
C6 C7 Fe1 67.9(3) . . ?
C6 C7 H7 125.3 . . ?
C8 C7 Fe1 71.7(3) . . ?
C8 C7 C6 109.4(5) . . ?
C8 C7 H7 125.3 . . ?
Fe1 C8 H8 127.3 . . ?
C7 C8 Fe1 67.5(3) . . ?
C7 C8 H8 126.1 . . ?
C9 C8 Fe1 70.5(3) . . ?
C9 C8 C7 107.8(5) . . ?
C9 C8 H8 126.1 . . ?
Fe1 C9 H9 125.4 . . ?
C8 C9 Fe1 70.3(3) . . ?
C8 C9 H9 125.4 . . ?
C8 C9 C10 109.0(5) . . ?
C10 C9 Fe1 67.4(3) . . ?
C10 C9 H9 125.4 . . ?
Fe1 C10 H10 124.9 . . ?
C6 C10 Fe1 68.3(3) . . ?
C6 C10 H10 124.9 . . ?
C9 C10 Fe1 72.5(3) . . ?
C9 C10 C6 110.1(5) . . ?
C9 C10 H10 124.9 . . ?
C12 C11 N1 108.9(4) . . ?
C16 C11 N1 106.6(4) . . ?
C16 C11 C12 107.9(4) . . ?
C17 C11 N1 110.9(4) . . ?
C17 C11 C12 111.5(4) . . ?
C17 C11 C16 110.8(4) . . ?
C11 C12 H12A 108.5 . . ?
C11 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C13 C12 C11 115.1(4) . . ?
C13 C12 H12A 108.5 . . ?
C13 C12 H12B 108.5 . . ?
C12 C13 H13A 109.8 . . ?
C12 C13 H13B 109.8 . . ?
C12 C13 C14 109.3(4) . . ?
H13A C13 H13B 108.3 . . ?
C14 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
C13 C14 H14A 108.8 . . ?
C13 C14 H14B 108.8 . . ?
C13 C14 C15 113.7(4) . . ?
H14A C14 H14B 107.7 . . ?
C15 C14 H14A 108.8 . . ?
C15 C14 H14B 108.8 . . ?
C14 C15 N1 108.5(4) . . ?
C18 C15 N1 112.2(4) . . ?
C18 C15 C14 111.1(4) . . ?
C18 C15 C19 109.8(4) . . ?
C19 C15 N1 106.9(4) . . ?
C19 C15 C14 108.2(4) . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C11 C17 H17A 109.5 . . ?
C11 C17 H17B 109.5 . . ?
C11 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C19 H19A 109.5 . . ?
C15 C19 H19B 109.5 . . ?
C15 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si1 C20 Fe2 132.3(2) . . ?
C21 C20 Fe2 67.5(3) . . ?
C21 C20 Si1 129.9(4) . . ?
C21 C20 C24 106.3(4) . . ?
C24 C20 Fe2 68.4(3) . . ?
C24 C20 Si1 123.6(4) . . ?
Fe2 C21 H21 124.6 . . ?
C20 C21 Fe2 72.0(3) . . ?
C20 C21 H21 124.6 . . ?
C20 C21 C22 110.8(4) . . ?
C22 C21 Fe2 68.5(3) . . ?
C22 C21 H21 124.6 . . ?
Si2 C22 Fe2 90.8(2) . . ?
C21 C22 Fe2 69.8(3) . . ?
C21 C22 Si2 116.5(4) . . ?
C23 C22 Fe2 69.5(3) . . ?
C23 C22 Si2 123.8(4) . . ?
C23 C22 C21 105.2(4) . . ?
Fe2 C23 H23 125.2 . . ?
C22 C23 Fe2 68.9(3) . . ?
C22 C23 H23 125.2 . . ?
C24 C23 Fe2 70.7(3) . . ?
C24 C23 C22 109.5(4) . . ?
C24 C23 H23 125.2 . . ?
Fe2 C24 H24 125.9 . . ?
C20 C24 Fe2 71.0(3) . . ?
C20 C24 H24 125.9 . . ?
C23 C24 Fe2 68.2(3) . . ?
C23 C24 C20 108.2(4) . . ?
C23 C24 H24 125.9 . . ?
Fe2 C25 H25 125.3 . . ?
C26 C25 Fe2 72.0(3) . . ?
C26 C25 H25 125.3 . . ?
C26 C25 C29 109.5(5) . . ?
C29 C25 Fe2 69.2(3) . . ?
C29 C25 H25 125.3 . . ?
Fe2 C26 H26 125.9 . . ?
C25 C26 Fe2 67.5(3) . . ?
C25 C26 H26 125.9 . . ?
C25 C26 C27 108.2(5) . . ?
C27 C26 Fe2 70.8(3) . . ?
C27 C26 H26 125.9 . . ?
Fe2 C27 H27 128.0 . . ?
C26 C27 Fe2 68.9(3) . . ?
C26 C27 H27 126.6 . . ?
C28 C27 Fe2 68.0(3) . . ?
C28 C27 C26 106.9(5) . . ?
C28 C27 H27 126.6 . . ?
Fe2 C28 H28 124.7 . . ?
C27 C28 Fe2 72.3(3) . . ?
C27 C28 H28 124.7 . . ?
C27 C28 C29 110.6(5) . . ?
C29 C28 Fe2 68.3(3) . . ?
C29 C28 H28 124.7 . . ?
Si2 C29 Fe2 90.7(2) . . ?
C25 C29 Fe2 68.9(3) . . ?
C25 C29 Si2 124.5(4) . . ?
C25 C29 C28 104.9(4) . . ?
C28 C29 Fe2 70.1(3) . . ?
C28 C29 Si2 115.8(4) . . ?
N2 C30 C31 110.4(4) . . ?
N2 C30 C35 109.0(4) . . ?
C31 C30 C35 105.4(4) . . ?
C36 C30 N2 111.8(4) . . ?
C36 C30 C31 109.5(4) . . ?
C36 C30 C35 110.7(5) . . ?
C30 C31 H31A 108.7 . . ?
C30 C31 H31B 108.7 . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 C30 114.4(4) . . ?
C32 C31 H31A 108.7 . . ?
C32 C31 H31B 108.7 . . ?
C31 C32 H32A 110.4 . . ?
C31 C32 H32B 110.4 . . ?
H32A C32 H32B 108.6 . . ?
C33 C32 C31 106.7(4) . . ?
C33 C32 H32A 110.4 . . ?
C33 C32 H32B 110.4 . . ?
C32 C33 H33A 108.9 . . ?
C32 C33 H33B 108.9 . . ?
C32 C33 C34 113.4(4) . . ?
H33A C33 H33B 107.7 . . ?
C34 C33 H33A 108.9 . . ?
C34 C33 H33B 108.9 . . ?
N2 C34 C33 112.6(4) . . ?
N2 C34 C37 112.0(4) . . ?
N2 C34 C38 108.7(4) . . ?
C33 C34 C38 105.0(4) . . ?
C37 C34 C33 109.4(4) . . ?
C37 C34 C38 108.8(4) . . ?
C30 C35 H35A 109.5 . . ?
C30 C35 H35B 109.5 . . ?
C30 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C30 C36 H36A 109.5 . . ?
C30 C36 H36B 109.5 . . ?
C30 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F1 C40 C41 F2 -0.7(7) . . . . ?
F1 C40 C41 C42 178.2(4) . . . . ?
F2 C41 C42 F3 0.3(8) . . . . ?
F2 C41 C42 C43 179.3(5) . . . . ?
F3 C42 C43 F4 0.4(8) . . . . ?
F3 C42 C43 C44 178.9(4) . . . . ?
F4 C43 C44 F5 -1.0(7) . . . . ?
F4 C43 C44 C39 179.7(4) . . . . ?
F6 C46 C47 F7 0.3(6) . . . . ?
F6 C46 C47 C48 -179.9(4) . . . . ?
F7 C47 C48 F8 1.1(7) . . . . ?
F7 C47 C48 C49 -179.0(4) . . . . ?
F8 C48 C49 F9 -0.5(7) . . . . ?
F8 C48 C49 C50 178.4(4) . . . . ?
F9 C49 C50 F10 -1.1(6) . . . . ?
F9 C49 C50 C45 178.6(4) . . . . ?
F11 C52 C53 F12 0.6(6) . . . . ?
F11 C52 C53 C54 178.6(4) . . . . ?
F12 C53 C54 F13 0.1(7) . . . . ?
F12 C53 C54 C55 179.7(4) . . . . ?
F13 C54 C55 F14 -1.3(7) . . . . ?
F13 C54 C55 C56 177.3(4) . . . . ?
F14 C55 C56 F15 1.2(6) . . . . ?
F14 C55 C56 C51 179.7(4) . . . . ?
F16 C58 C59 F17 1.2(7) . . . . ?
F16 C58 C59 C60 -179.0(4) . . . . ?
F17 C59 C60 F18 -0.5(7) . . . . ?
F17 C59 C60 C61 -178.8(4) . . . . ?
F18 C60 C61 F19 -0.3(7) . . . . ?
F18 C60 C61 C62 178.7(4) . . . . ?
F19 C61 C62 F20 -0.9(7) . . . . ?
F19 C61 C62 C57 179.8(4) . . . . ?
C39 C40 C41 F2 179.2(5) . . . . ?
C39 C40 C41 C42 -1.9(8) . . . . ?
C40 C39 C44 F5 178.5(4) . . . . ?
C40 C39 C44 C43 -2.3(7) . . . . ?
C40 C39 B1 C45 172.8(4) . . . . ?
C40 C39 B1 C51 -65.8(5) . . . . ?
C40 C39 B1 C57 56.2(6) . . . . ?
C40 C41 C42 F3 -178.6(4) . . . . ?
C40 C41 C42 C43 0.4(8) . . . . ?
C41 C42 C43 F4 -178.7(5) . . . . ?
C41 C42 C43 C44 -0.1(8) . . . . ?
C42 C43 C44 F5 -179.6(4) . . . . ?
C42 C43 C44 C39 1.2(8) . . . . ?
C44 C39 C40 F1 -177.4(4) . . . . ?
C44 C39 C40 C41 2.7(7) . . . . ?
C44 C39 B1 C45 -16.3(7) . . . . ?
C44 C39 B1 C51 105.0(5) . . . . ?
C44 C39 B1 C57 -132.9(5) . . . . ?
C45 C46 C47 F7 -179.0(4) . . . . ?
C45 C46 C47 C48 0.8(7) . . . . ?
C46 C45 C50 F10 -178.2(4) . . . . ?
C46 C45 C50 C49 2.1(7) . . . . ?
C46 C45 B1 C39 -56.3(6) . . . . ?
C46 C45 B1 C51 -170.4(4) . . . . ?
C46 C45 B1 C57 65.7(5) . . . . ?
C46 C47 C48 F8 -178.7(4) . . . . ?
C46 C47 C48 C49 1.2(7) . . . . ?
C47 C48 C49 F9 179.6(4) . . . . ?
C47 C48 C49 C50 -1.4(7) . . . . ?
C48 C49 C50 F10 179.9(4) . . . . ?
C48 C49 C50 C45 -0.4(7) . . . . ?
C50 C45 C46 F6 178.4(4) . . . . ?
C50 C45 C46 C47 -2.4(7) . . . . ?
C50 C45 B1 C39 129.9(5) . . . . ?
C50 C45 B1 C51 15.7(7) . . . . ?
C50 C45 B1 C57 -108.2(5) . . . . ?
C51 C52 C53 F12 -177.7(4) . . . . ?
C51 C52 C53 C54 0.4(7) . . . . ?
C52 C51 C56 F15 179.1(4) . . . . ?
C52 C51 C56 C55 0.7(7) . . . . ?
C52 C51 B1 C39 -60.5(5) . . . . ?
C52 C51 B1 C45 61.5(5) . . . . ?
C52 C51 B1 C57 178.9(4) . . . . ?
C52 C53 C54 F13 -178.0(4) . . . . ?
C52 C53 C54 C55 1.6(7) . . . . ?
C53 C54 C55 F14 179.2(4) . . . . ?
C53 C54 C55 C56 -2.3(7) . . . . ?
C54 C55 C56 F15 -177.4(4) . . . . ?
C54 C55 C56 C51 1.1(7) . . . . ?
C56 C51 C52 F11 -179.7(4) . . . . ?
C56 C51 C52 C53 -1.5(7) . . . . ?
C56 C51 B1 C39 106.7(5) . . . . ?
C56 C51 B1 C45 -131.2(5) . . . . ?
C56 C51 B1 C57 -13.8(7) . . . . ?
C57 C58 C59 F17 -177.3(4) . . . . ?
C57 C58 C59 C60 2.5(8) . . . . ?
C58 C57 C62 F20 -176.4(4) . . . . ?
C58 C57 C62 C61 2.8(7) . . . . ?
C58 C57 B1 C39 -168.1(4) . . . . ?
C58 C57 B1 C45 68.7(5) . . . . ?
C58 C57 B1 C51 -54.3(6) . . . . ?
C58 C59 C60 F18 179.7(4) . . . . ?
C58 C59 C60 C61 1.5(7) . . . . ?
C59 C60 C61 F19 177.9(4) . . . . ?
C59 C60 C61 C62 -3.0(8) . . . . ?
C60 C61 C62 F20 -179.9(4) . . . . ?
C60 C61 C62 C57 0.8(8) . . . . ?
C62 C57 C58 F16 177.1(4) . . . . ?
C62 C57 C58 C59 -4.5(7) . . . . ?
C62 C57 B1 C39 14.3(7) . . . . ?
C62 C57 B1 C45 -108.8(5) . . . . ?
C62 C57 B1 C51 128.1(5) . . . . ?
B1 C39 C40 F1 -5.3(6) . . . . ?
B1 C39 C40 C41 174.8(5) . . . . ?
B1 C39 C44 F5 7.1(7) . . . . ?
B1 C39 C44 C43 -173.6(5) . . . . ?
B1 C45 C46 F6 3.6(6) . . . . ?
B1 C45 C46 C47 -177.2(4) . . . . ?
B1 C45 C50 F10 -4.0(7) . . . . ?
B1 C45 C50 C49 176.3(4) . . . . ?
B1 C51 C52 F11 -10.6(6) . . . . ?
B1 C51 C52 C53 167.6(4) . . . . ?
B1 C51 C56 F15 11.2(7) . . . . ?
B1 C51 C56 C55 -167.1(4) . . . . ?
B1 C57 C58 F16 -0.8(6) . . . . ?
B1 C57 C58 C59 177.6(4) . . . . ?
B1 C57 C62 F20 1.3(7) . . . . ?
B1 C57 C62 C61 -179.5(4) . . . . ?
Fe1 Si1 C1 C2 66.4(3) . . . . ?
Fe1 Si1 C1 C5 -62.5(4) . . . . ?
Fe1 Si1 C6 C7 -66.0(3) . . . . ?
Fe1 Si1 C6 C10 61.4(4) . . . . ?
Fe1 Si1 C20 Fe2 167.3(2) . . . . ?
Fe1 Si1 C20 C21 -97.6(4) . . . . ?
Fe1 Si1 C20 C24 76.8(4) . . . . ?
Fe1 C1 C2 C3 -60.3(3) . . . . ?
Fe1 C1 C5 C4 60.6(4) . . . . ?
Fe1 C2 C3 C4 -57.6(4) . . . . ?
Fe1 C3 C4 C5 -57.2(4) . . . . ?
Fe1 C4 C5 C1 -58.5(3) . . . . ?
Fe1 C6 C7 C8 59.9(4) . . . . ?
Fe1 C6 C10 C9 -60.6(4) . . . . ?
Fe1 C7 C8 C9 59.3(4) . . . . ?
Fe1 C8 C9 C10 56.3(4) . . . . ?
Fe1 C9 C10 C6 58.1(4) . . . . ?
Fe2 Si2 N2 C30 75.4(4) . . . . ?
Fe2 Si2 N2 C34 -97.0(4) . . . . ?
Fe2 C20 C21 C22 -57.6(3) . . . . ?
Fe2 C20 C24 C23 58.2(3) . . . . ?
Fe2 C21 C22 Si2 80.4(3) . . . . ?
Fe2 C21 C22 C23 -60.8(3) . . . . ?
Fe2 C22 C23 C24 -59.2(4) . . . . ?
Fe2 C23 C24 C20 -59.9(3) . . . . ?
Fe2 C25 C26 C27 59.3(4) . . . . ?
Fe2 C25 C29 Si2 75.6(4) . . . . ?
Fe2 C25 C29 C28 -61.3(3) . . . . ?
Fe2 C26 C27 C28 57.6(4) . . . . ?
Fe2 C27 C28 C29 57.7(4) . . . . ?
Fe2 C28 C29 Si2 -80.8(3) . . . . ?
Fe2 C28 C29 C25 60.5(3) . . . . ?
Si1 N1 C11 C12 -167.5(3) . . . . ?
Si1 N1 C11 C16 -51.3(5) . . . . ?
Si1 N1 C11 C17 69.4(5) . . . . ?
Si1 N1 C15 C14 165.6(3) . . . . ?
Si1 N1 C15 C18 -71.3(4) . . . . ?
Si1 N1 C15 C19 49.1(4) . . . . ?
Si1 C1 C2 Fe1 -76.6(3) . . . . ?
Si1 C1 C2 C3 -136.9(4) . . . . ?
Si1 C1 C5 Fe1 71.5(3) . . . . ?
Si1 C1 C5 C4 132.2(4) . . . . ?
Si1 C6 C7 Fe1 76.9(3) . . . . ?
Si1 C6 C7 C8 136.8(4) . . . . ?
Si1 C6 C10 Fe1 -69.5(4) . . . . ?
Si1 C6 C10 C9 -130.1(4) . . . . ?
Si1 C20 C21 Fe2 -127.2(4) . . . . ?
Si1 C20 C21 C22 175.2(4) . . . . ?
Si1 C20 C24 Fe2 127.4(3) . . . . ?
Si1 C20 C24 C23 -174.4(3) . . . . ?
Si2 N2 C30 C31 152.0(4) . . . . ?
Si2 N2 C30 C35 36.7(5) . . . . ?
Si2 N2 C30 C36 -85.9(5) . . . . ?
Si2 N2 C34 C33 -152.4(3) . . . . ?
Si2 N2 C34 C37 83.8(4) . . . . ?
Si2 N2 C34 C38 -36.4(5) . . . . ?
Si2 C22 C23 Fe2 -76.5(3) . . . . ?
Si2 C22 C23 C24 -135.7(4) . . . . ?
N1 Si1 C1 Fe1 136.98(16) . . . . ?
N1 Si1 C1 C2 -156.6(3) . . . . ?
N1 Si1 C1 C5 74.5(4) . . . . ?
N1 Si1 C6 Fe1 -134.31(17) . . . . ?
N1 Si1 C6 C7 159.7(3) . . . . ?
N1 Si1 C6 C10 -72.9(5) . . . . ?
N1 Si1 C20 Fe2 -11.7(4) . . . . ?
N1 Si1 C20 C21 83.4(5) . . . . ?
N1 Si1 C20 C24 -102.2(4) . . . . ?
N1 C11 C12 C13 -51.2(6) . . . . ?
N2 C30 C31 C32 49.9(6) . . . . ?
C1 Si1 C6 Fe1 -7.9(2) . . . . ?
C1 Si1 C6 C7 -73.9(4) . . . . ?
C1 Si1 C6 C10 53.6(5) . . . . ?
C1 Si1 C20 Fe2 -138.4(3) . . . . ?
C1 Si1 C20 C21 -43.3(5) . . . . ?
C1 Si1 C20 C24 131.1(4) . . . . ?
C1 C2 C3 Fe1 58.0(3) . . . . ?
C1 C2 C3 C4 0.4(6) . . . . ?
C2 C1 C5 Fe1 -61.1(3) . . . . ?
C2 C1 C5 C4 -0.5(5) . . . . ?
C2 C3 C4 Fe1 56.6(4) . . . . ?
C2 C3 C4 C5 -0.7(6) . . . . ?
C3 C4 C5 Fe1 59.2(4) . . . . ?
C3 C4 C5 C1 0.7(6) . . . . ?
C5 C1 C2 Fe1 60.4(3) . . . . ?
C5 C1 C2 C3 0.0(5) . . . . ?
C6 Si1 C1 Fe1 7.9(2) . . . . ?
C6 Si1 C1 C2 74.2(4) . . . . ?
C6 Si1 C1 C5 -54.6(4) . . . . ?
C6 Si1 C20 Fe2 115.5(3) . . . . ?
C6 Si1 C20 C21 -149.4(4) . . . . ?
C6 Si1 C20 C24 25.0(5) . . . . ?
C6 C7 C8 Fe1 -57.6(3) . . . . ?
C6 C7 C8 C9 1.7(6) . . . . ?
C7 C6 C10 Fe1 61.5(3) . . . . ?
C7 C6 C10 C9 0.8(6) . . . . ?
C7 C8 C9 Fe1 -57.4(4) . . . . ?
C7 C8 C9 C10 -1.1(6) . . . . ?
C8 C9 C10 Fe1 -58.0(4) . . . . ?
C8 C9 C10 C6 0.2(6) . . . . ?
C10 C6 C7 Fe1 -61.4(3) . . . . ?
C10 C6 C7 C8 -1.5(5) . . . . ?
C11 N1 C15 C14 -48.9(5) . . . . ?
C11 N1 C15 C18 74.3(5) . . . . ?
C11 N1 C15 C19 -165.3(4) . . . . ?
C11 C12 C13 C14 57.8(6) . . . . ?
C12 C13 C14 C15 -59.4(6) . . . . ?
C13 C14 C15 N1 54.4(5) . . . . ?
C13 C14 C15 C18 -69.4(5) . . . . ?
C13 C14 C15 C19 170.0(4) . . . . ?
C15 N1 C11 C12 46.9(5) . . . . ?
C15 N1 C11 C16 163.1(4) . . . . ?
C15 N1 C11 C17 -76.1(5) . . . . ?
C16 C11 C12 C13 -166.5(4) . . . . ?
C17 C11 C12 C13 71.6(6) . . . . ?
C20 Si1 C1 Fe1 -104.0(2) . . . . ?
C20 Si1 C1 C2 -37.6(4) . . . . ?
C20 Si1 C1 C5 -166.5(4) . . . . ?
C20 Si1 C6 Fe1 110.1(2) . . . . ?
C20 Si1 C6 C7 44.1(4) . . . . ?
C20 Si1 C6 C10 171.6(4) . . . . ?
C20 C21 C22 Fe2 59.7(3) . . . . ?
C20 C21 C22 Si2 140.0(4) . . . . ?
C20 C21 C22 C23 -1.2(5) . . . . ?
C21 C20 C24 Fe2 -57.1(3) . . . . ?
C21 C20 C24 C23 1.1(5) . . . . ?
C21 C22 C23 Fe2 61.0(3) . . . . ?
C21 C22 C23 C24 1.8(5) . . . . ?
C22 Si2 N2 C30 130.2(4) . . . . ?
C22 Si2 N2 C34 -42.2(4) . . . . ?
C22 C23 C24 Fe2 58.1(3) . . . . ?
C22 C23 C24 C20 -1.9(6) . . . . ?
C24 C20 C21 Fe2 57.7(3) . . . . ?
C24 C20 C21 C22 0.1(5) . . . . ?
C25 C26 C27 Fe2 -57.3(4) . . . . ?
C25 C26 C27 C28 0.2(6) . . . . ?
C26 C25 C29 Fe2 61.1(4) . . . . ?
C26 C25 C29 Si2 136.6(4) . . . . ?
C26 C25 C29 C28 -0.2(6) . . . . ?
C26 C27 C28 Fe2 -58.1(4) . . . . ?
C26 C27 C28 C29 -0.4(6) . . . . ?
C27 C28 C29 Fe2 -60.1(4) . . . . ?
C27 C28 C29 Si2 -140.9(4) . . . . ?
C27 C28 C29 C25 0.4(6) . . . . ?
C29 Si2 N2 C30 19.1(5) . . . . ?
C29 Si2 N2 C34 -153.3(3) . . . . ?
C29 C25 C26 Fe2 -59.3(3) . . . . ?
C29 C25 C26 C27 0.0(6) . . . . ?
C30 N2 C34 C33 35.1(6) . . . . ?
C30 N2 C34 C37 -88.7(5) . . . . ?
C30 N2 C34 C38 151.0(4) . . . . ?
C30 C31 C32 C33 -62.2(6) . . . . ?
C31 C32 C33 C34 59.7(6) . . . . ?
C32 C33 C34 N2 -46.9(6) . . . . ?
C32 C33 C34 C37 78.4(6) . . . . ?
C32 C33 C34 C38 -165.0(5) . . . . ?
C34 N2 C30 C31 -35.9(6) . . . . ?
C34 N2 C30 C35 -151.2(4) . . . . ?
C34 N2 C30 C36 86.2(6) . . . . ?
C35 C30 C31 C32 167.4(5) . . . . ?
C36 C30 C31 C32 -73.5(6) . . . . ?
_shelx_res_file
;
TITL testm1 in P2(1)/n
CELL 0.71073 11.5252 26.6215 18.4948 90 91.736 90
ZERR 4 0.0005 0.001 0.0007 0 0.003 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H B F Fe N Si
UNIT 248 212 4 80 8 8 8
L.S. 4
PLAN 5
TEMP -173(2)
MORE -1
BOND $H
CONF
fmap 2
acta 52
SHEL 9999 0.82
REM
REM
REM
WGHT 0.059900 5.488700
FVAR 0.06208
F1 4 0.028254 0.591387 0.161944 11.00000 0.03533 0.04492 =
0.02912 -0.00251 0.00497 -0.00829
F2 4 -0.069895 0.502150 0.138652 11.00000 0.05511 0.06290 =
0.04963 0.01075 0.00025 -0.02904
F3 4 0.034766 0.433121 0.052613 11.00000 0.09462 0.03105 =
0.06388 0.00091 -0.02101 -0.02776
F4 4 0.240521 0.455886 -0.007257 11.00000 0.08329 0.02946 =
0.04243 -0.01345 -0.01283 0.00833
F5 4 0.342354 0.543194 0.016745 11.00000 0.04164 0.03829 =
0.02948 -0.00852 0.00118 0.00633
F6 4 0.433563 0.571779 0.154664 11.00000 0.03535 0.02935 =
0.02981 0.00377 -0.00296 0.00131
F7 4 0.656394 0.582212 0.125674 11.00000 0.03281 0.04669 =
0.04312 -0.00637 -0.00367 0.00991
F8 4 0.724986 0.656448 0.033674 11.00000 0.02876 0.05844 =
0.04738 -0.00993 0.01059 -0.01002
F9 4 0.563617 0.720882 -0.024197 11.00000 0.04559 0.03885 =
0.04010 0.00223 0.01253 -0.01135
F10 4 0.341414 0.711205 0.004425 11.00000 0.04004 0.02986 =
0.03451 0.00738 0.00219 -0.00089
F11 4 0.210482 0.623240 -0.048428 11.00000 0.03801 0.03742 =
0.02382 -0.00452 0.00522 0.00073
F12 4 0.033361 0.655591 -0.131170 11.00000 0.06029 0.05263 =
0.01927 0.00439 -0.00080 -0.00053
F13 4 -0.138165 0.711843 -0.074009 11.00000 0.05135 0.06140 =
0.03550 0.01461 -0.01186 0.01139
F14 4 -0.123088 0.737593 0.069127 11.00000 0.03191 0.03664 =
0.04205 0.00123 -0.00103 0.00935
F15 4 0.048317 0.704233 0.153511 11.00000 0.03052 0.04150 =
0.02414 -0.00936 0.00016 0.00391
F16 4 0.275616 0.730738 0.159365 11.00000 0.03842 0.02720 =
0.02793 0.00003 -0.00020 -0.00165
F17 4 0.279657 0.762694 0.294758 11.00000 0.05770 0.03466 =
0.03623 -0.01427 -0.00873 -0.00205
F18 4 0.261412 0.694952 0.407518 11.00000 0.06421 0.06339 =
0.01976 -0.01167 -0.00112 -0.00504
F19 4 0.242121 0.595718 0.377118 11.00000 0.05212 0.05374 =
0.02151 0.00746 -0.00067 -0.00555
F20 4 0.232019 0.563125 0.242815 11.00000 0.04691 0.02985 =
0.02647 0.00397 -0.00242 -0.00298
C39 1 0.192564 0.572138 0.093268 11.00000 0.02810 0.02543 =
0.02218 0.00056 -0.00381 0.00056
C40 1 0.086300 0.558078 0.120469 11.00000 0.04011 0.03017 =
0.02004 -0.00125 -0.00252 -0.00394
C41 1 0.032609 0.512675 0.109438 11.00000 0.04307 0.04408 =
0.02535 0.00452 -0.00646 -0.01182
C42 1 0.085264 0.478095 0.066471 11.00000 0.06228 0.02739 =
0.03345 0.00922 -0.01797 -0.01544
C43 1 0.188818 0.489184 0.036346 11.00000 0.06663 0.02167 =
0.02636 -0.00711 -0.01421 0.00361
C44 1 0.239733 0.535537 0.049490 11.00000 0.03724 0.03028 =
0.02044 0.00233 -0.00152 0.00203
C45 1 0.374283 0.639696 0.079751 11.00000 0.03077 0.02479 =
0.01976 -0.00329 0.00441 -0.00029
C46 1 0.461634 0.609807 0.108735 11.00000 0.03354 0.02560 =
0.02321 -0.00489 0.00448 -0.00293
C47 1 0.578249 0.614189 0.095010 11.00000 0.03211 0.03208 =
0.02403 -0.00867 -0.00378 0.00422
C48 1 0.612775 0.651252 0.049858 11.00000 0.03159 0.03591 =
0.02970 -0.01100 0.00462 -0.00524
C49 1 0.531354 0.683364 0.020728 11.00000 0.03762 0.02751 =
0.02609 -0.00793 0.00421 -0.00999
C50 1 0.415458 0.677288 0.035994 11.00000 0.03357 0.02604 =
0.02452 -0.00470 -0.00309 0.00288
C51 1 0.141405 0.661769 0.057326 11.00000 0.02541 0.02321 =
0.02490 -0.00378 0.00212 -0.00429
C52 1 0.129957 0.651999 -0.016200 11.00000 0.03205 0.02225 =
0.02468 0.00019 0.00238 -0.00264
C53 1 0.039766 0.668307 -0.060503 11.00000 0.04007 0.03512 =
0.01641 0.00301 0.00123 -0.00823
C54 1 -0.046676 0.696647 -0.031987 11.00000 0.03840 0.03440 =
0.02467 0.01169 -0.00745 -0.00447
C55 1 -0.039299 0.708983 0.039649 11.00000 0.02946 0.02338 =
0.03650 0.00103 0.00253 0.00163
C56 1 0.052336 0.691336 0.082331 11.00000 0.03217 0.02501 =
0.01931 -0.00024 -0.00091 -0.00499
C57 1 0.246922 0.645686 0.192618 11.00000 0.01972 0.03157 =
0.02430 -0.00178 -0.00032 0.00152
C58 1 0.263911 0.695593 0.211732 11.00000 0.02436 0.03155 =
0.02519 -0.00359 -0.00255 -0.00071
C59 1 0.267473 0.713214 0.281588 11.00000 0.03081 0.03287 =
0.02801 -0.00581 -0.00318 -0.00137
C60 1 0.257899 0.679385 0.338035 11.00000 0.03100 0.05246 =
0.01798 -0.01385 -0.00166 0.00055
C61 1 0.247901 0.629509 0.322618 11.00000 0.02954 0.04206 =
0.02509 0.00383 -0.00072 -0.00362
C62 1 0.241978 0.613688 0.251628 11.00000 0.02570 0.03015 =
0.02765 -0.00175 -0.00021 0.00098
B1 3 0.239522 0.630095 0.105986 11.00000 0.03090 0.02262 =
0.01797 -0.00271 0.00305 0.00268
FE1 5 0.892326 0.386911 0.368447 11.00000 0.02785 0.03117 =
0.03020 0.00119 0.00166 0.00140
FE2 5 0.397797 0.406425 0.438731 11.00000 0.02693 0.03843 =
0.02751 0.00100 0.00141 0.00381
SI1 7 0.664699 0.391947 0.342994 11.00000 0.02569 0.02735 =
0.02186 0.00238 0.00295 0.00077
SI2 7 0.311032 0.339861 0.540273 11.00000 0.03382 0.03339 =
0.02911 -0.00391 0.00295 -0.00181
AFIX 13
H2 2 0.306324 0.304979 0.520338 11.00000 -1.20000
AFIX 0
N1 6 0.550520 0.397924 0.265343 11.00000 0.03171 0.02287 =
0.02065 0.00542 -0.00022 -0.00075
AFIX 13
H1 2 0.478531 0.402260 0.293545 11.00000 -1.20000
AFIX 0
N2 6 0.264345 0.338688 0.627156 11.00000 0.02935 0.04133 =
0.02386 -0.00001 0.00407 0.00301
C1 1 0.768039 0.338280 0.337467 11.00000 0.02925 0.02755 =
0.02536 -0.00006 -0.00117 0.00359
C2 1 0.819454 0.322998 0.406472 11.00000 0.03753 0.02919 =
0.03019 0.00273 -0.00458 -0.00470
AFIX 43
H2A 2 0.779519 0.319548 0.450384 11.00000 -1.20000
AFIX 0
C3 1 0.939330 0.314068 0.397412 11.00000 0.03189 0.03381 =
0.05018 0.00194 -0.00952 0.00270
AFIX 43
H3 2 0.992799 0.303438 0.434409 11.00000 -1.20000
AFIX 0
C4 1 0.966751 0.323407 0.325075 11.00000 0.03052 0.04580 =
0.04652 -0.01279 0.00098 0.00248
AFIX 43
H4 2 1.041417 0.320519 0.305078 11.00000 -1.20000
AFIX 0
C5 1 0.863166 0.337909 0.287228 11.00000 0.03397 0.04058 =
0.02858 -0.00718 0.00215 0.00489
AFIX 13
H5 2 0.856560 0.346669 0.234685 11.00000 -1.20000
AFIX 0
C6 1 0.775427 0.442448 0.358717 11.00000 0.02860 0.02410 =
0.03735 0.00265 0.00006 0.00537
C7 1 0.826656 0.441206 0.432121 11.00000 0.03187 0.03834 =
0.03703 -0.00283 -0.00410 0.00027
AFIX 13
H7 2 0.782935 0.435208 0.477201 11.00000 -1.20000
AFIX 0
C8 1 0.949303 0.448458 0.429159 11.00000 0.03473 0.03368 =
0.05386 -0.00579 -0.01324 -0.00179
AFIX 43
H8 2 1.002831 0.448395 0.469244 11.00000 -1.20000
AFIX 0
C9 1 0.976383 0.455658 0.356765 11.00000 0.03036 0.04107 =
0.05914 0.00384 0.00239 -0.00238
AFIX 13
H9 2 1.056301 0.460309 0.338256 11.00000 -1.20000
AFIX 0
C10 1 0.873897 0.452151 0.313644 11.00000 0.03527 0.03848 =
0.04685 0.01226 0.00117 -0.00601
AFIX 13
H10 2 0.869770 0.455262 0.259744 11.00000 -1.20000
AFIX 0
C11 1 0.549314 0.448153 0.221059 11.00000 0.04869 0.02083 =
0.02484 0.00240 -0.00420 -0.00421
C12 1 0.437105 0.450482 0.173864 11.00000 0.06066 0.02576 =
0.02620 0.00560 -0.01304 -0.00225
AFIX 23
H12A 2 0.370829 0.455783 0.205824 11.00000 -1.20000
H12B 2 0.441435 0.480034 0.141564 11.00000 -1.20000
AFIX 0
C13 1 0.412833 0.404541 0.128078 11.00000 0.05269 0.03570 =
0.03009 0.00206 -0.01325 0.00343
AFIX 23
H13A 2 0.475185 0.400092 0.092979 11.00000 -1.20000
H13B 2 0.338337 0.408735 0.100676 11.00000 -1.20000
AFIX 0
C14 1 0.406781 0.358542 0.176828 11.00000 0.03939 0.03176 =
0.02859 -0.00365 -0.00761 -0.00274
AFIX 23
H14A 2 0.389626 0.328653 0.146502 11.00000 -1.20000
H14B 2 0.341801 0.362886 0.210069 11.00000 -1.20000
AFIX 0
C15 1 0.518827 0.348910 0.221788 11.00000 0.03426 0.02443 =
0.02757 -0.00099 -0.00123 -0.00383
C16 1 0.545370 0.491120 0.276543 11.00000 0.05189 0.02135 =
0.03131 -0.00059 -0.01337 0.00419
AFIX 137
H16A 2 0.485552 0.483973 0.311659 11.00000 -1.50000
H16B 2 0.526996 0.522709 0.251515 11.00000 -1.50000
H16C 2 0.621048 0.494049 0.301803 11.00000 -1.50000
AFIX 0
C17 1 0.655982 0.452322 0.175759 11.00000 0.06499 0.03729 =
0.03096 0.00947 0.00685 -0.00511
AFIX 137
H17A 2 0.721260 0.435238 0.200438 11.00000 -1.50000
H17B 2 0.675285 0.487827 0.168959 11.00000 -1.50000
H17C 2 0.640510 0.436603 0.128532 11.00000 -1.50000
AFIX 0
C18 1 0.616502 0.332124 0.173973 11.00000 0.04494 0.03456 =
0.02767 -0.00411 0.00158 0.00011
AFIX 137
H18A 2 0.635190 0.359215 0.140390 11.00000 -1.50000
H18B 2 0.592012 0.302280 0.146498 11.00000 -1.50000
H18C 2 0.685295 0.324052 0.204197 11.00000 -1.50000
AFIX 0
C19 1 0.494177 0.308077 0.277432 11.00000 0.03494 0.03275 =
0.03021 0.00136 -0.00075 -0.00236
AFIX 137
H19A 2 0.566378 0.299182 0.303721 11.00000 -1.50000
H19B 2 0.462734 0.278299 0.252611 11.00000 -1.50000
H19C 2 0.437625 0.320585 0.311617 11.00000 -1.50000
AFIX 0
C20 1 0.573309 0.390901 0.424317 11.00000 0.02669 0.03261 =
0.02245 0.00366 -0.00411 0.00312
C21 1 0.513894 0.350082 0.456818 11.00000 0.03020 0.03304 =
0.02220 0.00365 -0.00107 0.00183
AFIX 13
H21 2 0.506863 0.315618 0.435629 11.00000 -1.20000
AFIX 0
C22 1 0.461441 0.365831 0.522821 11.00000 0.02890 0.03644 =
0.02255 0.00143 0.00160 0.00143
C23 1 0.492285 0.417751 0.531178 11.00000 0.03059 0.04486 =
0.02701 -0.00682 0.00273 0.00199
AFIX 13
H23 2 0.469092 0.439841 0.572017 11.00000 -1.20000
AFIX 0
C24 1 0.558237 0.433485 0.470846 11.00000 0.02849 0.03609 =
0.02755 -0.00055 -0.00252 0.00447
AFIX 13
H24 2 0.587821 0.468221 0.462241 11.00000 -1.20000
AFIX 0
C25 1 0.251346 0.438213 0.473590 11.00000 0.02800 0.05258 =
0.03520 0.00221 0.00364 0.00903
AFIX 13
H25 2 0.245640 0.459433 0.517955 11.00000 -1.20000
AFIX 0
C26 1 0.270735 0.456446 0.403354 11.00000 0.02983 0.05250 =
0.04208 0.00703 0.00284 0.00642
AFIX 13
H26 2 0.283393 0.492370 0.389896 11.00000 -1.20000
AFIX 0
C27 1 0.272611 0.414319 0.354914 11.00000 0.02815 0.05297 =
0.03288 0.01226 -0.00387 0.00912
AFIX 43
H27 2 0.284342 0.415416 0.304317 11.00000 -1.20000
AFIX 0
C28 1 0.253796 0.371223 0.396638 11.00000 0.02976 0.05150 =
0.03206 0.00069 -0.00194 0.00087
AFIX 13
H28 2 0.252465 0.336125 0.377362 11.00000 -1.20000
AFIX 0
C29 1 0.240503 0.384379 0.471457 11.00000 0.02167 0.04181 =
0.03329 0.00033 -0.00384 0.00225
C30 1 0.147183 0.359166 0.647692 11.00000 0.03835 0.03756 =
0.03150 -0.00305 0.00706 0.00020
C31 1 0.103330 0.331709 0.714166 11.00000 0.03528 0.05000 =
0.03117 0.00346 0.00744 -0.00339
AFIX 23
H31A 2 0.033092 0.349109 0.730841 11.00000 -1.20000
H31B 2 0.080285 0.297215 0.699798 11.00000 -1.20000
AFIX 0
C32 1 0.191289 0.328493 0.777086 11.00000 0.04224 0.05520 =
0.03137 0.00029 0.00826 -0.00048
AFIX 23
H32A 2 0.216620 0.362539 0.792220 11.00000 -1.20000
H32B 2 0.156712 0.311522 0.818914 11.00000 -1.20000
AFIX 0
C33 1 0.293746 0.298419 0.750358 11.00000 0.04219 0.04596 =
0.03363 0.00756 0.00001 -0.00383
AFIX 23
H33A 2 0.266783 0.264265 0.736952 11.00000 -1.20000
H33B 2 0.352302 0.295008 0.790334 11.00000 -1.20000
AFIX 0
C34 1 0.351397 0.322277 0.685143 11.00000 0.03833 0.03607 =
0.02528 -0.00485 0.00177 -0.00145
C35 1 0.058341 0.347617 0.586799 11.00000 0.02955 0.08881 =
0.03402 0.00248 0.00212 0.00068
AFIX 137
H35A 2 0.076132 0.367593 0.544029 11.00000 -1.50000
H35B 2 -0.019660 0.356048 0.602644 11.00000 -1.50000
H35C 2 0.061653 0.311811 0.574725 11.00000 -1.50000
AFIX 0
C36 1 0.152097 0.414960 0.662726 11.00000 0.06349 0.04830 =
0.05781 0.00046 0.02786 0.00684
AFIX 137
H36A 2 0.198393 0.421053 0.707180 11.00000 -1.50000
H36B 2 0.073242 0.427806 0.668540 11.00000 -1.50000
H36C 2 0.187841 0.432185 0.622203 11.00000 -1.50000
AFIX 0
C37 1 0.429103 0.365389 0.710767 11.00000 0.04385 0.04826 =
0.03160 0.00133 -0.00185 -0.00446
AFIX 137
H37A 2 0.468607 0.379732 0.669370 11.00000 -1.50000
H37B 2 0.486952 0.352840 0.746256 11.00000 -1.50000
H37C 2 0.381767 0.391344 0.733169 11.00000 -1.50000
AFIX 0
C38 1 0.428180 0.280292 0.654060 11.00000 0.04881 0.04169 =
0.04000 0.00564 0.00351 0.00749
AFIX 137
H38A 2 0.378598 0.253676 0.633473 11.00000 -1.50000
H38B 2 0.478266 0.266317 0.692819 11.00000 -1.50000
H38C 2 0.476313 0.294288 0.616200 11.00000 -1.50000
AFIX 0
HKLF 4
REM testm1 in P2(1)/n
REM R1 = 0.0555 for 6230 Fo > 4sig(Fo) and 0.1208 for all 10766 data
REM 810 parameters refined using 0 restraints
END
WGHT 0.0598 5.5111
REM Highest difference peak 1.322, deepest hole -0.745, 1-sigma level 0.087
Q1 1 0.3858 0.3684 0.4190 11.00000 0.05 1.32
Q2 1 0.3261 0.4005 0.5612 11.00000 0.05 0.97
Q3 1 0.2563 0.3647 0.4983 11.00000 0.05 0.36
Q4 1 0.4232 0.4530 0.4382 11.00000 0.05 0.35
Q5 1 0.3152 0.2882 0.4968 11.00000 0.05 0.31
;
_shelx_res_checksum 592
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_testo1
_database_code_depnum_ccdc_archive 'CCDC 1589410'
_audit_update_record
;
2017-12-05 deposited with the CCDC.
2018-01-23 downloaded from the CCDC.
;
_audit_creation_date 2016-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number 2013-4
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C12 H18 Fe N6, 2(B C24 F20)'
_chemical_formula_sum 'C60 H18 B2 F40 Fe N6'
_chemical_formula_weight 1660.27
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
_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 62
_space_group_name_H-M_alt 'P n m a'
_space_group_name_Hall '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
_cell_length_a 17.9405(3)
_cell_length_b 24.5421(4)
_cell_length_c 14.0694(2)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 6194.72(17)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9979
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 26.59
_cell_measurement_theta_min 2.48
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.412
_exptl_absorpt_correction_T_max 0.7454
_exptl_absorpt_correction_T_min 0.6756
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0500 before and 0.0427 after correction.
The Ratio of minimum to maximum transmission is 0.9064.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour orange
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.780
_exptl_crystal_density_meas .
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 3264
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.33
_exptl_crystal_size_min 0.31
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0328
_diffrn_reflns_av_unetI/netI 0.0190
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -31
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 48712
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 26.764
_diffrn_reflns_theta_min 1.659
_diffrn_ambient_temperature 100(2)
_diffrn_detector 'Bruker area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type 'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5713
_reflns_number_total 6747
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.27A (Bruker, 2012)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max 0.295
_refine_diff_density_min -0.297
_refine_diff_density_rms 0.044
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.038
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 516
_refine_ls_number_reflns 6747
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0388
_refine_ls_R_factor_gt 0.0298
_refine_ls_restrained_S_all 1.038
_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^)+(0.0283P)^2^+3.7220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0673
_refine_ls_wR_factor_ref 0.0713
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.5 times of:
All C(H,H,H) groups
2. Others
Fixed Sof: H22A(0.5) H22B(0.5) H22C(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
H25D(0.5) H25E(0.5) H25F(0.5) H8A(0.5) H8B(0.5) H8C(0.5)
3.a Idealised Me refined as rotating group:
C93(H93A,H93B,H93C), C224(H22A,H22B,H22C), C250(H25A,H25B,H25C), C255(H25D,
H25E,H25F), C8(H8A,H8B,H8C)
;
_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
Fe2 Fe 0.06061(2) 0.2500 0.64038(2) 0.02089(8) Uani 1 2 d S T P . .
F8 F 0.24054(5) 0.66511(4) 0.68991(7) 0.0237(2) Uani 1 1 d . . . . .
F13 F 0.05450(5) 0.62006(4) 0.90906(7) 0.0266(2) Uani 1 1 d . . . . .
F21 F 0.34080(5) 0.50783(4) 0.82106(6) 0.0247(2) Uani 1 1 d . . . . .
F29 F 0.15476(5) 0.60343(4) 0.54056(6) 0.0255(2) Uani 1 1 d . . . . .
F41 F 0.41433(5) 0.56988(4) 0.51827(6) 0.0229(2) Uani 1 1 d . . . . .
F45 F 0.28171(6) 0.63672(4) 0.25708(7) 0.0301(2) Uani 1 1 d . . . . .
F53 F 0.18278(5) 0.48020(4) 0.75374(7) 0.0248(2) Uani 1 1 d . . . . .
F58 F 0.44517(5) 0.54342(4) 0.94066(6) 0.0312(2) Uani 1 1 d . . . . .
F68 F 0.42651(5) 0.48032(4) 0.66574(6) 0.0241(2) Uani 1 1 d . . . . .
F78 F 0.17722(5) 0.49144(4) 0.55698(6) 0.0231(2) Uani 1 1 d . . . . .
F84 F 0.51658(6) 0.63942(5) 0.90728(8) 0.0385(3) Uani 1 1 d . . . . .
F95 F 0.41277(5) 0.60777(4) 0.34049(7) 0.0282(2) Uani 1 1 d . . . . .
F10 F 0.18507(5) 0.38773(4) 0.50008(7) 0.0294(2) Uani 1 1 d . . . . .
F11 F 0.13794(5) 0.69570(4) 0.81480(7) 0.0281(2) Uani 1 1 d . . . . .
F1 F 0.07901(5) 0.51211(4) 0.87478(7) 0.0283(2) Uani 1 1 d . . . . .
F12 F 0.31102(6) 0.32848(4) 0.53039(7) 0.0304(2) Uani 1 1 d . . . . .
F2 F 0.38587(5) 0.66132(4) 0.62354(7) 0.0260(2) Uani 1 1 d . . . . .
F3 F 0.42973(5) 0.37627(4) 0.61765(7) 0.0294(2) Uani 1 1 d . . . . .
F15 F 0.15374(5) 0.63488(4) 0.36081(7) 0.0307(2) Uani 1 1 d . . . . .
F4 F 0.48519(5) 0.69633(4) 0.74640(8) 0.0367(3) Uani 1 1 d . . . . .
N4 N -0.04831(11) 0.2500 0.57159(14) 0.0254(4) Uani 1 2 d S T P . .
N6 N 0.10806(11) 0.2500 0.49812(15) 0.0266(4) Uani 1 2 d S T P . .
N10 N 0.17495(11) 0.2500 0.68747(15) 0.0282(5) Uani 1 2 d S T P . .
N14 N 0.05199(8) 0.33619(6) 0.64024(10) 0.0252(3) Uani 1 1 d . . . . .
N24 N 0.02330(12) 0.2500 0.78823(15) 0.0297(5) Uani 1 2 d S T P . .
C29 C 0.10632(8) 0.60413(7) 0.84593(11) 0.0205(3) Uani 1 1 d . . . . .
C40 C 0.28545(8) 0.58548(6) 0.54045(11) 0.0182(3) Uani 1 1 d . . . . .
C41 C 0.22114(8) 0.60271(6) 0.49484(11) 0.0203(3) Uani 1 1 d . . . . .
C51 C 0.21779(8) 0.57089(6) 0.71378(10) 0.0176(3) Uani 1 1 d . . . . .
C62 C 0.14831(8) 0.64237(6) 0.79829(11) 0.0204(3) Uani 1 1 d . . . . .
C64 C 0.20159(8) 0.62510(6) 0.73437(11) 0.0194(3) Uani 1 1 d . . . . .
C76 C 0.17381(8) 0.53462(6) 0.76445(11) 0.0187(3) Uani 1 1 d . . . . .
C89 C 0.46648(9) 0.62040(7) 0.84461(12) 0.0266(4) Uani 1 1 d . . . . .
C93 C 0.01558(10) 0.43809(7) 0.64995(12) 0.0274(4) Uani 1 1 d . . . . .
H93A H -0.0295 0.4441 0.6146 0.041 Uiso 1 1 calc GR . . . .
H93B H 0.0548 0.4601 0.6239 0.041 Uiso 1 1 calc GR . . . .
H93C H 0.0077 0.4478 0.7153 0.041 Uiso 1 1 calc GR . . . .
C97 C 0.11911(8) 0.54995(7) 0.82881(11) 0.0206(3) Uani 1 1 d . . . . .
C101 C 0.24418(9) 0.41122(7) 0.54277(11) 0.0215(3) Uani 1 1 d . . . . .
C105 C 0.34872(8) 0.58734(6) 0.48312(11) 0.0188(3) Uani 1 1 d . . . . .
C127 C 0.42975(9) 0.57216(7) 0.86155(11) 0.0238(3) Uani 1 1 d . . . . .
C131 C 0.37687(8) 0.55447(7) 0.79757(11) 0.0207(3) Uani 1 1 d . . . . .
C135 C 0.30767(9) 0.38107(6) 0.55805(11) 0.0224(3) Uani 1 1 d . . . . .
C149 C 0.03639(9) 0.38099(7) 0.64393(11) 0.0215(3) Uani 1 1 d . . . . .
C154 C 0.45027(9) 0.64880(7) 0.76343(13) 0.0259(4) Uani 1 1 d . . . . .
C156 C 0.29990(8) 0.49167(6) 0.61861(10) 0.0176(3) Uani 1 1 d . . . . .
C163 C 0.21894(9) 0.62002(6) 0.40138(12) 0.0225(3) Uani 1 1 d . . . . .
C179 C 0.39789(8) 0.62919(7) 0.70006(11) 0.0214(3) Uani 1 1 d . . . . .
C185 C 0.35918(8) 0.58082(6) 0.71295(11) 0.0191(3) Uani 1 1 d . . . . .
C193 C 0.28331(9) 0.62159(6) 0.34906(11) 0.0223(3) Uani 1 1 d . . . . .
C204 C 0.23697(14) 0.2500 0.70323(17) 0.0259(5) Uani 1 2 d S T P . .
C205 C 0.24166(8) 0.46456(6) 0.57294(11) 0.0191(3) Uani 1 1 d . . . . .
C211 C 0.01291(15) 0.2500 0.86811(18) 0.0322(6) Uani 1 2 d S T P . .
C222 C -0.08804(14) 0.2500 0.50940(18) 0.0264(5) Uani 1 2 d S T P . .
C224 C -0.00051(19) 0.2500 0.97036(19) 0.0507(8) Uani 1 2 d S T P . .
H22A H 0.0004 0.2868 0.9936 0.076 Uiso 0.5 1 calc GR . . A -1
H22B H 0.0376 0.2291 1.0015 0.076 Uiso 0.5 1 calc GR . . A -1
H22C H -0.0484 0.2341 0.9832 0.076 Uiso 0.5 1 calc GR . . A -1
C232 C 0.36324(8) 0.45965(7) 0.62815(10) 0.0196(3) Uani 1 1 d . . . . .
C237 C 0.36761(9) 0.40545(7) 0.60137(11) 0.0218(3) Uani 1 1 d . . . . .
C245 C 0.34927(9) 0.60592(6) 0.39074(11) 0.0214(3) Uani 1 1 d . . . . .
C250 C 0.18654(16) 0.2500 0.3448(2) 0.0537(9) Uani 1 2 d S T P . .
H25A H 0.1961 0.2869 0.3256 0.081 Uiso 0.5 1 calc GR . . B -1
H25B H 0.1601 0.2313 0.2952 0.081 Uiso 0.5 1 calc GR . . B -1
H25C H 0.2330 0.2318 0.3567 0.081 Uiso 0.5 1 calc GR . . B -1
C255 C 0.31663(14) 0.2500 0.7237(2) 0.0330(6) Uani 1 2 d S T P . .
H25D H 0.3428 0.2320 0.6732 0.049 Uiso 0.5 1 calc GR . . C -1
H25E H 0.3255 0.2312 0.7824 0.049 Uiso 0.5 1 calc GR . . C -1
H25F H 0.3340 0.2869 0.7290 0.049 Uiso 0.5 1 calc GR . . C -1
C1 C 0.14207(13) 0.2500 0.43051(18) 0.0270(5) Uani 1 2 d S T P . .
C8 C -0.13754(19) 0.2500 0.4276(2) 0.0506(8) Uani 1 2 d S T P . .
H8A H -0.1802 0.2724 0.4409 0.076 Uiso 0.5 1 calc GR . . D -1
H8B H -0.1535 0.2134 0.4146 0.076 Uiso 0.5 1 calc GR . . D -1
H8C H -0.1116 0.2642 0.3733 0.076 Uiso 0.5 1 calc GR . . D -1
B13 B 0.29058(9) 0.55692(7) 0.64608(12) 0.0177(3) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe2 0.02070(16) 0.02150(17) 0.02047(16) 0.000 -0.00331(13) 0.000
F8 0.0214(4) 0.0188(5) 0.0309(5) 0.0033(4) 0.0030(4) -0.0021(4)
F13 0.0208(5) 0.0343(5) 0.0247(5) -0.0030(4) 0.0060(4) 0.0042(4)
F21 0.0259(5) 0.0277(5) 0.0205(4) 0.0044(4) -0.0011(4) -0.0019(4)
F29 0.0164(4) 0.0347(5) 0.0254(5) 0.0047(4) 0.0012(4) 0.0039(4)
F41 0.0156(4) 0.0305(5) 0.0227(5) 0.0015(4) 0.0001(3) 0.0009(4)
F45 0.0415(6) 0.0300(5) 0.0188(5) 0.0090(4) 0.0004(4) 0.0018(5)
F53 0.0277(5) 0.0183(5) 0.0284(5) 0.0026(4) 0.0081(4) -0.0007(4)
F58 0.0290(5) 0.0441(6) 0.0204(5) -0.0034(4) -0.0064(4) 0.0100(5)
F68 0.0159(4) 0.0293(5) 0.0272(5) -0.0018(4) -0.0046(4) 0.0012(4)
F78 0.0152(4) 0.0250(5) 0.0291(5) 0.0003(4) -0.0041(4) 0.0008(4)
F84 0.0254(5) 0.0460(6) 0.0442(6) -0.0186(5) -0.0149(5) 0.0022(5)
F95 0.0259(5) 0.0344(6) 0.0243(5) 0.0045(4) 0.0081(4) -0.0042(4)
F10 0.0248(5) 0.0266(5) 0.0368(6) -0.0042(4) -0.0063(4) -0.0059(4)
F11 0.0254(5) 0.0210(5) 0.0379(6) -0.0052(4) 0.0025(4) 0.0024(4)
F1 0.0262(5) 0.0283(5) 0.0304(5) 0.0055(4) 0.0109(4) -0.0028(4)
F12 0.0366(6) 0.0193(5) 0.0354(5) -0.0035(4) 0.0005(4) 0.0017(4)
F2 0.0243(5) 0.0223(5) 0.0312(5) 0.0037(4) 0.0008(4) -0.0047(4)
F3 0.0255(5) 0.0298(5) 0.0329(5) 0.0001(4) -0.0029(4) 0.0113(4)
F15 0.0270(5) 0.0358(6) 0.0292(5) 0.0083(4) -0.0067(4) 0.0081(4)
F4 0.0260(5) 0.0279(5) 0.0563(7) -0.0074(5) -0.0025(5) -0.0095(4)
N4 0.0227(10) 0.0283(11) 0.0253(10) 0.000 -0.0035(8) 0.000
N6 0.0247(10) 0.0259(11) 0.0291(11) 0.000 0.0016(9) 0.000
N10 0.0274(11) 0.0220(10) 0.0353(12) 0.000 -0.0077(9) 0.000
N14 0.0265(7) 0.0257(8) 0.0234(7) -0.0017(6) -0.0036(6) 0.0007(6)
N24 0.0333(11) 0.0311(12) 0.0247(11) 0.000 -0.0036(9) 0.000
C29 0.0142(7) 0.0286(8) 0.0186(7) -0.0017(6) 0.0003(6) 0.0028(6)
C40 0.0181(7) 0.0164(7) 0.0202(7) 0.0005(6) -0.0005(6) -0.0016(6)
C41 0.0188(7) 0.0190(8) 0.0230(8) 0.0009(6) 0.0021(6) -0.0010(6)
C51 0.0153(7) 0.0213(8) 0.0163(7) 0.0016(6) -0.0025(6) -0.0002(6)
C62 0.0184(7) 0.0196(8) 0.0234(8) -0.0026(6) -0.0037(6) 0.0014(6)
C64 0.0161(7) 0.0204(8) 0.0216(8) 0.0029(6) -0.0023(6) -0.0037(6)
C76 0.0180(7) 0.0178(7) 0.0202(7) 0.0011(6) -0.0013(6) 0.0005(6)
C89 0.0150(7) 0.0345(10) 0.0305(9) -0.0146(8) -0.0061(6) 0.0035(7)
C93 0.0306(9) 0.0248(9) 0.0267(8) 0.0030(7) 0.0063(7) 0.0048(7)
C97 0.0170(7) 0.0257(8) 0.0192(7) 0.0033(6) 0.0006(6) -0.0027(6)
C101 0.0191(8) 0.0257(8) 0.0197(8) 0.0006(6) -0.0004(6) -0.0056(6)
C105 0.0170(7) 0.0185(7) 0.0211(7) -0.0001(6) -0.0016(6) -0.0017(6)
C127 0.0196(8) 0.0322(9) 0.0197(8) -0.0035(7) -0.0022(6) 0.0090(7)
C131 0.0177(7) 0.0235(8) 0.0210(7) -0.0027(6) 0.0024(6) 0.0005(6)
C135 0.0287(8) 0.0177(8) 0.0208(8) 0.0000(6) 0.0039(6) 0.0002(7)
C149 0.0196(7) 0.0288(9) 0.0161(7) 0.0005(7) -0.0002(6) -0.0012(7)
C154 0.0170(7) 0.0227(8) 0.0380(10) -0.0085(7) 0.0037(7) -0.0019(6)
C156 0.0171(7) 0.0207(8) 0.0150(7) 0.0030(6) 0.0019(6) -0.0012(6)
C163 0.0231(8) 0.0198(8) 0.0247(8) 0.0033(7) -0.0057(6) 0.0031(6)
C179 0.0160(7) 0.0239(8) 0.0243(8) -0.0010(7) 0.0010(6) 0.0016(6)
C185 0.0140(7) 0.0229(8) 0.0204(7) -0.0024(6) 0.0017(6) 0.0011(6)
C193 0.0320(9) 0.0178(8) 0.0172(7) 0.0043(6) -0.0008(6) -0.0009(7)
C204 0.0302(13) 0.0172(11) 0.0302(12) 0.000 -0.0062(10) 0.000
C205 0.0160(7) 0.0219(8) 0.0195(7) 0.0033(6) 0.0015(6) 0.0011(6)
C211 0.0334(14) 0.0352(14) 0.0281(14) 0.000 -0.0036(11) 0.000
C222 0.0280(12) 0.0195(12) 0.0316(13) 0.000 -0.0042(10) 0.000
C224 0.0570(19) 0.071(2) 0.0238(14) 0.000 0.0015(13) 0.000
C232 0.0170(7) 0.0254(8) 0.0162(7) 0.0026(6) -0.0008(6) -0.0013(6)
C237 0.0195(8) 0.0256(8) 0.0204(7) 0.0033(7) 0.0017(6) 0.0056(6)
C245 0.0228(8) 0.0192(8) 0.0222(8) -0.0001(6) 0.0057(6) -0.0039(6)
C250 0.0295(15) 0.094(3) 0.0375(16) 0.000 0.0126(12) 0.000
C255 0.0274(13) 0.0298(13) 0.0418(15) 0.000 -0.0112(11) 0.000
C1 0.0211(11) 0.0279(13) 0.0319(13) 0.000 -0.0006(10) 0.000
C8 0.059(2) 0.0424(17) 0.0509(18) 0.000 -0.0336(16) 0.000
B13 0.0137(7) 0.0208(9) 0.0186(8) 0.0020(7) 0.0007(6) -0.0017(7)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe2 N4 2.1805(19) . ?
Fe2 N6 2.175(2) . ?
Fe2 N10 2.156(2) . ?
Fe2 N14 2.1210(14) 8_565 ?
Fe2 N14 2.1210(14) . ?
Fe2 N24 2.185(2) . ?
F8 C64 1.3579(17) . ?
F13 C29 1.3438(17) . ?
F21 C131 1.3557(18) . ?
F29 C41 1.3538(17) . ?
F41 C105 1.3467(17) . ?
F45 C193 1.3467(17) . ?
F53 C76 1.3535(18) . ?
F58 C127 1.3465(19) . ?
F68 C232 1.3512(17) . ?
F78 C205 1.3498(17) . ?
F84 C89 1.3428(18) . ?
F95 C245 1.3415(17) . ?
F10 C101 1.3482(18) . ?
F11 C62 1.3422(18) . ?
F1 C97 1.3409(18) . ?
F12 C135 1.3496(18) . ?
F2 C179 1.3517(18) . ?
F3 C237 1.3443(18) . ?
F15 C163 1.3517(18) . ?
F4 C154 1.3454(19) . ?
N4 C222 1.129(3) . ?
N6 C1 1.130(3) . ?
N10 C204 1.135(3) . ?
N14 C149 1.136(2) . ?
N24 C211 1.139(3) . ?
C29 C62 1.378(2) . ?
C29 C97 1.371(2) . ?
C40 C41 1.386(2) . ?
C40 C105 1.393(2) . ?
C40 B13 1.646(2) . ?
C41 C163 1.382(2) . ?
C51 C64 1.392(2) . ?
C51 C76 1.387(2) . ?
C51 B13 1.652(2) . ?
C62 C64 1.379(2) . ?
C76 C97 1.387(2) . ?
C89 C127 1.376(2) . ?
C89 C154 1.369(3) . ?
C93 H93A 0.9600 . ?
C93 H93B 0.9600 . ?
C93 H93C 0.9600 . ?
C93 C149 1.453(2) . ?
C101 C135 1.375(2) . ?
C101 C205 1.377(2) . ?
C105 C245 1.377(2) . ?
C127 C131 1.378(2) . ?
C131 C185 1.392(2) . ?
C135 C237 1.373(2) . ?
C154 C179 1.382(2) . ?
C156 C205 1.395(2) . ?
C156 C232 1.388(2) . ?
C156 B13 1.656(2) . ?
C163 C193 1.370(2) . ?
C179 C185 1.387(2) . ?
C185 B13 1.656(2) . ?
C193 C245 1.375(2) . ?
C204 C255 1.458(3) . ?
C211 C224 1.459(4) . ?
C222 C8 1.453(4) . ?
C224 H22A 0.9600 . ?
C224 H22B 0.9600 . ?
C224 H22C 0.9600 . ?
C232 C237 1.385(2) . ?
C250 H25A 0.9600 . ?
C250 H25B 0.9600 . ?
C250 H25C 0.9600 . ?
C250 C1 1.446(4) . ?
C255 H25D 0.9600 . ?
C255 H25E 0.9600 . ?
C255 H25F 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 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
N4 Fe2 N24 98.51(8) . . ?
N6 Fe2 N4 86.69(8) . . ?
N6 Fe2 N24 174.80(8) . . ?
N10 Fe2 N4 171.55(8) . . ?
N10 Fe2 N6 84.86(8) . . ?
N10 Fe2 N24 89.94(8) . . ?
N14 Fe2 N4 86.23(4) 8_565 . ?
N14 Fe2 N4 86.23(4) . . ?
N14 Fe2 N6 91.59(4) 8_565 . ?
N14 Fe2 N6 91.59(4) . . ?
N14 Fe2 N10 93.99(4) 8_565 . ?
N14 Fe2 N10 93.99(4) . . ?
N14 Fe2 N14 171.64(8) 8_565 . ?
N14 Fe2 N24 88.77(4) 8_565 . ?
N14 Fe2 N24 88.77(4) . . ?
C222 N4 Fe2 155.5(2) . . ?
C1 N6 Fe2 170.37(19) . . ?
C204 N10 Fe2 173.4(2) . . ?
C149 N14 Fe2 169.55(14) . . ?
C211 N24 Fe2 171.6(2) . . ?
F13 C29 C62 120.11(14) . . ?
F13 C29 C97 120.95(14) . . ?
C97 C29 C62 118.94(14) . . ?
C41 C40 C105 113.58(14) . . ?
C41 C40 B13 126.47(13) . . ?
C105 C40 B13 119.42(13) . . ?
F29 C41 C40 121.08(13) . . ?
F29 C41 C163 115.02(13) . . ?
C163 C41 C40 123.90(14) . . ?
C64 C51 B13 118.89(13) . . ?
C76 C51 C64 112.81(13) . . ?
C76 C51 B13 127.80(14) . . ?
F11 C62 C29 120.29(14) . . ?
F11 C62 C64 120.57(14) . . ?
C29 C62 C64 119.13(14) . . ?
F8 C64 C51 119.19(13) . . ?
F8 C64 C62 115.77(14) . . ?
C62 C64 C51 125.04(14) . . ?
F53 C76 C51 120.56(13) . . ?
F53 C76 C97 115.11(13) . . ?
C51 C76 C97 124.33(14) . . ?
F84 C89 C127 120.40(16) . . ?
F84 C89 C154 120.86(16) . . ?
C154 C89 C127 118.74(15) . . ?
H93A C93 H93B 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
C149 C93 H93A 109.5 . . ?
C149 C93 H93B 109.5 . . ?
C149 C93 H93C 109.5 . . ?
F1 C97 C29 119.81(14) . . ?
F1 C97 C76 120.44(14) . . ?
C29 C97 C76 119.75(14) . . ?
F10 C101 C135 119.41(14) . . ?
F10 C101 C205 121.21(14) . . ?
C135 C101 C205 119.37(14) . . ?
F41 C105 C40 119.28(13) . . ?
F41 C105 C245 116.46(13) . . ?
C245 C105 C40 124.26(14) . . ?
F58 C127 C89 119.71(14) . . ?
F58 C127 C131 121.08(15) . . ?
C89 C127 C131 119.20(15) . . ?
F21 C131 C127 115.82(14) . . ?
F21 C131 C185 119.47(13) . . ?
C127 C131 C185 124.71(15) . . ?
F12 C135 C101 120.43(15) . . ?
F12 C135 C237 120.65(14) . . ?
C237 C135 C101 118.93(15) . . ?
N14 C149 C93 179.04(19) . . ?
F4 C154 C89 119.41(15) . . ?
F4 C154 C179 120.24(16) . . ?
C89 C154 C179 120.35(15) . . ?
C205 C156 B13 119.54(13) . . ?
C232 C156 C205 112.81(14) . . ?
C232 C156 B13 127.41(13) . . ?
F15 C163 C41 120.62(14) . . ?
F15 C163 C193 119.66(14) . . ?
C193 C163 C41 119.72(14) . . ?
F2 C179 C154 114.78(14) . . ?
F2 C179 C185 121.56(14) . . ?
C154 C179 C185 123.65(15) . . ?
C131 C185 B13 119.40(13) . . ?
C179 C185 C131 113.29(14) . . ?
C179 C185 B13 126.92(14) . . ?
F45 C193 C163 120.40(14) . . ?
F45 C193 C245 120.34(14) . . ?
C163 C193 C245 119.23(14) . . ?
N10 C204 C255 179.9(3) . . ?
F78 C205 C101 116.19(13) . . ?
F78 C205 C156 119.01(13) . . ?
C101 C205 C156 124.80(14) . . ?
N24 C211 C224 179.9(3) . . ?
N4 C222 C8 178.5(3) . . ?
C211 C224 H22A 109.5 . . ?
C211 C224 H22B 109.5 . . ?
C211 C224 H22C 109.5 . . ?
H22A C224 H22B 109.5 . . ?
H22A C224 H22C 109.5 . . ?
H22B C224 H22C 109.5 . . ?
F68 C232 C156 120.88(14) . . ?
F68 C232 C237 114.80(13) . . ?
C237 C232 C156 124.32(14) . . ?
F3 C237 C135 119.53(14) . . ?
F3 C237 C232 120.82(14) . . ?
C135 C237 C232 119.66(14) . . ?
F95 C245 C105 120.96(14) . . ?
F95 C245 C193 119.77(14) . . ?
C193 C245 C105 119.25(14) . . ?
H25A C250 H25B 109.5 . . ?
H25A C250 H25C 109.5 . . ?
H25B C250 H25C 109.5 . . ?
C1 C250 H25A 109.5 . . ?
C1 C250 H25B 109.5 . . ?
C1 C250 H25C 109.5 . . ?
C204 C255 H25D 109.5 . . ?
C204 C255 H25E 109.5 . . ?
C204 C255 H25F 109.5 . . ?
H25D C255 H25E 109.5 . . ?
H25D C255 H25F 109.5 . . ?
H25E C255 H25F 109.5 . . ?
N6 C1 C250 179.2(3) . . ?
C222 C8 H8A 109.5 . . ?
C222 C8 H8B 109.5 . . ?
C222 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C40 B13 C51 112.83(12) . . ?
C40 B13 C156 101.94(12) . . ?
C40 B13 C185 113.81(12) . . ?
C51 B13 C156 114.51(12) . . ?
C51 B13 C185 100.73(12) . . ?
C156 B13 C185 113.58(12) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F13 C29 C62 F11 0.2(2) . . . . ?
F13 C29 C62 C64 179.48(13) . . . . ?
F13 C29 C97 F1 0.7(2) . . . . ?
F13 C29 C97 C76 -178.91(13) . . . . ?
F21 C131 C185 C179 177.28(13) . . . . ?
F21 C131 C185 B13 4.0(2) . . . . ?
F29 C41 C163 F15 -1.6(2) . . . . ?
F29 C41 C163 C193 179.09(14) . . . . ?
F41 C105 C245 F95 -2.0(2) . . . . ?
F41 C105 C245 C193 176.57(14) . . . . ?
F45 C193 C245 F95 2.6(2) . . . . ?
F45 C193 C245 C105 -175.93(14) . . . . ?
F53 C76 C97 F1 -0.6(2) . . . . ?
F53 C76 C97 C29 179.05(13) . . . . ?
F58 C127 C131 F21 1.8(2) . . . . ?
F58 C127 C131 C185 -178.01(14) . . . . ?
F68 C232 C237 F3 3.5(2) . . . . ?
F68 C232 C237 C135 -176.81(13) . . . . ?
F84 C89 C127 F58 -1.2(2) . . . . ?
F84 C89 C127 C131 177.91(14) . . . . ?
F84 C89 C154 F4 0.1(2) . . . . ?
F84 C89 C154 C179 -179.12(14) . . . . ?
F10 C101 C135 F12 0.2(2) . . . . ?
F10 C101 C135 C237 179.83(14) . . . . ?
F10 C101 C205 F78 -0.2(2) . . . . ?
F10 C101 C205 C156 179.20(14) . . . . ?
F11 C62 C64 F8 -1.0(2) . . . . ?
F11 C62 C64 C51 178.52(14) . . . . ?
F12 C135 C237 F3 -1.1(2) . . . . ?
F12 C135 C237 C232 179.24(14) . . . . ?
F2 C179 C185 C131 -177.54(13) . . . . ?
F2 C179 C185 B13 -4.9(2) . . . . ?
F15 C163 C193 F45 -1.4(2) . . . . ?
F15 C163 C193 C245 -179.41(14) . . . . ?
F4 C154 C179 F2 -0.3(2) . . . . ?
F4 C154 C179 C185 -179.50(14) . . . . ?
C29 C62 C64 F8 179.75(13) . . . . ?
C29 C62 C64 C51 -0.7(2) . . . . ?
C40 C41 C163 F15 178.22(15) . . . . ?
C40 C41 C163 C193 -1.1(3) . . . . ?
C40 C105 C245 F95 178.34(14) . . . . ?
C40 C105 C245 C193 -3.1(2) . . . . ?
C41 C40 C105 F41 -177.77(13) . . . . ?
C41 C40 C105 C245 1.9(2) . . . . ?
C41 C40 B13 C51 -22.5(2) . . . . ?
C41 C40 B13 C156 100.84(17) . . . . ?
C41 C40 B13 C185 -136.47(16) . . . . ?
C41 C163 C193 F45 177.92(14) . . . . ?
C41 C163 C193 C245 -0.1(2) . . . . ?
C51 C76 C97 F1 179.94(14) . . . . ?
C51 C76 C97 C29 -0.5(2) . . . . ?
C62 C29 C97 F1 179.73(13) . . . . ?
C62 C29 C97 C76 0.1(2) . . . . ?
C64 C51 C76 F53 -179.29(13) . . . . ?
C64 C51 C76 C97 0.2(2) . . . . ?
C64 C51 B13 C40 -58.78(18) . . . . ?
C64 C51 B13 C156 -174.80(13) . . . . ?
C64 C51 B13 C185 62.93(16) . . . . ?
C76 C51 C64 F8 179.91(12) . . . . ?
C76 C51 C64 C62 0.4(2) . . . . ?
C76 C51 B13 C40 129.99(16) . . . . ?
C76 C51 B13 C156 14.0(2) . . . . ?
C76 C51 B13 C185 -108.31(16) . . . . ?
C89 C127 C131 F21 -177.29(13) . . . . ?
C89 C127 C131 C185 2.9(2) . . . . ?
C89 C154 C179 F2 178.90(14) . . . . ?
C89 C154 C179 C185 -0.3(2) . . . . ?
C97 C29 C62 F11 -178.83(14) . . . . ?
C97 C29 C62 C64 0.4(2) . . . . ?
C101 C135 C237 F3 179.29(14) . . . . ?
C101 C135 C237 C232 -0.4(2) . . . . ?
C105 C40 C41 F29 -179.99(14) . . . . ?
C105 C40 C41 C163 0.2(2) . . . . ?
C105 C40 B13 C51 166.39(13) . . . . ?
C105 C40 B13 C156 -70.30(16) . . . . ?
C105 C40 B13 C185 52.40(19) . . . . ?
C127 C89 C154 F4 179.31(14) . . . . ?
C127 C89 C154 C179 0.1(2) . . . . ?
C127 C131 C185 C179 -2.9(2) . . . . ?
C127 C131 C185 B13 -176.20(14) . . . . ?
C131 C185 B13 C40 -170.07(13) . . . . ?
C131 C185 B13 C51 68.91(16) . . . . ?
C131 C185 B13 C156 -54.02(18) . . . . ?
C135 C101 C205 F78 -178.97(13) . . . . ?
C135 C101 C205 C156 0.4(2) . . . . ?
C154 C89 C127 F58 179.60(14) . . . . ?
C154 C89 C127 C131 -1.3(2) . . . . ?
C154 C179 C185 C131 1.6(2) . . . . ?
C154 C179 C185 B13 174.26(15) . . . . ?
C156 C232 C237 F3 -176.33(14) . . . . ?
C156 C232 C237 C135 3.4(2) . . . . ?
C163 C193 C245 F95 -179.37(14) . . . . ?
C163 C193 C245 C105 2.1(2) . . . . ?
C179 C185 B13 C40 17.7(2) . . . . ?
C179 C185 B13 C51 -103.37(16) . . . . ?
C179 C185 B13 C156 133.71(15) . . . . ?
C205 C101 C135 F12 178.99(14) . . . . ?
C205 C101 C135 C237 -1.4(2) . . . . ?
C205 C156 C232 F68 176.14(13) . . . . ?
C205 C156 C232 C237 -4.0(2) . . . . ?
C205 C156 B13 C40 -65.24(16) . . . . ?
C205 C156 B13 C51 56.92(18) . . . . ?
C205 C156 B13 C185 171.91(13) . . . . ?
C232 C156 C205 F78 -178.47(13) . . . . ?
C232 C156 C205 C101 2.1(2) . . . . ?
C232 C156 B13 C40 108.65(16) . . . . ?
C232 C156 B13 C51 -129.18(15) . . . . ?
C232 C156 B13 C185 -14.2(2) . . . . ?
B13 C40 C41 F29 8.4(2) . . . . ?
B13 C40 C41 C163 -171.36(15) . . . . ?
B13 C40 C105 F41 -5.5(2) . . . . ?
B13 C40 C105 C245 174.14(15) . . . . ?
B13 C51 C64 F8 7.4(2) . . . . ?
B13 C51 C64 C62 -172.09(14) . . . . ?
B13 C51 C76 F53 -7.6(2) . . . . ?
B13 C51 C76 C97 171.88(14) . . . . ?
B13 C156 C205 F78 -3.7(2) . . . . ?
B13 C156 C205 C101 176.89(14) . . . . ?
B13 C156 C232 F68 1.9(2) . . . . ?
B13 C156 C232 C237 -178.28(14) . . . . ?
_shelx_res_file
;
TITL testo1 in Pnma
CELL 0.71073 17.9405 24.5421 14.0694 90 90 90
ZERR 4 0.0003 0.0004 0.0002 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,0.5-Z
SYMM -X,0.5+Y,-Z
SFAC C H B F Fe N
UNIT 240 72 8 160 4 24
L.S. 4 0 0
PLAN 5
MORE -1
BOND $H
CONF
fmap 2 53
acta 52
REM
REM
REM
WGHT 0.028300 3.722000
FVAR 0.04899
FE2 5 0.060608 0.250000 0.640380 10.50000 0.02070 0.02150 =
0.02047 0.00000 -0.00331 0.00000
F8 4 0.240538 0.665109 0.689909 11.00000 0.02141 0.01883 =
0.03093 0.00332 0.00297 -0.00210
F13 4 0.054501 0.620060 0.909062 11.00000 0.02076 0.03427 =
0.02473 -0.00305 0.00602 0.00416
F21 4 0.340801 0.507831 0.821062 11.00000 0.02594 0.02766 =
0.02047 0.00436 -0.00113 -0.00191
F29 4 0.154756 0.603430 0.540565 11.00000 0.01643 0.03472 =
0.02536 0.00467 0.00125 0.00391
F41 4 0.414330 0.569877 0.518267 11.00000 0.01560 0.03054 =
0.02271 0.00153 0.00012 0.00090
F45 4 0.281707 0.636724 0.257082 11.00000 0.04146 0.03005 =
0.01885 0.00895 0.00040 0.00184
F53 4 0.182781 0.480202 0.753739 11.00000 0.02771 0.01827 =
0.02842 0.00263 0.00812 -0.00071
F58 4 0.445174 0.543418 0.940657 11.00000 0.02901 0.04408 =
0.02041 -0.00337 -0.00637 0.01005
F68 4 0.426513 0.480319 0.665739 11.00000 0.01585 0.02932 =
0.02716 -0.00177 -0.00455 0.00119
F78 4 0.177223 0.491436 0.556984 11.00000 0.01519 0.02499 =
0.02912 0.00028 -0.00414 0.00085
F84 4 0.516575 0.639423 0.907284 11.00000 0.02537 0.04597 =
0.04416 -0.01857 -0.01493 0.00218
F95 4 0.412771 0.607774 0.340492 11.00000 0.02594 0.03442 =
0.02427 0.00449 0.00806 -0.00422
F10 4 0.185070 0.387728 0.500079 11.00000 0.02477 0.02656 =
0.03677 -0.00418 -0.00635 -0.00593
F11 4 0.137945 0.695704 0.814803 11.00000 0.02544 0.02103 =
0.03794 -0.00518 0.00250 0.00241
F1 4 0.079008 0.512113 0.874783 11.00000 0.02622 0.02826 =
0.03039 0.00554 0.01095 -0.00279
F12 4 0.311020 0.328476 0.530393 11.00000 0.03662 0.01933 =
0.03536 -0.00346 0.00052 0.00171
F2 4 0.385866 0.661316 0.623538 11.00000 0.02434 0.02235 =
0.03118 0.00368 0.00078 -0.00471
F3 4 0.429731 0.376274 0.617648 11.00000 0.02546 0.02976 =
0.03287 0.00012 -0.00290 0.01130
F15 4 0.153744 0.634878 0.360806 11.00000 0.02703 0.03581 =
0.02917 0.00828 -0.00668 0.00811
F4 4 0.485185 0.696329 0.746395 11.00000 0.02604 0.02788 =
0.05625 -0.00741 -0.00250 -0.00950
N4 6 -0.048305 0.250000 0.571593 10.50000 0.02266 0.02833 =
0.02526 0.00000 -0.00350 0.00000
N6 6 0.108062 0.250000 0.498116 10.50000 0.02471 0.02592 =
0.02910 0.00000 0.00163 0.00000
N10 6 0.174945 0.250000 0.687473 10.50000 0.02736 0.02201 =
0.03534 0.00000 -0.00774 0.00000
N14 6 0.051994 0.336193 0.640241 11.00000 0.02655 0.02569 =
0.02338 -0.00167 -0.00364 0.00073
N24 6 0.023296 0.250000 0.788226 10.50000 0.03329 0.03110 =
0.02474 0.00000 -0.00364 0.00000
C29 1 0.106316 0.604128 0.845933 11.00000 0.01419 0.02856 =
0.01862 -0.00168 0.00032 0.00276
C40 1 0.285454 0.585485 0.540453 11.00000 0.01812 0.01642 =
0.02018 0.00047 -0.00052 -0.00158
C41 1 0.221142 0.602712 0.494839 11.00000 0.01882 0.01897 =
0.02298 0.00093 0.00214 -0.00101
C51 1 0.217792 0.570886 0.713781 11.00000 0.01525 0.02127 =
0.01632 0.00161 -0.00246 -0.00018
C62 1 0.148308 0.642374 0.798288 11.00000 0.01835 0.01960 =
0.02337 -0.00256 -0.00373 0.00137
C64 1 0.201591 0.625097 0.734373 11.00000 0.01611 0.02039 =
0.02156 0.00292 -0.00234 -0.00369
C76 1 0.173810 0.534617 0.764448 11.00000 0.01798 0.01779 =
0.02020 0.00106 -0.00131 0.00045
C89 1 0.466485 0.620401 0.844609 11.00000 0.01496 0.03447 =
0.03051 -0.01464 -0.00605 0.00355
C93 1 0.015577 0.438094 0.649954 11.00000 0.03058 0.02478 =
0.02673 0.00305 0.00633 0.00482
AFIX 137
H93A 2 -0.029469 0.444060 0.614627 11.00000 -1.50000
H93B 2 0.054779 0.460149 0.623939 11.00000 -1.50000
H93C 2 0.007666 0.447807 0.715277 11.00000 -1.50000
AFIX 0
C97 1 0.119109 0.549946 0.828815 11.00000 0.01702 0.02567 =
0.01917 0.00328 0.00060 -0.00270
C101 1 0.244177 0.411222 0.542767 11.00000 0.01914 0.02574 =
0.01973 0.00065 -0.00041 -0.00559
C105 1 0.348725 0.587340 0.483122 11.00000 0.01697 0.01847 =
0.02109 -0.00007 -0.00160 -0.00174
C127 1 0.429754 0.572164 0.861549 11.00000 0.01955 0.03216 =
0.01967 -0.00346 -0.00219 0.00900
C131 1 0.376869 0.554469 0.797574 11.00000 0.01767 0.02350 =
0.02097 -0.00272 0.00242 0.00052
C135 1 0.307670 0.381074 0.558052 11.00000 0.02871 0.01770 =
0.02075 -0.00001 0.00391 0.00023
C149 1 0.036394 0.380988 0.643934 11.00000 0.01961 0.02879 =
0.01608 0.00049 -0.00017 -0.00117
C154 1 0.450275 0.648804 0.763430 11.00000 0.01698 0.02275 =
0.03799 -0.00849 0.00366 -0.00190
C156 1 0.299899 0.491666 0.618606 11.00000 0.01707 0.02071 =
0.01499 0.00299 0.00193 -0.00119
C163 1 0.218945 0.620016 0.401379 11.00000 0.02315 0.01979 =
0.02470 0.00330 -0.00567 0.00314
C179 1 0.397886 0.629192 0.700061 11.00000 0.01600 0.02386 =
0.02433 -0.00096 0.00101 0.00157
C185 1 0.359178 0.580820 0.712949 11.00000 0.01402 0.02292 =
0.02037 -0.00238 0.00169 0.00111
C193 1 0.283311 0.621589 0.349064 11.00000 0.03198 0.01781 =
0.01723 0.00433 -0.00081 -0.00086
C204 1 0.236967 0.250000 0.703233 10.50000 0.03016 0.01715 =
0.03024 0.00000 -0.00616 0.00000
C205 1 0.241658 0.464559 0.572944 11.00000 0.01600 0.02187 =
0.01947 0.00335 0.00147 0.00112
C211 1 0.012907 0.250000 0.868114 10.50000 0.03336 0.03516 =
0.02813 0.00000 -0.00362 0.00000
C222 1 -0.088038 0.250000 0.509400 10.50000 0.02799 0.01949 =
0.03159 0.00000 -0.00417 0.00000
C224 1 -0.000507 0.250000 0.970363 10.50000 0.05699 0.07122 =
0.02375 0.00000 0.00145 0.00000
PART -1
AFIX 137
H22A 2 0.000432 0.286767 0.993624 10.50000 -1.50000
H22B 2 0.037570 0.229125 1.001546 10.50000 -1.50000
H22C 2 -0.048352 0.234108 0.983217 10.50000 -1.50000
AFIX 0
PART 0
C232 1 0.363238 0.459653 0.628146 11.00000 0.01703 0.02544 =
0.01620 0.00256 -0.00079 -0.00134
C237 1 0.367612 0.405449 0.601368 11.00000 0.01952 0.02555 =
0.02043 0.00327 0.00173 0.00557
C245 1 0.349268 0.605915 0.390735 11.00000 0.02284 0.01915 =
0.02220 -0.00006 0.00569 -0.00391
C250 1 0.186541 0.250000 0.344817 10.50000 0.02947 0.09417 =
0.03748 0.00000 0.01263 0.00000
PART -1
AFIX 137
H25A 2 0.196066 0.286878 0.325582 10.50000 -1.50000
H25B 2 0.160109 0.231320 0.295239 10.50000 -1.50000
H25C 2 0.232977 0.231802 0.356729 10.50000 -1.50000
AFIX 0
PART 0
C255 1 0.316626 0.250000 0.723739 10.50000 0.02737 0.02984 =
0.04177 0.00000 -0.01117 0.00000
PART -1
AFIX 137
H25D 2 0.342818 0.231967 0.673234 10.50000 -1.50000
H25E 2 0.325528 0.231157 0.782447 10.50000 -1.50000
H25F 2 0.333983 0.286876 0.729039 10.50000 -1.50000
AFIX 0
PART 0
C1 1 0.142070 0.250000 0.430507 10.50000 0.02111 0.02793 =
0.03195 0.00000 -0.00059 0.00000
C8 1 -0.137538 0.250000 0.427617 10.50000 0.05865 0.04240 =
0.05087 0.00000 -0.03364 0.00000
PART -1
AFIX 137
H8A 2 -0.180185 0.272374 0.440857 10.50000 -1.50000
H8B 2 -0.153545 0.213424 0.414640 10.50000 -1.50000
H8C 2 -0.111578 0.264202 0.373338 10.50000 -1.50000
AFIX 0
PART 0
B13 3 0.290582 0.556922 0.646075 11.00000 0.01369 0.02081 =
0.01864 0.00205 0.00068 -0.00167
HKLF 4
REM testo1 in Pnma
REM R1 = 0.0298 for 5713 Fo > 4sig(Fo) and 0.0388 for all 6747 data
REM 516 parameters refined using 0 restraints
END
WGHT 0.0281 3.7488
REM Highest difference peak 0.295, deepest hole -0.297, 1-sigma level 0.044
Q1 1 0.2524 0.5600 0.6830 11.00000 0.05 0.29
Q2 1 0.1301 0.5415 0.7832 11.00000 0.05 0.27
Q3 1 0.2978 0.5195 0.6358 11.00000 0.05 0.27
Q4 1 0.3445 0.5824 0.4266 11.00000 0.05 0.27
Q5 1 0.3143 0.5800 0.5042 11.00000 0.05 0.26
;
_shelx_res_checksum 11860
_olex2_submission_special_instructions 'No special instructions were received'