# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_1
_database_code_depnum_ccdc_archive 'CCDC 1586854'
loop_
_audit_author_name
_audit_author_address
'Ajeet Singh'
;Indian Institute of Technology Indore
India
;
_audit_update_record
;
2019-10-26 deposited with the CCDC. 2020-01-20 downloaded from the CCDC.
;
_audit_creation_date 2019-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic 'Fc Trip'
_chemical_formula_moiety 'C10 H10 Fe, C20 H14'
_chemical_formula_sum 'C30 H24 Fe'
_chemical_formula_weight 440.34
_chemical_melting_point ?
_chemical_oxdiff_formula 'c32 h26 n6 br2'
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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.4217(5)
_cell_length_b 10.3198(6)
_cell_length_c 13.0913(6)
_cell_angle_alpha 67.835(5)
_cell_angle_beta 71.685(5)
_cell_angle_gamma 86.556(5)
_cell_volume 1116.62(11)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 5563
_cell_measurement_temperature 293
_cell_measurement_theta_max 30.6760
_cell_measurement_theta_min 3.9570
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.690
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.71328
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour orange
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.310
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 460
_exptl_crystal_preparation 'Hexane chloroform'
_exptl_crystal_recrystallization_method 'Hexane Chlorofrom'
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.38
_exptl_crystal_size_min 0.3
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0331
_diffrn_reflns_av_unetI/netI 0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 13361
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 32.213
_diffrn_reflns_theta_min 3.021
_diffrn_ambient_temperature 293
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.0309
_diffrn_detector_type Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega 0.00 93.00 1.0000 38.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 37.0000 -60.0000 93
#__ type_ start__ end____ width___ exp.time_
2 omega 37.00 67.00 1.0000 38.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 -99.0000 -90.0000 30
#__ type_ start__ end____ width___ exp.time_
3 omega 35.00 67.00 1.0000 38.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 -99.0000 -180.0000 32
#__ type_ start__ end____ width___ exp.time_
4 omega -18.00 67.00 1.0000 38.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 -99.0000 30.0000 85
#__ type_ start__ end____ width___ exp.time_
5 omega -20.00 57.00 1.0000 38.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 -99.0000 120.0000 77
#__ type_ start__ end____ width___ exp.time_
6 omega -42.00 51.00 1.0000 38.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 -37.0000 120.0000 93
#__ type_ start__ end____ width___ exp.time_
7 omega 35.00 63.00 1.0000 38.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 178.0000 120.0000 28
#__ type_ start__ end____ width___ exp.time_
8 omega 54.00 86.00 1.0000 38.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 178.0000 30.0000 32
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0242168000
_diffrn_orient_matrix_UB_12 0.0691612000
_diffrn_orient_matrix_UB_13 -0.0162688000
_diffrn_orient_matrix_UB_21 0.0635609000
_diffrn_orient_matrix_UB_22 0.0238596000
_diffrn_orient_matrix_UB_23 0.0076311000
_diffrn_orient_matrix_UB_31 0.0411109000
_diffrn_orient_matrix_UB_32 0.0134130000
_diffrn_orient_matrix_UB_33 -0.0589739000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5288
_reflns_number_total 7220
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 30.44
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.362
_refine_diff_density_min -0.521
_refine_diff_density_rms 0.062
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.028
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 280
_refine_ls_number_reflns 7220
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0733
_refine_ls_R_factor_gt 0.0538
_refine_ls_restrained_S_all 1.028
_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^)+(0.0656P)^2^+0.3085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1391
_refine_ls_wR_factor_ref 0.1533
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Ternary CH refined with riding coordinates:
C11(H11), C12(H12), C8(H8)
2.b Aromatic/amide H refined with riding coordinates:
C25(H25), C23(H23), C20(H20), C28(H28), C22(H22), C21(H21), C14(H14),
C26(H26), C27(H27), C17(H17), C1(H1), C5(H5), C4(H4), C16(H16), C6(H6),
C15(H15), C10(H10), C7(H7), C2(H2), C3(H3), C9(H9)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.12812(3) 0.29378(3) 0.68775(2) 0.04967(12) Uani 1 1 d . . . . .
C24 C 0.5243(2) 0.15876(19) 0.26005(15) 0.0388(4) Uani 1 1 d . . . . .
C19 C 0.5766(2) 0.40674(19) 0.20065(15) 0.0383(3) Uani 1 1 d . . . . .
C29 C 0.6315(2) 0.16117(19) 0.15733(15) 0.0416(4) Uani 1 1 d . . . . .
C11 C 0.5600(2) 0.2678(2) 0.30230(14) 0.0390(4) Uani 1 1 d . . . . .
H11 H 0.484487 0.266284 0.374092 0.047 Uiso 1 1 calc R . . . .
C0AA C 0.6849(2) 0.4093(2) 0.09838(15) 0.0406(4) Uani 1 1 d . . . . .
C13 C 0.7147(2) 0.2394(2) 0.31433(16) 0.0428(4) Uani 1 1 d . . . . .
C12 C 0.7599(2) 0.2719(2) 0.11216(16) 0.0445(4) Uani 1 1 d . . . . .
H12 H 0.835496 0.273524 0.040316 0.053 Uiso 1 1 calc R . . . .
C25 C 0.3996(2) 0.0668(2) 0.31205(18) 0.0509(5) Uani 1 1 d . . . . .
H25 H 0.328930 0.065318 0.380643 0.061 Uiso 1 1 calc R . . . .
C18 C 0.8229(2) 0.2411(2) 0.21175(18) 0.0464(4) Uani 1 1 d . . . . .
C23 C 0.7099(2) 0.5267(2) -0.00237(17) 0.0502(5) Uani 1 1 d . . . . .
H23 H 0.782854 0.529058 -0.070241 0.060 Uiso 1 1 calc R . . . .
C20 C 0.4921(2) 0.5199(2) 0.20132(18) 0.0486(4) Uani 1 1 d . . . . .
H20 H 0.419751 0.518205 0.269273 0.058 Uiso 1 1 calc R . . . .
C28 C 0.6131(3) 0.0699(2) 0.10768(19) 0.0576(6) Uani 1 1 d . . . . .
H28 H 0.685008 0.069557 0.040203 0.069 Uiso 1 1 calc R . . . .
C22 C 0.6256(3) 0.6413(2) -0.00205(19) 0.0558(5) Uani 1 1 d . . . . .
H22 H 0.642461 0.721130 -0.069659 0.067 Uiso 1 1 calc R . . . .
C21 C 0.5167(3) 0.6369(2) 0.0986(2) 0.0571(5) Uani 1 1 d . . . . .
H21 H 0.458793 0.713322 0.097724 0.068 Uiso 1 1 calc R . . . .
C14 C 0.7528(3) 0.2129(2) 0.4138(2) 0.0579(6) Uani 1 1 d . . . . .
H14 H 0.681211 0.213272 0.481386 0.069 Uiso 1 1 calc R . . . .
C26 C 0.3807(3) -0.0238(3) 0.2606(2) 0.0675(7) Uani 1 1 d . . . . .
H26 H 0.296537 -0.086216 0.294554 0.081 Uiso 1 1 calc R . . . .
C27 C 0.4865(4) -0.0215(2) 0.1593(2) 0.0706(7) Uani 1 1 d . . . . .
H27 H 0.472673 -0.082144 0.125198 0.085 Uiso 1 1 calc R . . . .
C17 C 0.9686(2) 0.2152(3) 0.2098(3) 0.0671(7) Uani 1 1 d . . . . .
H17 H 1.041181 0.215747 0.142360 0.081 Uiso 1 1 calc R . . . .
C1 C 0.3057(3) 0.2051(4) 0.6123(2) 0.0849(10) Uani 1 1 d . . . . .
H1 H 0.347590 0.124926 0.650828 0.102 Uiso 1 1 calc R . . . .
C5 C 0.1956(3) 0.2085(4) 0.5645(2) 0.0758(8) Uani 1 1 d . . . . .
H5 H 0.149882 0.130535 0.565318 0.091 Uiso 1 1 calc R . . . .
C4 C 0.1634(4) 0.3430(4) 0.5156(2) 0.0754(8) Uani 1 1 d . . . . .
H4 H 0.092032 0.371763 0.477406 0.090 Uiso 1 1 calc R . . . .
C16 C 1.0057(3) 0.1882(3) 0.3107(3) 0.0838(10) Uani 1 1 d . . . . .
H16 H 1.104011 0.171519 0.309982 0.101 Uiso 1 1 calc R . . . .
C6 C -0.0556(4) 0.1821(4) 0.8143(3) 0.0881(10) Uani 1 1 d . . . . .
H6 H -0.102805 0.104620 0.815651 0.106 Uiso 1 1 calc R . . . .
C15 C 0.8992(4) 0.1859(3) 0.4108(3) 0.0787(9) Uani 1 1 d . . . . .
H15 H 0.925792 0.165937 0.477581 0.094 Uiso 1 1 calc R . . . .
C10 C 0.0564(4) 0.1781(5) 0.8593(2) 0.1032(14) Uani 1 1 d . . . . .
H10 H 0.099774 0.098371 0.896637 0.124 Uiso 1 1 calc R . . . .
C7 C -0.0873(4) 0.3136(6) 0.7682(3) 0.1178(17) Uani 1 1 d . . . . .
H7 H -0.160767 0.342844 0.732229 0.141 Uiso 1 1 calc R . . . .
C2 C 0.3454(3) 0.3440(6) 0.5936(3) 0.1095(16) Uani 1 1 d . . . . .
H2 H 0.417028 0.373266 0.616948 0.131 Uiso 1 1 calc R . . . .
C3 C 0.2518(4) 0.4304(4) 0.5309(3) 0.0938(12) Uani 1 1 d . . . . .
H3 H 0.251211 0.527594 0.505298 0.113 Uiso 1 1 calc R . . . .
C9 C 0.0949(5) 0.3169(8) 0.8389(4) 0.139(2) Uani 1 1 d . . . . .
H9 H 0.167938 0.347696 0.860095 0.167 Uiso 1 1 calc R . . . .
C8 C 0.0013(8) 0.3983(4) 0.7807(4) 0.149(3) Uani 1 1 d . . . . .
H8 H -0.001325 0.500482 0.755221 0.179 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.04489(17) 0.0579(2) 0.04392(17) -0.02435(14) -0.00431(12) 0.00168(13)
C24 0.0419(8) 0.0348(8) 0.0392(8) -0.0105(7) -0.0171(7) 0.0066(7)
C19 0.0428(9) 0.0361(8) 0.0384(8) -0.0159(7) -0.0142(7) 0.0047(7)
C29 0.0523(10) 0.0334(8) 0.0400(8) -0.0138(7) -0.0173(8) 0.0116(7)
C11 0.0385(8) 0.0437(9) 0.0324(7) -0.0153(7) -0.0070(6) 0.0035(7)
C0AA 0.0427(9) 0.0384(9) 0.0389(8) -0.0149(7) -0.0105(7) 0.0037(7)
C13 0.0447(9) 0.0370(9) 0.0450(9) -0.0105(7) -0.0177(8) 0.0012(7)
C12 0.0431(9) 0.0420(10) 0.0374(8) -0.0131(7) -0.0015(7) 0.0074(7)
C25 0.0501(10) 0.0468(11) 0.0510(10) -0.0087(9) -0.0209(9) -0.0021(9)
C18 0.0403(9) 0.0374(9) 0.0541(10) -0.0108(8) -0.0133(8) 0.0042(7)
C23 0.0572(11) 0.0448(11) 0.0409(9) -0.0101(8) -0.0118(8) -0.0032(9)
C20 0.0560(11) 0.0451(10) 0.0534(11) -0.0276(9) -0.0194(9) 0.0124(9)
C28 0.0890(17) 0.0446(11) 0.0503(11) -0.0252(9) -0.0306(11) 0.0207(11)
C22 0.0729(14) 0.0388(10) 0.0541(11) -0.0083(9) -0.0286(11) 0.0006(10)
C21 0.0743(15) 0.0388(10) 0.0686(13) -0.0237(10) -0.0349(12) 0.0182(10)
C14 0.0704(14) 0.0501(12) 0.0556(12) -0.0104(10) -0.0337(11) -0.0026(10)
C26 0.0836(17) 0.0478(12) 0.0754(16) -0.0119(11) -0.0417(14) -0.0110(12)
C27 0.112(2) 0.0428(12) 0.0807(17) -0.0279(11) -0.0564(17) 0.0065(13)
C17 0.0393(10) 0.0543(13) 0.0913(18) -0.0149(13) -0.0146(11) 0.0045(9)
C1 0.0653(16) 0.115(3) 0.0585(15) -0.0305(16) -0.0065(12) 0.0352(17)
C5 0.0815(18) 0.088(2) 0.0621(15) -0.0443(15) -0.0086(13) 0.0094(15)
C4 0.0808(18) 0.093(2) 0.0504(13) -0.0274(14) -0.0195(12) 0.0138(16)
C16 0.0556(14) 0.0627(16) 0.130(3) -0.0131(17) -0.0545(18) 0.0052(12)
C6 0.0688(18) 0.104(3) 0.0756(18) -0.0405(18) 0.0112(15) -0.0252(17)
C15 0.0823(19) 0.0669(17) 0.095(2) -0.0111(15) -0.0607(18) -0.0030(14)
C10 0.088(2) 0.132(3) 0.0456(14) -0.0088(17) 0.0009(14) 0.041(2)
C7 0.073(2) 0.162(4) 0.0705(19) -0.020(3) 0.0021(16) 0.060(2)
C2 0.0492(14) 0.216(5) 0.0691(18) -0.078(3) 0.0109(13) -0.039(2)
C3 0.118(3) 0.0709(19) 0.0590(16) -0.0247(14) 0.0215(17) -0.0195(19)
C9 0.091(3) 0.269(7) 0.074(2) -0.109(4) 0.0187(19) -0.070(4)
C8 0.198(6) 0.075(3) 0.107(3) -0.056(2) 0.076(4) -0.022(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
Fe1 C1 2.018(3) . ?
Fe1 C5 2.036(3) . ?
Fe1 C4 2.033(3) . ?
Fe1 C6 2.016(3) . ?
Fe1 C10 2.011(3) . ?
Fe1 C7 2.010(3) . ?
Fe1 C2 2.009(3) . ?
Fe1 C3 2.018(3) . ?
Fe1 C9 2.007(3) . ?
Fe1 C8 1.998(3) . ?
C24 C29 1.397(3) . ?
C24 C11 1.522(2) . ?
C24 C25 1.374(3) . ?
C19 C11 1.519(2) . ?
C19 C0AA 1.397(2) . ?
C19 C20 1.375(3) . ?
C29 C12 1.526(3) . ?
C29 C28 1.375(3) . ?
C11 H11 0.9800 . ?
C11 C13 1.514(3) . ?
C0AA C12 1.520(3) . ?
C0AA C23 1.377(3) . ?
C13 C18 1.403(3) . ?
C13 C14 1.383(3) . ?
C12 H12 0.9800 . ?
C12 C18 1.518(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.390(3) . ?
C18 C17 1.378(3) . ?
C23 H23 0.9300 . ?
C23 C22 1.384(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.390(3) . ?
C28 H28 0.9300 . ?
C28 C27 1.385(4) . ?
C22 H22 0.9300 . ?
C22 C21 1.379(3) . ?
C21 H21 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.382(4) . ?
C26 H26 0.9300 . ?
C26 C27 1.379(4) . ?
C27 H27 0.9300 . ?
C17 H17 0.9300 . ?
C17 C16 1.393(4) . ?
C1 H1 0.9300 . ?
C1 C5 1.362(4) . ?
C1 C2 1.413(5) . ?
C5 H5 0.9300 . ?
C5 C4 1.353(4) . ?
C4 H4 0.9300 . ?
C4 C3 1.371(5) . ?
C16 H16 0.9300 . ?
C16 C15 1.371(5) . ?
C6 H6 0.9300 . ?
C6 C10 1.353(5) . ?
C6 C7 1.320(6) . ?
C15 H15 0.9300 . ?
C10 H10 0.9300 . ?
C10 C9 1.402(7) . ?
C7 H7 0.9300 . ?
C7 C8 1.330(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.433(6) . ?
C3 H3 0.9300 . ?
C9 H9 0.9300 . ?
C9 C8 1.383(8) . ?
C8 H8 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 Fe1 C5 39.27(13) . . ?
C1 Fe1 C4 66.29(13) . . ?
C1 Fe1 C3 68.28(14) . . ?
C4 Fe1 C5 38.84(12) . . ?
C6 Fe1 C1 123.27(17) . . ?
C6 Fe1 C5 109.24(14) . . ?
C6 Fe1 C4 123.68(14) . . ?
C6 Fe1 C3 158.03(18) . . ?
C10 Fe1 C1 108.35(14) . . ?
C10 Fe1 C5 123.17(17) . . ?
C10 Fe1 C4 157.50(19) . . ?
C10 Fe1 C6 39.25(15) . . ?
C10 Fe1 C3 161.3(2) . . ?
C7 Fe1 C1 157.5(2) . . ?
C7 Fe1 C5 124.1(2) . . ?
C7 Fe1 C4 110.44(15) . . ?
C7 Fe1 C6 38.27(17) . . ?
C7 Fe1 C10 65.56(14) . . ?
C7 Fe1 C3 124.54(18) . . ?
C2 Fe1 C1 41.09(16) . . ?
C2 Fe1 C5 67.63(14) . . ?
C2 Fe1 C4 67.86(13) . . ?
C2 Fe1 C6 159.0(2) . . ?
C2 Fe1 C10 123.63(17) . . ?
C2 Fe1 C7 160.6(2) . . ?
C2 Fe1 C3 41.68(16) . . ?
C3 Fe1 C5 66.64(13) . . ?
C3 Fe1 C4 39.56(13) . . ?
C9 Fe1 C1 124.4(2) . . ?
C9 Fe1 C5 159.4(3) . . ?
C9 Fe1 C4 160.3(3) . . ?
C9 Fe1 C6 66.83(15) . . ?
C9 Fe1 C10 40.9(2) . . ?
C9 Fe1 C7 66.35(19) . . ?
C9 Fe1 C2 108.32(14) . . ?
C9 Fe1 C3 124.7(2) . . ?
C8 Fe1 C1 161.6(3) . . ?
C8 Fe1 C5 158.4(3) . . ?
C8 Fe1 C4 124.8(2) . . ?
C8 Fe1 C6 65.47(16) . . ?
C8 Fe1 C10 67.19(18) . . ?
C8 Fe1 C7 38.7(2) . . ?
C8 Fe1 C2 125.1(2) . . ?
C8 Fe1 C3 109.83(16) . . ?
C8 Fe1 C9 40.4(2) . . ?
C29 C24 C11 113.26(15) . . ?
C25 C24 C29 120.84(19) . . ?
C25 C24 C11 125.88(17) . . ?
C0AA C19 C11 113.23(16) . . ?
C20 C19 C11 126.18(17) . . ?
C20 C19 C0AA 120.50(17) . . ?
C24 C29 C12 112.98(16) . . ?
C28 C29 C24 119.89(19) . . ?
C28 C29 C12 127.13(19) . . ?
C24 C11 H11 113.1 . . ?
C19 C11 C24 104.80(13) . . ?
C19 C11 H11 113.1 . . ?
C13 C11 C24 105.52(15) . . ?
C13 C11 C19 106.37(14) . . ?
C13 C11 H11 113.1 . . ?
C19 C0AA C12 113.14(15) . . ?
C23 C0AA C19 120.12(18) . . ?
C23 C0AA C12 126.68(17) . . ?
C18 C13 C11 113.22(16) . . ?
C14 C13 C11 126.05(19) . . ?
C14 C13 C18 120.7(2) . . ?
C29 C12 H12 113.2 . . ?
C0AA C12 C29 104.88(15) . . ?
C0AA C12 H12 113.2 . . ?
C18 C12 C29 105.52(14) . . ?
C18 C12 C0AA 106.25(16) . . ?
C18 C12 H12 113.2 . . ?
C24 C25 H25 120.5 . . ?
C24 C25 C26 119.0(2) . . ?
C26 C25 H25 120.5 . . ?
C13 C18 C12 113.06(16) . . ?
C17 C18 C13 119.8(2) . . ?
C17 C18 C12 127.1(2) . . ?
C0AA C23 H23 120.2 . . ?
C0AA C23 C22 119.6(2) . . ?
C22 C23 H23 120.2 . . ?
C19 C20 H20 120.6 . . ?
C19 C20 C21 118.8(2) . . ?
C21 C20 H20 120.6 . . ?
C29 C28 H28 120.4 . . ?
C29 C28 C27 119.3(2) . . ?
C27 C28 H28 120.4 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 C23 119.97(19) . . ?
C21 C22 H22 120.0 . . ?
C20 C21 H21 119.5 . . ?
C22 C21 C20 121.0(2) . . ?
C22 C21 H21 119.5 . . ?
C13 C14 H14 120.6 . . ?
C15 C14 C13 118.7(3) . . ?
C15 C14 H14 120.6 . . ?
C25 C26 H26 119.9 . . ?
C27 C26 C25 120.1(2) . . ?
C27 C26 H26 119.9 . . ?
C28 C27 H27 119.6 . . ?
C26 C27 C28 120.9(2) . . ?
C26 C27 H27 119.6 . . ?
C18 C17 H17 120.5 . . ?
C18 C17 C16 118.9(3) . . ?
C16 C17 H17 120.5 . . ?
Fe1 C1 H1 125.6 . . ?
C5 C1 Fe1 71.06(16) . . ?
C5 C1 H1 125.8 . . ?
C5 C1 C2 108.4(3) . . ?
C2 C1 Fe1 69.13(18) . . ?
C2 C1 H1 125.8 . . ?
Fe1 C5 H5 126.1 . . ?
C1 C5 Fe1 69.66(17) . . ?
C1 C5 H5 125.3 . . ?
C4 C5 Fe1 70.49(16) . . ?
C4 C5 C1 109.3(3) . . ?
C4 C5 H5 125.3 . . ?
Fe1 C4 H4 126.1 . . ?
C5 C4 Fe1 70.66(16) . . ?
C5 C4 H4 125.2 . . ?
C5 C4 C3 109.7(3) . . ?
C3 C4 Fe1 69.63(16) . . ?
C3 C4 H4 125.2 . . ?
C17 C16 H16 119.5 . . ?
C15 C16 C17 120.9(2) . . ?
C15 C16 H16 119.5 . . ?
Fe1 C6 H6 125.4 . . ?
C10 C6 Fe1 70.16(18) . . ?
C10 C6 H6 125.5 . . ?
C7 C6 Fe1 70.59(19) . . ?
C7 C6 H6 125.5 . . ?
C7 C6 C10 109.1(4) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 C14 120.8(3) . . ?
C16 C15 H15 119.6 . . ?
Fe1 C10 H10 125.1 . . ?
C6 C10 Fe1 70.59(18) . . ?
C6 C10 H10 126.5 . . ?
C6 C10 C9 107.1(4) . . ?
C9 C10 Fe1 69.42(19) . . ?
C9 C10 H10 126.5 . . ?
Fe1 C7 H7 125.3 . . ?
C6 C7 Fe1 71.14(18) . . ?
C6 C7 H7 125.0 . . ?
C6 C7 C8 110.1(4) . . ?
C8 C7 Fe1 70.2(2) . . ?
C8 C7 H7 125.0 . . ?
Fe1 C2 H2 125.1 . . ?
C1 C2 Fe1 69.78(16) . . ?
C1 C2 H2 127.3 . . ?
C1 C2 C3 105.5(3) . . ?
C3 C2 Fe1 69.49(17) . . ?
C3 C2 H2 127.3 . . ?
Fe1 C3 H3 125.5 . . ?
C4 C3 Fe1 70.82(16) . . ?
C4 C3 C2 107.2(3) . . ?
C4 C3 H3 126.4 . . ?
C2 C3 Fe1 68.83(16) . . ?
C2 C3 H3 126.4 . . ?
Fe1 C9 H9 125.2 . . ?
C10 C9 Fe1 69.7(2) . . ?
C10 C9 H9 127.2 . . ?
C8 C9 Fe1 69.5(2) . . ?
C8 C9 C10 105.6(4) . . ?
C8 C9 H9 127.2 . . ?
Fe1 C8 H8 125.9 . . ?
C7 C8 Fe1 71.1(2) . . ?
C7 C8 C9 108.2(4) . . ?
C7 C8 H8 125.9 . . ?
C9 C8 Fe1 70.1(2) . . ?
C9 C8 H8 125.9 . . ?
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
Fe1 C1 C5 C4 59.5(2) . . . . ?
Fe1 C1 C2 C3 -60.70(19) . . . . ?
Fe1 C5 C4 C3 58.9(2) . . . . ?
Fe1 C4 C3 C2 59.49(19) . . . . ?
Fe1 C6 C10 C9 60.1(2) . . . . ?
Fe1 C6 C7 C8 -59.6(3) . . . . ?
Fe1 C10 C9 C8 60.6(2) . . . . ?
Fe1 C7 C8 C9 -60.6(3) . . . . ?
Fe1 C2 C3 C4 -60.8(2) . . . . ?
Fe1 C9 C8 C7 61.2(3) . . . . ?
C24 C29 C12 C0AA -56.50(19) . . . . ?
C24 C29 C12 C18 55.5(2) . . . . ?
C24 C29 C28 C27 1.3(3) . . . . ?
C24 C11 C13 C18 55.6(2) . . . . ?
C24 C11 C13 C14 -124.0(2) . . . . ?
C24 C25 C26 C27 0.4(3) . . . . ?
C19 C11 C13 C18 -55.4(2) . . . . ?
C19 C11 C13 C14 125.1(2) . . . . ?
C19 C0AA C12 C29 55.9(2) . . . . ?
C19 C0AA C12 C18 -55.6(2) . . . . ?
C19 C0AA C23 C22 -0.9(3) . . . . ?
C19 C20 C21 C22 -1.2(3) . . . . ?
C29 C24 C11 C19 55.94(19) . . . . ?
C29 C24 C11 C13 -56.14(19) . . . . ?
C29 C24 C25 C26 -0.3(3) . . . . ?
C29 C12 C18 C13 -56.0(2) . . . . ?
C29 C12 C18 C17 123.5(2) . . . . ?
C29 C28 C27 C26 -1.3(4) . . . . ?
C11 C24 C29 C12 0.5(2) . . . . ?
C11 C24 C29 C28 -179.06(17) . . . . ?
C11 C24 C25 C26 177.98(19) . . . . ?
C11 C19 C0AA C12 0.6(2) . . . . ?
C11 C19 C0AA C23 178.03(17) . . . . ?
C11 C19 C20 C21 -176.55(18) . . . . ?
C11 C13 C18 C12 0.4(2) . . . . ?
C11 C13 C18 C17 -179.20(19) . . . . ?
C11 C13 C14 C15 178.6(2) . . . . ?
C0AA C19 C11 C24 -56.66(19) . . . . ?
C0AA C19 C11 C13 54.8(2) . . . . ?
C0AA C19 C20 C21 -0.2(3) . . . . ?
C0AA C12 C18 C13 55.0(2) . . . . ?
C0AA C12 C18 C17 -125.5(2) . . . . ?
C0AA C23 C22 C21 -0.5(3) . . . . ?
C13 C18 C17 C16 -0.2(4) . . . . ?
C13 C14 C15 C16 1.4(4) . . . . ?
C12 C29 C28 C27 -178.1(2) . . . . ?
C12 C0AA C23 C22 176.14(19) . . . . ?
C12 C18 C17 C16 -179.7(2) . . . . ?
C25 C24 C29 C12 179.00(17) . . . . ?
C25 C24 C29 C28 -0.5(3) . . . . ?
C25 C24 C11 C19 -122.49(19) . . . . ?
C25 C24 C11 C13 125.43(19) . . . . ?
C25 C26 C27 C28 0.4(4) . . . . ?
C18 C13 C14 C15 -1.0(3) . . . . ?
C18 C17 C16 C15 0.6(4) . . . . ?
C23 C0AA C12 C29 -121.3(2) . . . . ?
C23 C0AA C12 C18 127.2(2) . . . . ?
C23 C22 C21 C20 1.6(3) . . . . ?
C20 C19 C11 C24 119.93(19) . . . . ?
C20 C19 C11 C13 -128.60(19) . . . . ?
C20 C19 C0AA C12 -176.17(17) . . . . ?
C20 C19 C0AA C23 1.2(3) . . . . ?
C28 C29 C12 C0AA 123.0(2) . . . . ?
C28 C29 C12 C18 -125.0(2) . . . . ?
C14 C13 C18 C12 180.00(18) . . . . ?
C14 C13 C18 C17 0.4(3) . . . . ?
C17 C16 C15 C14 -1.2(5) . . . . ?
C1 C5 C4 Fe1 -59.01(19) . . . . ?
C1 C5 C4 C3 -0.2(3) . . . . ?
C1 C2 C3 Fe1 60.90(18) . . . . ?
C1 C2 C3 C4 0.1(3) . . . . ?
C5 C1 C2 Fe1 60.48(19) . . . . ?
C5 C1 C2 C3 -0.2(3) . . . . ?
C5 C4 C3 Fe1 -59.5(2) . . . . ?
C5 C4 C3 C2 0.0(3) . . . . ?
C6 C10 C9 Fe1 -60.9(2) . . . . ?
C6 C10 C9 C8 -0.3(4) . . . . ?
C6 C7 C8 Fe1 60.2(3) . . . . ?
C6 C7 C8 C9 -0.4(4) . . . . ?
C10 C6 C7 Fe1 59.8(2) . . . . ?
C10 C6 C7 C8 0.2(4) . . . . ?
C10 C9 C8 Fe1 -60.8(2) . . . . ?
C10 C9 C8 C7 0.4(4) . . . . ?
C7 C6 C10 Fe1 -60.1(2) . . . . ?
C7 C6 C10 C9 0.0(4) . . . . ?
C2 C1 C5 Fe1 -59.28(19) . . . . ?
C2 C1 C5 C4 0.2(3) . . . . ?
_shelx_res_file
;
TITL smm543_a.res in P-1
smm543.res
created by SHELXL-2018/3 at 00:49:43 on 26-Oct-2019
REM Old TITL smm543 in P-1 #2
REM SHELXT solution in P-1
REM R1 0.157, Rweak 0.013, Alpha 0.073, Orientation as input
REM Formula found by SHELXT: C11 Fe
CELL 0.71073 9.421692 10.31978 13.091348 67.8354 71.6848 86.5556
ZERR 2 0.000527 0.000585 0.000642 0.0049 0.0047 0.0046
LATT 1
SFAC C H Fe
UNIT 60 48 2
L.S. 40
PLAN 20
TEMP 19.85
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
OMIT 3 0 3
REM
REM
REM
WGHT 0.065600 0.308500
FVAR 0.78644
FE1 3 0.128115 0.293785 0.687752 11.00000 0.04489 0.05787 =
0.04392 -0.02435 -0.00431 0.00168
C24 1 0.524343 0.158763 0.260054 11.00000 0.04186 0.03476 =
0.03924 -0.01048 -0.01708 0.00657
C19 1 0.576631 0.406743 0.200647 11.00000 0.04284 0.03606 =
0.03841 -0.01588 -0.01421 0.00467
C29 1 0.631457 0.161175 0.157334 11.00000 0.05231 0.03344 =
0.04000 -0.01383 -0.01732 0.01162
C11 1 0.560045 0.267757 0.302298 11.00000 0.03855 0.04365 =
0.03239 -0.01532 -0.00704 0.00346
AFIX 13
H11 2 0.484487 0.266284 0.374092 11.00000 -1.20000
AFIX 0
C0AA 1 0.684943 0.409338 0.098383 11.00000 0.04271 0.03843 =
0.03886 -0.01485 -0.01053 0.00374
C13 1 0.714667 0.239404 0.314333 11.00000 0.04474 0.03698 =
0.04501 -0.01050 -0.01771 0.00118
C12 1 0.759935 0.271908 0.112156 11.00000 0.04309 0.04204 =
0.03741 -0.01308 -0.00149 0.00740
AFIX 13
H12 2 0.835496 0.273524 0.040316 11.00000 -1.20000
AFIX 0
C25 1 0.399632 0.066845 0.312054 11.00000 0.05012 0.04677 =
0.05099 -0.00867 -0.02087 -0.00208
AFIX 43
H25 2 0.328930 0.065318 0.380643 11.00000 -1.20000
AFIX 0
C18 1 0.822875 0.241066 0.211751 11.00000 0.04029 0.03738 =
0.05413 -0.01076 -0.01333 0.00422
C23 1 0.709852 0.526740 -0.002375 11.00000 0.05722 0.04480 =
0.04087 -0.01007 -0.01176 -0.00316
AFIX 43
H23 2 0.782854 0.529058 -0.070241 11.00000 -1.20000
AFIX 0
C20 1 0.492088 0.519893 0.201318 11.00000 0.05600 0.04508 =
0.05343 -0.02757 -0.01935 0.01240
AFIX 43
H20 2 0.419751 0.518205 0.269273 11.00000 -1.20000
AFIX 0
C28 1 0.613150 0.069885 0.107684 11.00000 0.08899 0.04457 =
0.05034 -0.02524 -0.03061 0.02066
AFIX 43
H28 2 0.685008 0.069557 0.040203 11.00000 -1.20000
AFIX 0
C22 1 0.625609 0.641265 -0.002047 11.00000 0.07291 0.03885 =
0.05406 -0.00827 -0.02864 0.00063
AFIX 43
H22 2 0.642461 0.721130 -0.069659 11.00000 -1.20000
AFIX 0
C21 1 0.516658 0.636894 0.098595 11.00000 0.07426 0.03876 =
0.06861 -0.02368 -0.03486 0.01818
AFIX 43
H21 2 0.458793 0.713322 0.097724 11.00000 -1.20000
AFIX 0
C14 1 0.752755 0.212921 0.413778 11.00000 0.07039 0.05011 =
0.05560 -0.01036 -0.03366 -0.00259
AFIX 43
H14 2 0.681211 0.213272 0.481386 11.00000 -1.20000
AFIX 0
C26 1 0.380730 -0.023850 0.260585 11.00000 0.08356 0.04783 =
0.07537 -0.01193 -0.04174 -0.01101
AFIX 43
H26 2 0.296537 -0.086216 0.294554 11.00000 -1.20000
AFIX 0
C27 1 0.486527 -0.021525 0.159302 11.00000 0.11187 0.04283 =
0.08066 -0.02789 -0.05641 0.00651
AFIX 43
H27 2 0.472673 -0.082144 0.125198 11.00000 -1.20000
AFIX 0
C17 1 0.968647 0.215201 0.209850 11.00000 0.03933 0.05426 =
0.09129 -0.01493 -0.01457 0.00449
AFIX 43
H17 2 1.041181 0.215747 0.142360 11.00000 -1.20000
AFIX 0
C1 1 0.305692 0.205059 0.612346 11.00000 0.06534 0.11479 =
0.05848 -0.03048 -0.00651 0.03516
AFIX 43
H1 2 0.347590 0.124926 0.650828 11.00000 -1.20000
AFIX 0
C5 1 0.195646 0.208459 0.564494 11.00000 0.08152 0.08752 =
0.06212 -0.04434 -0.00862 0.00935
AFIX 43
H5 2 0.149882 0.130535 0.565318 11.00000 -1.20000
AFIX 0
C4 1 0.163372 0.342983 0.515583 11.00000 0.08075 0.09317 =
0.05045 -0.02742 -0.01948 0.01377
AFIX 43
H4 2 0.092032 0.371763 0.477406 11.00000 -1.20000
AFIX 0
C16 1 1.005678 0.188209 0.310656 11.00000 0.05564 0.06272 =
0.13003 -0.01305 -0.05449 0.00520
AFIX 43
H16 2 1.104011 0.171519 0.309982 11.00000 -1.20000
AFIX 0
C6 1 -0.055622 0.182133 0.814299 11.00000 0.06883 0.10435 =
0.07565 -0.04047 0.01125 -0.02525
AFIX 43
H6 2 -0.102805 0.104620 0.815651 11.00000 -1.20000
AFIX 0
C15 1 0.899197 0.185911 0.410809 11.00000 0.08234 0.06693 =
0.09465 -0.01110 -0.06072 -0.00295
AFIX 43
H15 2 0.925792 0.165937 0.477581 11.00000 -1.20000
AFIX 0
C10 1 0.056416 0.178116 0.859266 11.00000 0.08768 0.13226 =
0.04556 -0.00882 0.00089 0.04094
AFIX 43
H10 2 0.099774 0.098371 0.896637 11.00000 -1.20000
AFIX 0
C7 1 -0.087267 0.313647 0.768199 11.00000 0.07261 0.16245 =
0.07045 -0.02015 0.00209 0.05966
AFIX 43
H7 2 -0.160767 0.342844 0.732229 11.00000 -1.20000
AFIX 0
C2 1 0.345352 0.344045 0.593554 11.00000 0.04923 0.21650 =
0.06912 -0.07781 0.01088 -0.03904
AFIX 43
H2 2 0.417028 0.373266 0.616948 11.00000 -1.20000
AFIX 0
C3 1 0.251814 0.430424 0.530850 11.00000 0.11765 0.07094 =
0.05903 -0.02466 0.02149 -0.01946
AFIX 43
H3 2 0.251211 0.527594 0.505298 11.00000 -1.20000
AFIX 0
C9 1 0.094868 0.316879 0.838908 11.00000 0.09124 0.26912 =
0.07433 -0.10883 0.01869 -0.07017
AFIX 43
H9 2 0.167938 0.347696 0.860095 11.00000 -1.20000
AFIX 0
C8 1 0.001316 0.398305 0.780705 11.00000 0.19813 0.07477 =
0.10667 -0.05632 0.07578 -0.02155
AFIX 13
H8 2 -0.001325 0.500482 0.755221 11.00000 -1.20000
AFIX 0
HKLF 4
REM smm543_a.res in P-1
REM wR2 = 0.1533, GooF = S = 1.028, Restrained GooF = 1.028 for all data
REM R1 = 0.0538 for 5288 Fo > 4sig(Fo) and 0.0733 for all 7220 data
REM 280 parameters refined using 0 restraints
END
WGHT 0.0656 0.3084
REM Highest difference peak 0.362, deepest hole -0.521, 1-sigma level 0.062
Q1 1 0.3159 0.4410 0.5804 11.00000 0.05 0.36
Q2 1 -0.0825 0.2606 0.7857 11.00000 0.05 0.35
Q3 1 0.3633 0.2869 0.6387 11.00000 0.05 0.32
Q4 1 -0.0415 0.3856 0.7710 11.00000 0.05 0.29
Q5 1 -0.0010 0.1716 0.8480 11.00000 0.05 0.24
Q6 1 0.3553 0.3194 0.5828 11.00000 0.05 0.23
Q7 1 0.0580 0.1240 0.8672 11.00000 0.05 0.23
Q8 1 -0.2018 0.2884 0.7089 11.00000 0.05 0.22
Q9 1 0.1373 0.4575 0.8104 11.00000 0.05 0.22
Q10 1 0.0446 0.0174 0.8882 11.00000 0.05 0.21
Q11 1 -0.0218 -0.0139 0.8630 11.00000 0.05 0.20
Q12 1 0.2038 0.0428 0.6388 11.00000 0.05 0.20
Q13 1 0.1205 0.2354 0.8554 11.00000 0.05 0.20
Q14 1 0.2161 0.2199 0.8954 11.00000 0.05 0.20
Q15 1 0.2207 0.5023 0.5058 11.00000 0.05 0.19
Q16 1 0.4615 0.1349 0.2773 11.00000 0.05 0.19
Q17 1 0.6321 0.4067 0.1490 11.00000 0.05 0.19
Q18 1 0.6448 0.2534 0.3113 11.00000 0.05 0.19
Q19 1 0.4455 -0.0423 0.2160 11.00000 0.05 0.18
Q20 1 0.3763 0.6983 0.1572 11.00000 0.05 0.18
;
_shelx_res_checksum 93012
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_3
_database_code_depnum_ccdc_archive 'CCDC 1839843'
loop_
_audit_author_name
_audit_author_address
'Ajeet Singh'
;Indian Institute of Technology Indore
India
;
_audit_update_record
;
2019-10-26 deposited with the CCDC. 2020-01-20 downloaded from the CCDC.
;
_audit_creation_date 2019-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic FCC2trip
_chemical_formula_moiety 'C24 H18 Fe2, 2(C20 H14)'
_chemical_formula_sum 'C64 H46 Fe2'
_chemical_formula_weight 926.71
_chemical_melting_point ?
_chemical_oxdiff_formula 'C40 H40 Fe2'
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'
_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 13.3320(15)
_cell_length_b 13.4018(12)
_cell_length_c 16.138(2)
_cell_angle_alpha 95.029(9)
_cell_angle_beta 105.145(11)
_cell_angle_gamma 119.521(10)
_cell_volume 2340.2(5)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 2268
_cell_measurement_temperature 298
_cell_measurement_theta_max 28.7986
_cell_measurement_theta_min 3.0286
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.662
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.79255
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour red
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.315
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 964
_exptl_crystal_preparation CHCl3-Hexane
_exptl_crystal_recrystallization_method CHCL3-Hexane
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.28
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1238
_diffrn_reflns_av_unetI/netI 0.1770
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 21024
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.000
_diffrn_reflns_theta_max 25.000
_diffrn_reflns_theta_min 3.035
_diffrn_ambient_temperature 298
_diffrn_detector_area_resol_mean 16.0309
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega 6.00 32.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 16.9534 -57.0000 30.0000 26
#__ type_ start__ end____ width___ exp.time_
2 omega 49.00 75.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 16.9534 0.0000 -30.0000 26
#__ type_ start__ end____ width___ exp.time_
3 omega 0.00 26.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 16.9534 0.0000 -30.0000 26
#__ type_ start__ end____ width___ exp.time_
4 omega -43.00 -12.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 16.9534 0.0000 -30.0000 31
#__ type_ start__ end____ width___ exp.time_
5 omega -56.00 43.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 16.9534 -37.0000 120.0000 99
#__ type_ start__ end____ width___ exp.time_
6 omega 36.00 92.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 16.9534 178.0000 90.0000 56
#__ type_ start__ end____ width___ exp.time_
7 omega 33.00 58.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 16.9534 -99.0000 -120.0000 25
#__ type_ start__ end____ width___ exp.time_
8 omega -11.00 52.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 16.9534 77.0000 90.0000 63
#__ type_ start__ end____ width___ exp.time_
9 omega -8.00 86.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 16.9534 37.0000 -60.0000 94
#__ type_ start__ end____ width___ exp.time_
10 omega -10.00 15.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 16.9534 -99.0000 -60.0000 25
#__ type_ start__ end____ width___ exp.time_
11 omega -78.00 -53.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- -18.9065 127.0000 42.0000 25
#__ type_ start__ end____ width___ exp.time_
12 omega -88.00 -53.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- -18.9065 143.0000 -148.0000 35
;
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0198524000
_diffrn_orient_matrix_UB_12 -0.0182612000
_diffrn_orient_matrix_UB_13 -0.0469813000
_diffrn_orient_matrix_UB_21 0.0046335000
_diffrn_orient_matrix_UB_22 0.0545201000
_diffrn_orient_matrix_UB_23 -0.0029484000
_diffrn_orient_matrix_UB_31 0.0620313000
_diffrn_orient_matrix_UB_32 0.0256166000
_diffrn_orient_matrix_UB_33 0.0026127000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3258
_reflns_number_total 8192
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.735
_refine_diff_density_min -0.380
_refine_diff_density_rms 0.087
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.021
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 595
_refine_ls_number_reflns 8192
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.2107
_refine_ls_R_factor_gt 0.0914
_refine_ls_restrained_S_all 1.021
_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^)+(0.0904P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1986
_refine_ls_wR_factor_ref 0.2736
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Ternary CH refined with riding coordinates:
C004(H004), C006(H006), C00E(H00E), C00G(H00G)
2.b Aromatic/amide H refined with riding coordinates:
C00C(H00C), C00H(H00H), C00M(H00M), C00P(H00P), C00R(H00R), C00S(H00S),
C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00Y(H00Y), C00Z(H00Z),
C011(H011), C012(H012), C013(H013), C014(H014), C015(H015), C016(H016),
C017(H017), C018(H018), C019(H019), C01A(H01A), C01B(H01B), C01C(H01C),
C01D(H01D), C01E(H01E), C01F(H01F), C01G(H01G), C01H(H01H), C01I(H01I),
C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01M), C01N(H01N), C01O(H01O),
C01P(H01P), C01Q(H01Q), C01R(H01R), C01S(H01S), C01T(H01T), C01U(H01U)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe01 Fe 0.20426(10) 0.94095(10) 0.54420(8) 0.0552(4) Uani 1 1 d . . . . .
Fe02 Fe -0.09214(10) 0.67464(10) -0.04722(8) 0.0593(4) Uani 1 1 d . . . . .
C003 C 0.5412(7) 0.7284(7) 0.9958(5) 0.0471(19) Uani 1 1 d . . . . .
C004 C 0.3520(7) 0.6516(7) 0.4141(5) 0.053(2) Uani 1 1 d . . . . .
H004 H 0.421295 0.724083 0.410056 0.064 Uiso 1 1 calc R . . . .
C005 C 0.2435(6) 0.5567(7) 0.5121(5) 0.047(2) Uani 1 1 d . . . . .
C006 C 0.1695(7) 0.4608(7) 0.4250(5) 0.051(2) Uani 1 1 d . . . . .
H006 H 0.099890 0.388259 0.428728 0.061 Uiso 1 1 calc R . . . .
C007 C 0.6427(7) 0.7560(7) 1.1515(5) 0.0492(19) Uani 1 1 d . . . . .
C008 C 0.3610(6) 0.5439(7) 0.3950(5) 0.0469(19) Uani 1 1 d . . . . .
C009 C 0.6475(6) 0.8295(6) 0.9948(5) 0.0442(18) Uani 1 1 d . . . . .
C00A C 0.1308(6) 0.5171(6) 0.3578(5) 0.0463(19) Uani 1 1 d . . . . .
C00B C 0.1100(7) 0.8827(8) 0.1186(7) 0.058(2) Uani 1 1 d . . . . .
C00C C 0.2220(7) 0.5535(8) 0.5906(6) 0.057(2) Uani 1 1 d . . . . .
H00C H 0.155434 0.485691 0.594758 0.068 Uiso 1 1 calc R . . . .
C00D C 0.2906(7) 1.0276(7) 0.4630(6) 0.055(2) Uani 1 1 d . . . . .
C00E C 0.7206(6) 0.9224(6) 1.0856(5) 0.0460(19) Uani 1 1 d . . . . .
H00E H 0.794779 0.993885 1.085773 0.055 Uiso 1 1 calc R . . . .
C00F C 0.5256(7) 0.8472(7) 1.1083(5) 0.050(2) Uani 1 1 d . . . . .
C00G C 0.5256(6) 0.7342(6) 1.0870(5) 0.050(2) Uani 1 1 d . . . . .
H00G H 0.451829 0.663211 1.087878 0.060 Uiso 1 1 calc R . . . .
C00H C 0.6390(7) 1.0562(7) 1.1183(5) 0.054(2) Uani 1 1 d . . . . .
H00H H 0.708371 1.123441 1.116617 0.065 Uiso 1 1 calc R . . . .
C00I C 0.2431(7) 0.9945(7) 0.3677(7) 0.061(2) Uani 1 1 d . . . . .
C00J C 0.2260(7) 0.6202(7) 0.3496(5) 0.050(2) Uani 1 1 d . . . . .
C00K C 0.3421(6) 0.6608(7) 0.5055(5) 0.0439(19) Uani 1 1 d . . . . .
C00L C 0.2042(7) 0.9657(7) 0.2884(7) 0.059(2) Uani 1 1 d . . . . .
C00M C 0.4174(7) 0.7564(7) 0.5769(6) 0.055(2) Uani 1 1 d . . . . .
H00M H 0.483120 0.824556 0.572352 0.066 Uiso 1 1 calc R . . . .
C00N C 0.7485(7) 0.8571(7) 1.1511(5) 0.050(2) Uani 1 1 d . . . . .
C00O C 0.6295(7) 0.9480(7) 1.1067(5) 0.0484(19) Uani 1 1 d . . . . .
C00P C 0.6756(7) 0.8387(7) 0.9203(6) 0.053(2) Uani 1 1 d . . . . .
H00P H 0.745195 0.906495 0.919511 0.064 Uiso 1 1 calc R . . . .
C00Q C 0.2621(6) 0.4403(6) 0.4013(5) 0.0441(18) Uani 1 1 d . . . . .
C00R C 0.2023(8) 0.6838(7) 0.2934(5) 0.061(2) Uani 1 1 d . . . . .
H00R H 0.267072 0.753134 0.289093 0.073 Uiso 1 1 calc R . . . .
C00S C 0.3401(9) 1.1125(8) 0.6084(7) 0.080(3) Uani 1 1 d . . . . .
H00S H 0.347394 1.157369 0.659545 0.096 Uiso 1 1 calc R . . . .
C00T C 0.4572(7) 0.5413(7) 0.3793(5) 0.054(2) Uani 1 1 d . . . . .
H00T H 0.523292 0.609974 0.375527 0.065 Uiso 1 1 calc R . . . .
C00U C 0.4309(8) 0.8546(8) 1.1232(5) 0.063(2) Uani 1 1 d . . . . .
H00U H 0.361329 0.787327 1.124692 0.076 Uiso 1 1 calc R . . . .
C00V C 0.2584(8) 0.3353(7) 0.3884(5) 0.059(2) Uani 1 1 d . . . . .
H00V H 0.190856 0.265819 0.389722 0.071 Uiso 1 1 calc R . . . .
C00W C 0.4645(7) 0.6348(7) 0.9217(6) 0.056(2) Uani 1 1 d . . . . .
H00W H 0.394627 0.567123 0.922456 0.067 Uiso 1 1 calc R . . . .
C00X C 0.1544(7) 0.9232(8) 0.1965(7) 0.063(2) Uani 1 1 d . . . . .
C00Y C 0.2984(8) 0.6501(9) 0.6635(6) 0.067(2) Uani 1 1 d . . . . .
H00Y H 0.284542 0.646805 0.717081 0.080 Uiso 1 1 calc R . . . .
C00Z C -0.1796(7) 0.5893(7) 0.0346(6) 0.063(2) Uani 1 1 d . . . . .
H00Z H -0.157811 0.619731 0.094963 0.075 Uiso 1 1 calc R . . . .
C010 C 0.0599(7) 0.8365(7) 0.0249(6) 0.060(2) Uani 1 1 d . . . . .
C011 C 0.3962(8) 0.7522(8) 0.6565(6) 0.065(2) Uani 1 1 d . . . . .
H011 H 0.447466 0.817799 0.705261 0.078 Uiso 1 1 calc R . . . .
C012 C 0.0098(7) 0.4778(7) 0.3067(5) 0.058(2) Uani 1 1 d . . . . .
H012 H -0.055490 0.408818 0.310938 0.070 Uiso 1 1 calc R . . . .
C013 C 0.0500(7) 0.7807(7) 0.4715(6) 0.064(2) Uani 1 1 d . . . . .
H013 H 0.027143 0.746673 0.411694 0.077 Uiso 1 1 calc R . . . .
C014 C 0.3902(8) 1.0421(10) 0.6063(7) 0.087(3) Uani 1 1 d . . . . .
H014 H 0.435139 1.031334 0.655404 0.104 Uiso 1 1 calc R . . . .
C015 C 0.3564(8) 0.3331(8) 0.3734(5) 0.064(2) Uani 1 1 d . . . . .
H015 H 0.355553 0.262979 0.366479 0.077 Uiso 1 1 calc R . . . .
C016 C 0.0816(8) 0.6442(8) 0.2432(6) 0.072(3) Uani 1 1 d . . . . .
H016 H 0.064859 0.686851 0.205354 0.086 Uiso 1 1 calc R . . . .
C017 C 0.2766(8) 1.1043(7) 0.5204(7) 0.070(3) Uani 1 1 d . . . . .
H017 H 0.234004 1.141287 0.503084 0.084 Uiso 1 1 calc R . . . .
C018 C 0.4952(8) 0.6448(8) 0.8455(6) 0.064(2) Uani 1 1 d . . . . .
H018 H 0.444979 0.582889 0.794176 0.077 Uiso 1 1 calc R . . . .
C019 C 0.5985(8) 0.7449(8) 0.8450(6) 0.062(2) Uani 1 1 d . . . . .
H019 H 0.617073 0.749925 0.793288 0.074 Uiso 1 1 calc R . . . .
C01A C 0.0179(8) 0.8546(9) 0.5062(8) 0.078(3) Uani 1 1 d . . . . .
H01A H -0.031254 0.878457 0.473403 0.093 Uiso 1 1 calc R . . . .
C01B C 0.6529(8) 0.6848(8) 1.2059(6) 0.065(2) Uani 1 1 d . . . . .
H01B H 0.582747 0.617630 1.206764 0.078 Uiso 1 1 calc R . . . .
C01C C -0.2596(8) 0.5995(9) -0.0342(7) 0.075(3) Uani 1 1 d . . . . .
H01C H -0.300373 0.637865 -0.028013 0.090 Uiso 1 1 calc R . . . .
C01D C 0.5447(8) 1.0638(8) 1.1323(5) 0.068(2) Uani 1 1 d . . . . .
H01D H 0.550553 1.136384 1.139282 0.082 Uiso 1 1 calc R . . . .
C01E C 0.4418(8) 0.9647(9) 1.1361(6) 0.067(2) Uani 1 1 d . . . . .
H01E H 0.379850 0.971148 1.147108 0.081 Uiso 1 1 calc R . . . .
C01F C 0.7699(9) 0.7149(9) 1.2595(6) 0.079(3) Uani 1 1 d . . . . .
H01F H 0.777375 0.668039 1.296870 0.095 Uiso 1 1 calc R . . . .
C01G C -0.0266(8) 0.8485(7) -0.0368(7) 0.069(3) Uani 1 1 d . . . . .
H01G H -0.062419 0.888789 -0.022303 0.083 Uiso 1 1 calc R . . . .
C01H C -0.1375(8) 0.5252(8) -0.0028(8) 0.076(3) Uani 1 1 d . . . . .
H01H H -0.082909 0.505808 0.028093 0.092 Uiso 1 1 calc R . . . .
C01I C 0.0906(8) 0.7697(9) -0.0264(7) 0.080(3) Uani 1 1 d . . . . .
H01I H 0.146124 0.747487 -0.003769 0.096 Uiso 1 1 calc R . . . .
C01J C 0.3609(7) 0.9908(8) 0.5172(6) 0.066(2) Uani 1 1 d . . . . .
H01J H 0.383956 0.940769 0.497058 0.079 Uiso 1 1 calc R . . . .
C01K C 0.4546(8) 0.4368(8) 0.3691(5) 0.063(2) Uani 1 1 d . . . . .
H01K H 0.519889 0.435864 0.359281 0.075 Uiso 1 1 calc R . . . .
C01L C 0.1212(8) 0.7672(8) 0.5415(8) 0.075(3) Uani 1 1 d . . . . .
H01L H 0.154481 0.721122 0.536515 0.090 Uiso 1 1 calc R . . . .
C01M C 0.8653(7) 0.8863(8) 1.2035(6) 0.065(2) Uani 1 1 d . . . . .
H01M H 0.935866 0.952871 1.202461 0.078 Uiso 1 1 calc R . . . .
C01N C -0.0126(8) 0.5416(8) 0.2500(6) 0.069(3) Uani 1 1 d . . . . .
H01N H -0.093379 0.514447 0.215740 0.083 Uiso 1 1 calc R . . . .
C01O C 0.8735(9) 0.8130(9) 1.2575(6) 0.075(3) Uani 1 1 d . . . . .
H01O H 0.950563 0.830886 1.292716 0.091 Uiso 1 1 calc R . . . .
C01P C 0.1373(9) 0.8310(10) 0.6204(8) 0.095(4) Uani 1 1 d . . . . .
H01P H 0.182446 0.836011 0.677099 0.114 Uiso 1 1 calc R . . . .
C01Q C 0.0225(10) 0.7437(10) -0.1162(8) 0.099(4) Uani 1 1 d . . . . .
H01Q H 0.025756 0.701698 -0.163442 0.119 Uiso 1 1 calc R . . . .
C01R C -0.2675(8) 0.5421(9) -0.1135(8) 0.090(3) Uani 1 1 d . . . . .
H01R H -0.314844 0.534993 -0.170032 0.108 Uiso 1 1 calc R . . . .
C01S C -0.0517(10) 0.7917(10) -0.1232(8) 0.097(4) Uani 1 1 d . . . . .
H01S H -0.106722 0.786533 -0.175163 0.117 Uiso 1 1 calc R . . . .
C01T C 0.0719(11) 0.8872(8) 0.5987(9) 0.092(4) Uani 1 1 d . . . . .
H01T H 0.065819 0.936809 0.638426 0.111 Uiso 1 1 calc R . . . .
C01U C -0.1921(11) 0.4966(8) -0.0937(9) 0.094(3) Uani 1 1 d . . . . .
H01U H -0.180671 0.454101 -0.135113 0.113 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe01 0.0565(7) 0.0483(8) 0.0567(9) 0.0160(7) 0.0204(6) 0.0246(6)
Fe02 0.0547(7) 0.0518(8) 0.0599(9) 0.0121(7) 0.0198(6) 0.0211(7)
C003 0.050(4) 0.054(5) 0.048(5) 0.021(5) 0.018(4) 0.033(4)
C004 0.051(4) 0.046(5) 0.070(6) 0.024(5) 0.023(4) 0.028(4)
C005 0.047(4) 0.061(6) 0.047(5) 0.021(5) 0.013(4) 0.039(4)
C006 0.047(4) 0.051(5) 0.063(6) 0.024(5) 0.022(4) 0.030(4)
C007 0.063(5) 0.047(5) 0.048(5) 0.010(4) 0.022(4) 0.036(4)
C008 0.052(4) 0.055(5) 0.052(5) 0.020(4) 0.022(4) 0.039(4)
C009 0.048(4) 0.048(5) 0.045(5) 0.009(4) 0.020(4) 0.030(4)
C00A 0.050(4) 0.042(5) 0.053(5) 0.011(4) 0.015(4) 0.031(4)
C00B 0.050(5) 0.054(6) 0.064(6) 0.024(5) 0.027(5) 0.020(4)
C00C 0.061(5) 0.063(6) 0.055(6) 0.014(5) 0.022(5) 0.039(5)
C00D 0.052(5) 0.054(5) 0.065(6) 0.020(5) 0.022(5) 0.030(4)
C00E 0.044(4) 0.041(5) 0.046(5) 0.007(4) 0.017(4) 0.019(4)
C00F 0.052(4) 0.053(5) 0.050(5) 0.015(4) 0.022(4) 0.029(4)
C00G 0.051(4) 0.041(5) 0.058(6) 0.016(4) 0.012(4) 0.027(4)
C00H 0.076(5) 0.041(5) 0.047(5) 0.007(4) 0.019(4) 0.034(5)
C00I 0.056(5) 0.045(5) 0.072(7) 0.016(6) 0.023(5) 0.020(4)
C00J 0.066(5) 0.056(5) 0.050(5) 0.021(4) 0.029(4) 0.043(5)
C00K 0.047(4) 0.053(5) 0.048(5) 0.014(4) 0.020(4) 0.036(4)
C00L 0.051(5) 0.047(5) 0.072(7) 0.019(6) 0.024(5) 0.019(4)
C00M 0.048(5) 0.066(6) 0.056(6) 0.005(5) 0.014(4) 0.038(5)
C00N 0.054(5) 0.049(5) 0.050(5) 0.007(4) 0.014(4) 0.033(4)
C00O 0.055(5) 0.052(5) 0.042(5) 0.014(4) 0.015(4) 0.031(4)
C00P 0.066(5) 0.052(5) 0.056(6) 0.019(5) 0.024(5) 0.040(5)
C00Q 0.048(4) 0.039(5) 0.043(5) 0.004(4) 0.012(4) 0.024(4)
C00R 0.081(6) 0.056(6) 0.054(6) 0.021(5) 0.027(5) 0.040(5)
C00S 0.087(7) 0.050(6) 0.064(7) 0.005(5) 0.022(6) 0.014(5)
C00T 0.062(5) 0.058(6) 0.047(5) 0.011(5) 0.023(4) 0.034(5)
C00U 0.077(6) 0.078(7) 0.050(6) 0.014(5) 0.027(5) 0.051(6)
C00V 0.075(6) 0.048(5) 0.055(6) 0.010(5) 0.020(5) 0.036(5)
C00W 0.059(5) 0.048(5) 0.064(6) 0.015(5) 0.021(5) 0.031(4)
C00X 0.057(5) 0.051(6) 0.066(7) 0.017(6) 0.026(5) 0.015(5)
C00Y 0.076(6) 0.095(8) 0.058(6) 0.035(6) 0.028(5) 0.061(6)
C00Z 0.058(5) 0.059(6) 0.068(6) 0.027(5) 0.022(5) 0.028(5)
C010 0.062(5) 0.060(6) 0.054(6) 0.021(5) 0.024(5) 0.028(5)
C011 0.066(6) 0.082(7) 0.055(6) 0.001(5) 0.010(5) 0.053(6)
C012 0.061(5) 0.066(6) 0.060(6) 0.010(5) 0.020(5) 0.045(5)
C013 0.053(5) 0.055(6) 0.067(7) 0.014(5) 0.013(5) 0.021(5)
C014 0.068(6) 0.086(8) 0.076(8) 0.035(7) 0.013(6) 0.024(6)
C015 0.086(6) 0.066(6) 0.065(6) 0.021(5) 0.029(5) 0.056(6)
C016 0.090(7) 0.067(7) 0.068(7) 0.022(6) 0.019(6) 0.053(6)
C017 0.078(6) 0.043(5) 0.091(8) 0.030(6) 0.034(6) 0.029(5)
C018 0.078(6) 0.063(6) 0.052(6) 0.004(5) 0.009(5) 0.045(5)
C019 0.096(7) 0.070(7) 0.044(6) 0.019(5) 0.026(5) 0.061(6)
C01A 0.057(6) 0.074(7) 0.117(10) 0.033(7) 0.035(6) 0.042(6)
C01B 0.085(6) 0.066(6) 0.082(7) 0.035(6) 0.047(6) 0.055(5)
C01C 0.058(6) 0.084(7) 0.091(8) 0.020(7) 0.036(6) 0.040(6)
C01D 0.091(7) 0.078(7) 0.060(6) 0.007(5) 0.023(5) 0.066(6)
C01E 0.057(5) 0.085(7) 0.070(7) 0.008(6) 0.022(5) 0.047(6)
C01F 0.098(7) 0.093(8) 0.073(7) 0.032(6) 0.033(6) 0.066(7)
C01G 0.071(6) 0.046(6) 0.074(7) 0.020(6) 0.013(5) 0.024(5)
C01H 0.066(6) 0.059(6) 0.119(10) 0.027(7) 0.045(7) 0.038(5)
C01I 0.057(5) 0.083(7) 0.091(8) 0.011(7) 0.039(6) 0.027(6)
C01J 0.058(5) 0.068(6) 0.073(7) 0.027(6) 0.031(5) 0.031(5)
C01K 0.072(6) 0.083(7) 0.054(6) 0.006(5) 0.019(5) 0.059(6)
C01L 0.068(6) 0.041(6) 0.099(9) 0.031(6) 0.021(6) 0.019(5)
C01M 0.063(5) 0.070(6) 0.070(6) 0.008(5) 0.017(5) 0.046(5)
C01N 0.073(6) 0.074(7) 0.081(7) 0.029(6) 0.020(5) 0.056(6)
C01O 0.084(7) 0.101(8) 0.060(6) 0.014(6) 0.014(5) 0.069(7)
C01P 0.082(7) 0.075(8) 0.062(8) 0.032(7) 0.009(6) 0.002(6)
C01Q 0.074(7) 0.084(8) 0.069(8) -0.010(7) 0.037(7) -0.008(6)
C01R 0.057(6) 0.069(7) 0.090(9) 0.015(7) 0.009(6) 0.003(6)
C01S 0.083(7) 0.073(8) 0.084(9) 0.036(7) 0.017(7) 0.009(6)
C01T 0.111(9) 0.052(6) 0.104(10) 0.002(7) 0.075(8) 0.021(7)
C01U 0.102(9) 0.038(6) 0.112(11) -0.006(7) 0.045(8) 0.016(6)
_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
Fe01 C00D 2.032(8) . ?
Fe01 C00S 2.034(9) . ?
Fe01 C013 2.040(8) . ?
Fe01 C014 2.035(9) . ?
Fe01 C017 2.032(8) . ?
Fe01 C01A 2.034(8) . ?
Fe01 C01J 2.038(8) . ?
Fe01 C01L 2.016(8) . ?
Fe01 C01P 2.019(9) . ?
Fe01 C01T 2.019(9) . ?
Fe02 C00Z 2.041(8) . ?
Fe02 C010 2.039(9) . ?
Fe02 C01C 2.027(8) . ?
Fe02 C01G 2.017(8) . ?
Fe02 C01H 2.043(9) . ?
Fe02 C01I 2.027(8) . ?
Fe02 C01Q 2.027(9) . ?
Fe02 C01R 2.009(9) . ?
Fe02 C01S 2.026(9) . ?
Fe02 C01U 2.016(9) . ?
C003 C009 1.402(9) . ?
C003 C00G 1.541(10) . ?
C003 C00W 1.372(10) . ?
C004 H004 0.9800 . ?
C004 C008 1.518(10) . ?
C004 C00J 1.548(10) . ?
C004 C00K 1.514(10) . ?
C005 C006 1.520(10) . ?
C005 C00C 1.369(10) . ?
C005 C00K 1.406(9) . ?
C006 H006 0.9800 . ?
C006 C00A 1.499(9) . ?
C006 C00Q 1.519(9) . ?
C007 C00G 1.500(10) . ?
C007 C00N 1.396(10) . ?
C007 C01B 1.383(10) . ?
C008 C00Q 1.402(9) . ?
C008 C00T 1.387(9) . ?
C009 C00E 1.545(10) . ?
C009 C00P 1.348(9) . ?
C00A C00J 1.389(9) . ?
C00A C012 1.397(9) . ?
C00B C00X 1.183(11) . ?
C00B C010 1.421(12) . ?
C00C H00C 0.9300 . ?
C00C C00Y 1.381(11) . ?
C00D C00I 1.435(12) . ?
C00D C017 1.437(11) . ?
C00D C01J 1.411(10) . ?
C00E H00E 0.9800 . ?
C00E C00N 1.516(10) . ?
C00E C00O 1.521(9) . ?
C00F C00G 1.523(10) . ?
C00F C00O 1.387(10) . ?
C00F C00U 1.394(9) . ?
C00G H00G 0.9800 . ?
C00H H00H 0.9300 . ?
C00H C00O 1.384(10) . ?
C00H C01D 1.383(10) . ?
C00I C00L 1.194(11) . ?
C00J C00R 1.379(10) . ?
C00K C00M 1.358(10) . ?
C00L C00X 1.389(13) . ?
C00M H00M 0.9300 . ?
C00M C011 1.385(10) . ?
C00N C01M 1.395(10) . ?
C00P H00P 0.9300 . ?
C00P C019 1.385(10) . ?
C00Q C00V 1.380(10) . ?
C00R H00R 0.9300 . ?
C00R C016 1.390(10) . ?
C00S H00S 0.9300 . ?
C00S C014 1.403(12) . ?
C00S C017 1.414(12) . ?
C00T H00T 0.9300 . ?
C00T C01K 1.378(10) . ?
C00U H00U 0.9300 . ?
C00U C01E 1.400(11) . ?
C00V H00V 0.9300 . ?
C00V C015 1.404(10) . ?
C00W H00W 0.9300 . ?
C00W C018 1.392(10) . ?
C00Y H00Y 0.9300 . ?
C00Y C011 1.390(11) . ?
C00Z H00Z 0.9300 . ?
C00Z C01C 1.392(11) . ?
C00Z C01H 1.408(11) . ?
C010 C01G 1.399(11) . ?
C010 C01I 1.436(12) . ?
C011 H011 0.9300 . ?
C012 H012 0.9300 . ?
C012 C01N 1.380(10) . ?
C013 H013 0.9300 . ?
C013 C01A 1.387(12) . ?
C013 C01L 1.362(11) . ?
C014 H014 0.9300 . ?
C014 C01J 1.401(12) . ?
C015 H015 0.9300 . ?
C015 C01K 1.386(10) . ?
C016 H016 0.9300 . ?
C016 C01N 1.370(10) . ?
C017 H017 0.9300 . ?
C018 H018 0.9300 . ?
C018 C019 1.372(10) . ?
C019 H019 0.9300 . ?
C01A H01A 0.9300 . ?
C01A C01T 1.397(13) . ?
C01B H01B 0.9300 . ?
C01B C01F 1.399(11) . ?
C01C H01C 0.9300 . ?
C01C C01R 1.384(13) . ?
C01D H01D 0.9300 . ?
C01D C01E 1.383(11) . ?
C01E H01E 0.9300 . ?
C01F H01F 0.9300 . ?
C01F C01O 1.371(11) . ?
C01G H01G 0.9300 . ?
C01G C01S 1.398(13) . ?
C01H H01H 0.9300 . ?
C01H C01U 1.378(13) . ?
C01I H01I 0.9300 . ?
C01I C01Q 1.399(13) . ?
C01J H01J 0.9300 . ?
C01K H01K 0.9300 . ?
C01L H01L 0.9300 . ?
C01L C01P 1.372(13) . ?
C01M H01M 0.9300 . ?
C01M C01O 1.393(11) . ?
C01N H01N 0.9300 . ?
C01O H01O 0.9300 . ?
C01P H01P 0.9300 . ?
C01P C01T 1.410(14) . ?
C01Q H01Q 0.9300 . ?
C01Q C01S 1.410(14) . ?
C01R H01R 0.9300 . ?
C01R C01U 1.399(13) . ?
C01S H01S 0.9300 . ?
C01T H01T 0.9300 . ?
C01U H01U 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C00D Fe01 C00S 68.4(4) . . ?
C00D Fe01 C013 109.9(4) . . ?
C00D Fe01 C014 68.3(3) . . ?
C00D Fe01 C01A 119.9(4) . . ?
C00D Fe01 C01J 40.6(3) . . ?
C00S Fe01 C013 170.0(4) . . ?
C00S Fe01 C014 40.3(4) . . ?
C00S Fe01 C01J 67.7(4) . . ?
C014 Fe01 C013 149.1(5) . . ?
C014 Fe01 C01J 40.2(3) . . ?
C017 Fe01 C00D 41.4(3) . . ?
C017 Fe01 C00S 40.7(3) . . ?
C017 Fe01 C013 131.6(4) . . ?
C017 Fe01 C014 68.7(4) . . ?
C017 Fe01 C01A 111.0(4) . . ?
C017 Fe01 C01J 68.8(3) . . ?
C01A Fe01 C00S 131.8(5) . . ?
C01A Fe01 C013 39.8(3) . . ?
C01A Fe01 C014 168.1(5) . . ?
C01A Fe01 C01J 151.6(4) . . ?
C01J Fe01 C013 117.8(4) . . ?
C01L Fe01 C00D 129.3(4) . . ?
C01L Fe01 C00S 149.4(4) . . ?
C01L Fe01 C013 39.2(3) . . ?
C01L Fe01 C014 116.5(4) . . ?
C01L Fe01 C017 168.7(4) . . ?
C01L Fe01 C01A 66.2(4) . . ?
C01L Fe01 C01J 108.1(4) . . ?
C01L Fe01 C01P 39.8(4) . . ?
C01L Fe01 C01T 67.1(4) . . ?
C01P Fe01 C00D 165.6(5) . . ?
C01P Fe01 C00S 116.9(4) . . ?
C01P Fe01 C013 67.3(4) . . ?
C01P Fe01 C014 106.4(4) . . ?
C01P Fe01 C017 150.8(5) . . ?
C01P Fe01 C01A 67.7(4) . . ?
C01P Fe01 C01J 127.0(5) . . ?
C01T Fe01 C00D 152.6(5) . . ?
C01T Fe01 C00S 109.2(4) . . ?
C01T Fe01 C013 67.6(4) . . ?
C01T Fe01 C014 128.6(5) . . ?
C01T Fe01 C017 118.5(4) . . ?
C01T Fe01 C01A 40.3(4) . . ?
C01T Fe01 C01J 165.9(5) . . ?
C01T Fe01 C01P 40.9(4) . . ?
C00Z Fe02 C01H 40.3(3) . . ?
C010 Fe02 C00Z 109.6(3) . . ?
C010 Fe02 C01H 122.1(4) . . ?
C01C Fe02 C00Z 40.0(3) . . ?
C01C Fe02 C010 126.2(4) . . ?
C01C Fe02 C01H 67.8(4) . . ?
C01G Fe02 C00Z 121.2(4) . . ?
C01G Fe02 C010 40.3(3) . . ?
C01G Fe02 C01C 107.7(4) . . ?
C01G Fe02 C01H 156.2(5) . . ?
C01G Fe02 C01I 67.9(4) . . ?
C01G Fe02 C01Q 67.7(4) . . ?
C01G Fe02 C01S 40.5(4) . . ?
C01I Fe02 C00Z 128.9(4) . . ?
C01I Fe02 C010 41.4(3) . . ?
C01I Fe02 C01C 165.2(4) . . ?
C01I Fe02 C01H 110.1(4) . . ?
C01I Fe02 C01Q 40.4(4) . . ?
C01Q Fe02 C00Z 165.4(5) . . ?
C01Q Fe02 C010 68.8(4) . . ?
C01Q Fe02 C01C 152.7(5) . . ?
C01Q Fe02 C01H 127.2(5) . . ?
C01R Fe02 C00Z 67.2(4) . . ?
C01R Fe02 C010 162.3(5) . . ?
C01R Fe02 C01C 40.1(4) . . ?
C01R Fe02 C01G 125.0(5) . . ?
C01R Fe02 C01H 67.6(4) . . ?
C01R Fe02 C01I 154.1(5) . . ?
C01R Fe02 C01Q 118.8(5) . . ?
C01R Fe02 C01S 105.7(4) . . ?
C01R Fe02 C01U 40.7(4) . . ?
C01S Fe02 C00Z 153.5(5) . . ?
C01S Fe02 C010 68.9(4) . . ?
C01S Fe02 C01C 118.0(5) . . ?
C01S Fe02 C01H 162.9(5) . . ?
C01S Fe02 C01I 68.6(4) . . ?
C01S Fe02 C01Q 40.7(4) . . ?
C01U Fe02 C00Z 67.1(4) . . ?
C01U Fe02 C010 156.0(5) . . ?
C01U Fe02 C01C 67.7(4) . . ?
C01U Fe02 C01G 162.4(5) . . ?
C01U Fe02 C01H 39.7(4) . . ?
C01U Fe02 C01I 120.7(5) . . ?
C01U Fe02 C01Q 108.0(5) . . ?
C01U Fe02 C01S 125.2(5) . . ?
C009 C003 C00G 113.1(7) . . ?
C00W C003 C009 121.1(7) . . ?
C00W C003 C00G 125.7(7) . . ?
C008 C004 H004 112.8 . . ?
C008 C004 C00J 107.0(6) . . ?
C00J C004 H004 112.8 . . ?
C00K C004 H004 112.8 . . ?
C00K C004 C008 105.6(6) . . ?
C00K C004 C00J 105.2(6) . . ?
C00C C005 C006 128.2(7) . . ?
C00C C005 C00K 119.4(8) . . ?
C00K C005 C006 112.4(7) . . ?
C005 C006 H006 113.0 . . ?
C00A C006 C005 105.4(6) . . ?
C00A C006 H006 113.0 . . ?
C00A C006 C00Q 106.9(6) . . ?
C00Q C006 C005 105.0(6) . . ?
C00Q C006 H006 113.0 . . ?
C00N C007 C00G 113.7(7) . . ?
C01B C007 C00G 126.4(7) . . ?
C01B C007 C00N 119.9(7) . . ?
C00Q C008 C004 112.8(6) . . ?
C00T C008 C004 127.3(7) . . ?
C00T C008 C00Q 119.8(7) . . ?
C003 C009 C00E 112.1(7) . . ?
C00P C009 C003 120.9(8) . . ?
C00P C009 C00E 127.1(7) . . ?
C00J C00A C006 115.4(6) . . ?
C00J C00A C012 118.6(7) . . ?
C012 C00A C006 126.0(7) . . ?
C00X C00B C010 178.4(9) . . ?
C005 C00C H00C 119.7 . . ?
C005 C00C C00Y 120.5(8) . . ?
C00Y C00C H00C 119.7 . . ?
C00I C00D Fe01 126.6(6) . . ?
C00I C00D C017 126.7(8) . . ?
C017 C00D Fe01 69.3(4) . . ?
C01J C00D Fe01 69.9(5) . . ?
C01J C00D C00I 125.6(9) . . ?
C01J C00D C017 107.7(8) . . ?
C009 C00E H00E 113.0 . . ?
C00N C00E C009 104.8(6) . . ?
C00N C00E H00E 113.0 . . ?
C00N C00E C00O 107.2(6) . . ?
C00O C00E C009 105.3(6) . . ?
C00O C00E H00E 113.0 . . ?
C00O C00F C00G 113.5(6) . . ?
C00O C00F C00U 120.2(8) . . ?
C00U C00F C00G 126.2(7) . . ?
C003 C00G H00G 113.1 . . ?
C007 C00G C003 105.4(6) . . ?
C007 C00G C00F 106.6(6) . . ?
C007 C00G H00G 113.1 . . ?
C00F C00G C003 104.8(6) . . ?
C00F C00G H00G 113.1 . . ?
C00O C00H H00H 120.2 . . ?
C00O C00H C01D 119.7(8) . . ?
C01D C00H H00H 120.2 . . ?
C00L C00I C00D 178.9(10) . . ?
C00A C00J C004 110.7(6) . . ?
C00R C00J C004 128.1(7) . . ?
C00R C00J C00A 121.1(7) . . ?
C005 C00K C004 113.1(7) . . ?
C00M C00K C004 126.4(7) . . ?
C00M C00K C005 120.4(7) . . ?
C00I C00L C00X 175.6(10) . . ?
C00K C00M H00M 120.0 . . ?
C00K C00M C011 120.0(8) . . ?
C011 C00M H00M 120.0 . . ?
C007 C00N C00E 112.8(6) . . ?
C01M C00N C007 120.9(7) . . ?
C01M C00N C00E 126.1(7) . . ?
C00F C00O C00E 113.0(7) . . ?
C00H C00O C00E 126.5(7) . . ?
C00H C00O C00F 120.3(7) . . ?
C009 C00P H00P 120.7 . . ?
C009 C00P C019 118.6(8) . . ?
C019 C00P H00P 120.7 . . ?
C008 C00Q C006 112.9(6) . . ?
C00V C00Q C006 127.1(7) . . ?
C00V C00Q C008 120.0(7) . . ?
C00J C00R H00R 120.1 . . ?
C00J C00R C016 119.9(8) . . ?
C016 C00R H00R 120.1 . . ?
Fe01 C00S H00S 126.7 . . ?
C014 C00S Fe01 69.9(6) . . ?
C014 C00S H00S 125.5 . . ?
C014 C00S C017 109.1(9) . . ?
C017 C00S Fe01 69.6(5) . . ?
C017 C00S H00S 125.5 . . ?
C008 C00T H00T 120.1 . . ?
C01K C00T C008 119.9(7) . . ?
C01K C00T H00T 120.1 . . ?
C00F C00U H00U 120.4 . . ?
C00F C00U C01E 119.2(8) . . ?
C01E C00U H00U 120.4 . . ?
C00Q C00V H00V 120.0 . . ?
C00Q C00V C015 120.1(7) . . ?
C015 C00V H00V 120.0 . . ?
C003 C00W H00W 121.3 . . ?
C003 C00W C018 117.5(7) . . ?
C018 C00W H00W 121.3 . . ?
C00B C00X C00L 177.5(10) . . ?
C00C C00Y H00Y 120.2 . . ?
C00C C00Y C011 119.6(8) . . ?
C011 C00Y H00Y 120.2 . . ?
Fe02 C00Z H00Z 126.4 . . ?
C01C C00Z Fe02 69.4(5) . . ?
C01C C00Z H00Z 125.8 . . ?
C01C C00Z C01H 108.3(9) . . ?
C01H C00Z Fe02 69.9(5) . . ?
C01H C00Z H00Z 125.8 . . ?
C00B C010 Fe02 127.7(6) . . ?
C00B C010 C01I 126.6(9) . . ?
C01G C010 Fe02 69.0(5) . . ?
C01G C010 C00B 127.7(9) . . ?
C01G C010 C01I 105.7(9) . . ?
C01I C010 Fe02 68.9(5) . . ?
C00M C011 C00Y 120.1(9) . . ?
C00M C011 H011 120.0 . . ?
C00Y C011 H011 120.0 . . ?
C00A C012 H012 120.1 . . ?
C01N C012 C00A 119.8(8) . . ?
C01N C012 H012 120.1 . . ?
Fe01 C013 H013 125.9 . . ?
C01A C013 Fe01 69.8(5) . . ?
C01A C013 H013 126.4 . . ?
C01L C013 Fe01 69.4(5) . . ?
C01L C013 H013 126.4 . . ?
C01L C013 C01A 107.2(9) . . ?
Fe01 C014 H014 125.8 . . ?
C00S C014 Fe01 69.8(5) . . ?
C00S C014 H014 126.0 . . ?
C01J C014 Fe01 70.0(5) . . ?
C01J C014 C00S 108.1(9) . . ?
C01J C014 H014 126.0 . . ?
C00V C015 H015 120.5 . . ?
C01K C015 C00V 119.1(8) . . ?
C01K C015 H015 120.5 . . ?
C00R C016 H016 120.4 . . ?
C01N C016 C00R 119.3(8) . . ?
C01N C016 H016 120.4 . . ?
Fe01 C017 H017 125.8 . . ?
C00D C017 Fe01 69.3(5) . . ?
C00D C017 H017 126.7 . . ?
C00S C017 Fe01 69.7(5) . . ?
C00S C017 C00D 106.6(9) . . ?
C00S C017 H017 126.7 . . ?
C00W C018 H018 119.6 . . ?
C019 C018 C00W 120.9(8) . . ?
C019 C018 H018 119.6 . . ?
C00P C019 H019 119.4 . . ?
C018 C019 C00P 121.1(8) . . ?
C018 C019 H019 119.4 . . ?
Fe01 C01A H01A 126.1 . . ?
C013 C01A Fe01 70.4(5) . . ?
C013 C01A H01A 125.8 . . ?
C013 C01A C01T 108.4(9) . . ?
C01T C01A Fe01 69.3(5) . . ?
C01T C01A H01A 125.8 . . ?
C007 C01B H01B 120.4 . . ?
C007 C01B C01F 119.3(8) . . ?
C01F C01B H01B 120.4 . . ?
Fe02 C01C H01C 125.7 . . ?
C00Z C01C Fe02 70.5(5) . . ?
C00Z C01C H01C 126.2 . . ?
C01R C01C Fe02 69.2(5) . . ?
C01R C01C C00Z 107.7(9) . . ?
C01R C01C H01C 126.2 . . ?
C00H C01D H01D 119.7 . . ?
C01E C01D C00H 120.6(8) . . ?
C01E C01D H01D 119.7 . . ?
C00U C01E H01E 120.0 . . ?
C01D C01E C00U 119.9(8) . . ?
C01D C01E H01E 120.0 . . ?
C01B C01F H01F 119.7 . . ?
C01O C01F C01B 120.5(9) . . ?
C01O C01F H01F 119.7 . . ?
Fe02 C01G H01G 126.2 . . ?
C010 C01G Fe02 70.7(5) . . ?
C010 C01G H01G 124.6 . . ?
C01S C01G Fe02 70.1(6) . . ?
C01S C01G C010 110.7(9) . . ?
C01S C01G H01G 124.6 . . ?
Fe02 C01H H01H 126.3 . . ?
C00Z C01H Fe02 69.8(5) . . ?
C00Z C01H H01H 126.4 . . ?
C01U C01H Fe02 69.1(6) . . ?
C01U C01H C00Z 107.2(9) . . ?
C01U C01H H01H 126.4 . . ?
Fe02 C01I H01I 126.1 . . ?
C010 C01I Fe02 69.8(5) . . ?
C010 C01I H01I 125.9 . . ?
C01Q C01I Fe02 69.8(5) . . ?
C01Q C01I C010 108.3(10) . . ?
C01Q C01I H01I 125.9 . . ?
Fe01 C01J H01J 126.6 . . ?
C00D C01J Fe01 69.5(4) . . ?
C00D C01J H01J 125.7 . . ?
C014 C01J Fe01 69.8(5) . . ?
C014 C01J C00D 108.6(9) . . ?
C014 C01J H01J 125.7 . . ?
C00T C01K C015 121.1(7) . . ?
C00T C01K H01K 119.4 . . ?
C015 C01K H01K 119.4 . . ?
Fe01 C01L H01L 125.4 . . ?
C013 C01L Fe01 71.4(5) . . ?
C013 C01L H01L 124.6 . . ?
C013 C01L C01P 110.8(10) . . ?
C01P C01L Fe01 70.2(6) . . ?
C01P C01L H01L 124.6 . . ?
C00N C01M H01M 120.9 . . ?
C01O C01M C00N 118.2(8) . . ?
C01O C01M H01M 120.9 . . ?
C012 C01N H01N 119.3 . . ?
C016 C01N C012 121.4(8) . . ?
C016 C01N H01N 119.3 . . ?
C01F C01O C01M 121.2(8) . . ?
C01F C01O H01O 119.4 . . ?
C01M C01O H01O 119.4 . . ?
Fe01 C01P H01P 125.3 . . ?
C01L C01P Fe01 70.0(5) . . ?
C01L C01P H01P 126.8 . . ?
C01L C01P C01T 106.5(9) . . ?
C01T C01P Fe01 69.5(5) . . ?
C01T C01P H01P 126.8 . . ?
Fe02 C01Q H01Q 126.5 . . ?
C01I C01Q Fe02 69.8(5) . . ?
C01I C01Q H01Q 125.7 . . ?
C01I C01Q C01S 108.6(10) . . ?
C01S C01Q Fe02 69.6(6) . . ?
C01S C01Q H01Q 125.7 . . ?
Fe02 C01R H01R 125.1 . . ?
C01C C01R Fe02 70.7(6) . . ?
C01C C01R H01R 125.9 . . ?
C01C C01R C01U 108.1(10) . . ?
C01U C01R Fe02 69.9(5) . . ?
C01U C01R H01R 125.9 . . ?
Fe02 C01S H01S 125.8 . . ?
C01G C01S Fe02 69.4(5) . . ?
C01G C01S C01Q 106.7(10) . . ?
C01G C01S H01S 126.7 . . ?
C01Q C01S Fe02 69.7(6) . . ?
C01Q C01S H01S 126.7 . . ?
Fe01 C01T H01T 125.2 . . ?
C01A C01T Fe01 70.4(5) . . ?
C01A C01T C01P 107.2(9) . . ?
C01A C01T H01T 126.4 . . ?
C01P C01T Fe01 69.6(6) . . ?
C01P C01T H01T 126.4 . . ?
Fe02 C01U H01U 125.3 . . ?
C01H C01U Fe02 71.2(6) . . ?
C01H C01U C01R 108.6(10) . . ?
C01H C01U H01U 125.7 . . ?
C01R C01U Fe02 69.4(6) . . ?
C01R C01U H01U 125.7 . . ?
_shelx_res_file
;
TITL smm881_a.res in P-1
smm881.res
created by SHELXL-2018/3 at 14:11:41 on 26-Oct-2019
REM Old TITL SMM881 in P-1
REM SHELXT solution in P-1
REM R1 0.245, Rweak 0.026, Alpha 0.096, Orientation as input
REM Formula found by SHELXT: C64 Fe2
CELL 0.71073 13.332 13.4018 16.1384 95.029 105.145 119.521
ZERR 2 0.0015 0.0012 0.0021 0.009 0.011 0.01
LATT 1
SFAC C H Fe
UNIT 128 92 4
L.S. 30
PLAN 20
TEMP 24.85
BOND $H
LIST 6
fmap 2
acta
OMIT -3 50
OMIT 3 3 3
OMIT 1 -7 7
OMIT -14 10 14
OMIT -8 2 2
OMIT -8 6 18
OMIT -3 -3 9
OMIT -1 -5 7
OMIT 5 0 0
OMIT 2 -8 2
OMIT 7 3 4
OMIT -1 -5 5
OMIT 2 4 0
OMIT 3 -9 9
OMIT 0 -6 2
OMIT -7 7 7
REM
REM
REM
WGHT 0.090400
FVAR 0.33508
FE01 3 0.204261 0.940946 0.544195 11.00000 0.05653 0.04827 =
0.05666 0.01604 0.02037 0.02458
FE02 3 -0.092141 0.674640 -0.047218 11.00000 0.05470 0.05185 =
0.05994 0.01207 0.01981 0.02111
C003 1 0.541211 0.728435 0.995771 11.00000 0.04998 0.05380 =
0.04783 0.02150 0.01775 0.03341
C004 1 0.351976 0.651591 0.414132 11.00000 0.05080 0.04590 =
0.06966 0.02384 0.02342 0.02756
AFIX 13
H004 2 0.421295 0.724083 0.410056 11.00000 -1.20000
AFIX 0
C005 1 0.243515 0.556683 0.512103 11.00000 0.04663 0.06117 =
0.04741 0.02145 0.01329 0.03863
C006 1 0.169512 0.460774 0.424977 11.00000 0.04730 0.05076 =
0.06334 0.02354 0.02156 0.02964
AFIX 13
H006 2 0.099890 0.388259 0.428728 11.00000 -1.20000
AFIX 0
C007 1 0.642672 0.756019 1.151471 11.00000 0.06330 0.04685 =
0.04815 0.00993 0.02203 0.03612
C008 1 0.360960 0.543918 0.394993 11.00000 0.05242 0.05519 =
0.05158 0.01993 0.02245 0.03874
C009 1 0.647489 0.829510 0.994821 11.00000 0.04776 0.04755 =
0.04545 0.00861 0.01981 0.03001
C00A 1 0.130775 0.517098 0.357805 11.00000 0.05036 0.04241 =
0.05305 0.01053 0.01503 0.03144
C00B 1 0.110042 0.882740 0.118605 11.00000 0.04989 0.05379 =
0.06430 0.02391 0.02660 0.01987
C00C 1 0.222012 0.553460 0.590574 11.00000 0.06134 0.06279 =
0.05545 0.01354 0.02234 0.03861
AFIX 43
H00C 2 0.155434 0.485691 0.594758 11.00000 -1.20000
AFIX 0
C00D 1 0.290642 1.027606 0.462990 11.00000 0.05167 0.05369 =
0.06481 0.02044 0.02203 0.03019
C00E 1 0.720628 0.922401 1.085650 11.00000 0.04427 0.04144 =
0.04636 0.00668 0.01654 0.01924
AFIX 13
H00E 2 0.794779 0.993885 1.085773 11.00000 -1.20000
AFIX 0
C00F 1 0.525611 0.847190 1.108275 11.00000 0.05202 0.05286 =
0.05004 0.01454 0.02205 0.02936
C00G 1 0.525636 0.734201 1.087023 11.00000 0.05076 0.04140 =
0.05756 0.01588 0.01238 0.02721
AFIX 13
H00G 2 0.451829 0.663211 1.087878 11.00000 -1.20000
AFIX 0
C00H 1 0.638958 1.056171 1.118278 11.00000 0.07569 0.04124 =
0.04710 0.00703 0.01908 0.03404
AFIX 43
H00H 2 0.708371 1.123441 1.116617 11.00000 -1.20000
AFIX 0
C00I 1 0.243111 0.994466 0.367670 11.00000 0.05590 0.04542 =
0.07194 0.01612 0.02344 0.01960
C00J 1 0.226011 0.620169 0.349565 11.00000 0.06615 0.05562 =
0.05011 0.02108 0.02860 0.04326
C00K 1 0.342116 0.660787 0.505514 11.00000 0.04694 0.05296 =
0.04778 0.01445 0.01988 0.03613
C00L 1 0.204221 0.965656 0.288386 11.00000 0.05078 0.04746 =
0.07153 0.01898 0.02371 0.01948
C00M 1 0.417387 0.756354 0.576906 11.00000 0.04776 0.06631 =
0.05603 0.00548 0.01416 0.03839
AFIX 43
H00M 2 0.483120 0.824556 0.572352 11.00000 -1.20000
AFIX 0
C00N 1 0.748542 0.857090 1.151081 11.00000 0.05380 0.04936 =
0.04998 0.00695 0.01351 0.03303
C00O 1 0.629504 0.947954 1.106728 11.00000 0.05456 0.05158 =
0.04197 0.01433 0.01452 0.03130
C00P 1 0.675573 0.838690 0.920340 11.00000 0.06610 0.05155 =
0.05577 0.01879 0.02385 0.03959
AFIX 43
H00P 2 0.745195 0.906495 0.919511 11.00000 -1.20000
AFIX 0
C00Q 1 0.262125 0.440349 0.401253 11.00000 0.04824 0.03859 =
0.04283 0.00403 0.01229 0.02423
C00R 1 0.202348 0.683822 0.293390 11.00000 0.08117 0.05619 =
0.05416 0.02075 0.02655 0.04029
AFIX 43
H00R 2 0.267072 0.753134 0.289093 11.00000 -1.20000
AFIX 0
C00S 1 0.340065 1.112493 0.608422 11.00000 0.08656 0.05022 =
0.06443 0.00506 0.02184 0.01408
AFIX 43
H00S 2 0.347394 1.157369 0.659545 11.00000 -1.20000
AFIX 0
C00T 1 0.457196 0.541332 0.379252 11.00000 0.06228 0.05814 =
0.04726 0.01114 0.02283 0.03402
AFIX 43
H00T 2 0.523292 0.609974 0.375527 11.00000 -1.20000
AFIX 0
C00U 1 0.430889 0.854636 1.123243 11.00000 0.07748 0.07784 =
0.04997 0.01373 0.02686 0.05055
AFIX 43
H00U 2 0.361329 0.787327 1.124692 11.00000 -1.20000
AFIX 0
C00V 1 0.258401 0.335271 0.388431 11.00000 0.07463 0.04831 =
0.05538 0.01031 0.01953 0.03637
AFIX 43
H00V 2 0.190856 0.265819 0.389722 11.00000 -1.20000
AFIX 0
C00W 1 0.464482 0.634764 0.921722 11.00000 0.05874 0.04830 =
0.06439 0.01511 0.02137 0.03116
AFIX 43
H00W 2 0.394627 0.567123 0.922456 11.00000 -1.20000
AFIX 0
C00X 1 0.154381 0.923167 0.196470 11.00000 0.05693 0.05072 =
0.06616 0.01707 0.02558 0.01529
C00Y 1 0.298420 0.650057 0.663541 11.00000 0.07604 0.09472 =
0.05815 0.03457 0.02774 0.06138
AFIX 43
H00Y 2 0.284542 0.646805 0.717081 11.00000 -1.20000
AFIX 0
C00Z 1 -0.179636 0.589334 0.034608 11.00000 0.05771 0.05876 =
0.06829 0.02679 0.02173 0.02770
AFIX 43
H00Z 2 -0.157811 0.619731 0.094963 11.00000 -1.20000
AFIX 0
C010 1 0.059859 0.836484 0.024878 11.00000 0.06193 0.05954 =
0.05410 0.02116 0.02374 0.02760
C011 1 0.396210 0.752195 0.656497 11.00000 0.06647 0.08179 =
0.05451 0.00113 0.01007 0.05344
AFIX 43
H011 2 0.447466 0.817799 0.705261 11.00000 -1.20000
AFIX 0
C012 1 0.009764 0.477775 0.306745 11.00000 0.06150 0.06609 =
0.06019 0.01031 0.02045 0.04474
AFIX 43
H012 2 -0.055490 0.408818 0.310938 11.00000 -1.20000
AFIX 0
C013 1 0.049984 0.780687 0.471512 11.00000 0.05331 0.05495 =
0.06658 0.01364 0.01323 0.02128
AFIX 43
H013 2 0.027143 0.746673 0.411694 11.00000 -1.20000
AFIX 0
C014 1 0.390246 1.042071 0.606255 11.00000 0.06838 0.08605 =
0.07581 0.03524 0.01279 0.02418
AFIX 43
H014 2 0.435139 1.031334 0.655404 11.00000 -1.20000
AFIX 0
C015 1 0.356446 0.333070 0.373438 11.00000 0.08642 0.06595 =
0.06476 0.02078 0.02852 0.05642
AFIX 43
H015 2 0.355553 0.262979 0.366479 11.00000 -1.20000
AFIX 0
C016 1 0.081560 0.644192 0.243190 11.00000 0.09028 0.06680 =
0.06753 0.02167 0.01913 0.05253
AFIX 43
H016 2 0.064859 0.686851 0.205354 11.00000 -1.20000
AFIX 0
C017 1 0.276568 1.104284 0.520418 11.00000 0.07846 0.04271 =
0.09073 0.03016 0.03372 0.02943
AFIX 43
H017 2 0.234004 1.141287 0.503084 11.00000 -1.20000
AFIX 0
C018 1 0.495155 0.644819 0.845484 11.00000 0.07753 0.06257 =
0.05158 0.00361 0.00901 0.04548
AFIX 43
H018 2 0.444979 0.582889 0.794176 11.00000 -1.20000
AFIX 0
C019 1 0.598485 0.744937 0.845035 11.00000 0.09636 0.07039 =
0.04450 0.01932 0.02585 0.06103
AFIX 43
H019 2 0.617073 0.749925 0.793288 11.00000 -1.20000
AFIX 0
C01A 1 0.017867 0.854644 0.506166 11.00000 0.05694 0.07389 =
0.11713 0.03296 0.03459 0.04189
AFIX 43
H01A 2 -0.031254 0.878457 0.473403 11.00000 -1.20000
AFIX 0
C01B 1 0.652879 0.684811 1.205859 11.00000 0.08452 0.06637 =
0.08203 0.03486 0.04660 0.05542
AFIX 43
H01B 2 0.582747 0.617630 1.206764 11.00000 -1.20000
AFIX 0
C01C 1 -0.259621 0.599463 -0.034201 11.00000 0.05771 0.08413 =
0.09116 0.02043 0.03628 0.03969
AFIX 43
H01C 2 -0.300373 0.637865 -0.028013 11.00000 -1.20000
AFIX 0
C01D 1 0.544673 1.063848 1.132311 11.00000 0.09129 0.07754 =
0.05982 0.00699 0.02263 0.06594
AFIX 43
H01D 2 0.550553 1.136384 1.139282 11.00000 -1.20000
AFIX 0
C01E 1 0.441764 0.964705 1.136070 11.00000 0.05660 0.08480 =
0.07049 0.00797 0.02166 0.04668
AFIX 43
H01E 2 0.379850 0.971148 1.147108 11.00000 -1.20000
AFIX 0
C01F 1 0.769866 0.714921 1.259522 11.00000 0.09800 0.09269 =
0.07342 0.03216 0.03339 0.06581
AFIX 43
H01F 2 0.777375 0.668039 1.296870 11.00000 -1.20000
AFIX 0
C01G 1 -0.026576 0.848507 -0.036787 11.00000 0.07115 0.04600 =
0.07350 0.01974 0.01327 0.02419
AFIX 43
H01G 2 -0.062419 0.888789 -0.022303 11.00000 -1.20000
AFIX 0
C01H 1 -0.137459 0.525221 -0.002801 11.00000 0.06622 0.05916 =
0.11885 0.02743 0.04455 0.03768
AFIX 43
H01H 2 -0.082909 0.505808 0.028093 11.00000 -1.20000
AFIX 0
C01I 1 0.090567 0.769667 -0.026383 11.00000 0.05742 0.08269 =
0.09085 0.01142 0.03919 0.02719
AFIX 43
H01I 2 0.146124 0.747487 -0.003769 11.00000 -1.20000
AFIX 0
C01J 1 0.360932 0.990763 0.517152 11.00000 0.05815 0.06848 =
0.07278 0.02670 0.03052 0.03069
AFIX 43
H01J 2 0.383956 0.940769 0.497058 11.00000 -1.20000
AFIX 0
C01K 1 0.454649 0.436812 0.369145 11.00000 0.07187 0.08273 =
0.05419 0.00587 0.01932 0.05904
AFIX 43
H01K 2 0.519889 0.435864 0.359281 11.00000 -1.20000
AFIX 0
C01L 1 0.121227 0.767234 0.541509 11.00000 0.06820 0.04060 =
0.09923 0.03121 0.02099 0.01866
AFIX 43
H01L 2 0.154481 0.721122 0.536515 11.00000 -1.20000
AFIX 0
C01M 1 0.865342 0.886273 1.203510 11.00000 0.06310 0.06966 =
0.06977 0.00783 0.01650 0.04578
AFIX 43
H01M 2 0.935866 0.952871 1.202461 11.00000 -1.20000
AFIX 0
C01N 1 -0.012624 0.541635 0.250034 11.00000 0.07328 0.07364 =
0.08092 0.02940 0.01973 0.05560
AFIX 43
H01N 2 -0.093379 0.514447 0.215740 11.00000 -1.20000
AFIX 0
C01O 1 0.873475 0.812974 1.257468 11.00000 0.08447 0.10119 =
0.05960 0.01407 0.01399 0.06942
AFIX 43
H01O 2 0.950563 0.830886 1.292716 11.00000 -1.20000
AFIX 0
C01P 1 0.137293 0.830955 0.620419 11.00000 0.08238 0.07482 =
0.06175 0.03186 0.00942 0.00222
AFIX 43
H01P 2 0.182446 0.836011 0.677099 11.00000 -1.20000
AFIX 0
C01Q 1 0.022538 0.743661 -0.116207 11.00000 0.07393 0.08421 =
0.06915 -0.00958 0.03726 -0.00807
AFIX 43
H01Q 2 0.025756 0.701698 -0.163442 11.00000 -1.20000
AFIX 0
C01R 1 -0.267547 0.542076 -0.113471 11.00000 0.05681 0.06858 =
0.08956 0.01450 0.00935 0.00342
AFIX 43
H01R 2 -0.314844 0.534993 -0.170032 11.00000 -1.20000
AFIX 0
C01S 1 -0.051713 0.791676 -0.123182 11.00000 0.08322 0.07300 =
0.08418 0.03625 0.01719 0.00938
AFIX 43
H01S 2 -0.106722 0.786533 -0.175163 11.00000 -1.20000
AFIX 0
C01T 1 0.071876 0.887248 0.598652 11.00000 0.11081 0.05182 =
0.10392 0.00213 0.07503 0.02147
AFIX 43
H01T 2 0.065819 0.936809 0.638426 11.00000 -1.20000
AFIX 0
C01U 1 -0.192084 0.496590 -0.093746 11.00000 0.10213 0.03750 =
0.11168 -0.00619 0.04450 0.01580
AFIX 43
H01U 2 -0.180671 0.454101 -0.135113 11.00000 -1.20000
AFIX 0
HKLF 4
REM smm881_a.res in P-1
REM wR2 = 0.2736, GooF = S = 1.021, Restrained GooF = 1.021 for all data
REM R1 = 0.0914 for 3258 Fo > 4sig(Fo) and 0.2107 for all 8192 data
REM 595 parameters refined using 0 restraints
END
WGHT 0.0903 0.0000
REM Highest difference peak 0.735, deepest hole -0.380, 1-sigma level 0.087
Q1 1 0.3820 1.1178 0.5446 11.00000 0.05 0.73
Q2 1 -0.2548 0.5155 -0.0496 11.00000 0.05 0.70
Q3 1 0.0386 0.7794 0.5452 11.00000 0.05 0.70
Q4 1 0.0853 0.8472 -0.0494 11.00000 0.05 0.66
Q5 1 0.0179 0.2813 0.4538 11.00000 0.05 0.66
Q6 1 0.4134 0.6487 1.0488 11.00000 0.05 0.65
Q7 1 0.3188 0.5523 1.0455 11.00000 0.05 0.65
Q8 1 0.3032 1.0379 0.5493 11.00000 0.05 0.46
Q9 1 -0.0039 0.7684 -0.0451 11.00000 0.05 0.44
Q10 1 0.5012 0.7738 0.4499 11.00000 0.05 0.40
Q11 1 0.7548 1.0011 1.0447 11.00000 0.05 0.39
Q12 1 0.3622 0.6697 1.0940 11.00000 0.05 0.36
Q13 1 0.4248 1.2405 0.5999 11.00000 0.05 0.36
Q14 1 0.8204 1.0003 0.9891 11.00000 0.05 0.35
Q15 1 0.5000 0.8107 0.5070 11.00000 0.05 0.35
Q16 1 0.9023 1.0137 1.1516 11.00000 0.05 0.34
Q17 1 1.0245 0.9680 1.2606 11.00000 0.05 0.33
Q18 1 0.8347 1.1503 1.1083 11.00000 0.05 0.33
Q19 1 -0.0406 0.3518 0.3633 11.00000 0.05 0.32
Q20 1 0.3988 0.5563 1.1219 11.00000 0.05 0.32
;
_shelx_res_checksum 13916
_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_5
_database_code_depnum_ccdc_archive 'CCDC 1586857'
loop_
_audit_author_name
_audit_author_address
'Ajeet Singh'
;Indian Institute of Technology Indore
India
;
_audit_update_record
;
2019-10-26 deposited with the CCDC. 2020-01-20 downloaded from the CCDC.
;
_audit_creation_date 2019-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic 'Cocrystal 4'
_chemical_formula_moiety 'C20 H18 Fe2, 2(C20 H14)'
_chemical_formula_sum 'C60 H46 Fe2'
_chemical_formula_weight 878.67
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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 8.93360(10)
_cell_length_b 8.41050(10)
_cell_length_c 28.5683(4)
_cell_angle_alpha 90
_cell_angle_beta 93.5820(10)
_cell_angle_gamma 90
_cell_volume 2142.31(5)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 6494
_cell_measurement_temperature 293
_cell_measurement_theta_max 71.0230
_cell_measurement_theta_min 5.1130
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 5.734
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.36798
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour orange
_exptl_crystal_colour_lustre ?
_exptl_crystal_colour_modifier ?
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.362
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 916
_exptl_crystal_preparation 'CHCl3 Hexane'
_exptl_crystal_recrystallization_method 'CHCl3 Hexane'
_exptl_crystal_size_max 0.38
_exptl_crystal_size_mid 0.33
_exptl_crystal_size_min 0.28
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0347
_diffrn_reflns_av_unetI/netI 0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_limit_l_min -35
_diffrn_reflns_number 13762
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full 66.9682
_diffrn_reflns_theta_max 71.287
_diffrn_reflns_theta_min 3.100
_diffrn_ambient_temperature 293
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.0309
_diffrn_detector_type Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega 4.00 30.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 57.0000 90.0000 26
#__ type_ start__ end____ width___ exp.time_
2 omega 41.00 69.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 57.0000 90.0000 28
#__ type_ start__ end____ width___ exp.time_
3 omega 53.00 101.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 57.0000 120.0000 48
#__ type_ start__ end____ width___ exp.time_
4 omega 87.00 178.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 37.0000 120.0000 91
#__ type_ start__ end____ width___ exp.time_
5 omega 120.00 165.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 63.0000 30.0000 45
#__ type_ start__ end____ width___ exp.time_
6 omega 95.00 163.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 63.0000 -30.0000 68
#__ type_ start__ end____ width___ exp.time_
7 omega 93.00 168.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 63.0000 60.0000 75
#__ type_ start__ end____ width___ exp.time_
8 omega 97.00 129.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 178.0000 -30.0000 32
#__ type_ start__ end____ width___ exp.time_
9 omega 25.00 124.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 77.0000 150.0000 99
#__ type_ start__ end____ width___ exp.time_
10 omega 50.00 91.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -37.0000 60.0000 41
#__ type_ start__ end____ width___ exp.time_
11 omega 45.00 73.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -91.0000 -30.0000 28
#__ type_ start__ end____ width___ exp.time_
12 omega 47.00 142.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -91.0000 0.0000 95
#__ type_ start__ end____ width___ exp.time_
13 omega 59.00 102.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -113.0000 -164.0000 43
#__ type_ start__ end____ width___ exp.time_
14 omega 46.00 82.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -37.0000 -120.0000 36
#__ type_ start__ end____ width___ exp.time_
15 omega 35.00 93.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -25.0000 -60.0000 58
#__ type_ start__ end____ width___ exp.time_
16 omega 41.00 100.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -50.0000 0.0000 59
#__ type_ start__ end____ width___ exp.time_
17 omega 47.00 73.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 -125.0000 90.0000 26
#__ type_ start__ end____ width___ exp.time_
18 omega 40.00 102.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -50.0000 120.0000 62
#__ type_ start__ end____ width___ exp.time_
19 omega 35.00 88.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -25.0000 150.0000 53
#__ type_ start__ end____ width___ exp.time_
20 omega -14.00 76.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 -37.0000 0.0000 90
#__ type_ start__ end____ width___ exp.time_
21 omega 40.00 113.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -111.0000 -60.0000 73
#__ type_ start__ end____ width___ exp.time_
22 omega 39.00 109.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 -125.0000 -90.0000 70
#__ type_ start__ end____ width___ exp.time_
23 omega 12.00 83.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 19.0000 -60.0000 71
#__ type_ start__ end____ width___ exp.time_
24 omega -7.00 29.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -77.0000 -30.0000 36
#__ type_ start__ end____ width___ exp.time_
25 omega -13.00 73.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 -57.0000 -90.0000 86
#__ type_ start__ end____ width___ exp.time_
26 omega -68.00 -13.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -77.0000 -30.0000 55
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 0.1482245000
_diffrn_orient_matrix_UB_12 0.0500658000
_diffrn_orient_matrix_UB_13 0.0263689000
_diffrn_orient_matrix_UB_21 -0.0809047000
_diffrn_orient_matrix_UB_22 0.0122735000
_diffrn_orient_matrix_UB_23 0.0459333000
_diffrn_orient_matrix_UB_31 0.0365379000
_diffrn_orient_matrix_UB_32 -0.1758003000
_diffrn_orient_matrix_UB_33 0.0107318000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3679
_reflns_number_total 4112
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.346
_refine_diff_density_min -0.537
_refine_diff_density_rms 0.093
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 280
_refine_ls_number_reflns 4112
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0497
_refine_ls_R_factor_gt 0.0438
_refine_ls_restrained_S_all 1.042
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0990P)^2^+0.1780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1287
_refine_ls_wR_factor_ref 0.1397
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Ternary CH refined with riding coordinates:
C11(H11), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
C26(H26), C29(H29), C17(H17), C20(H20), C23(H23), C14(H14), C10(H10), C5(H5),
C22(H22), C21(H21), C2(H2), C27(H27), C28(H28), C9(H9), C16(H16), C8(H8),
C6(H6), C15(H15), C4(H4), C7(H7), C3(H3)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.81007(4) 1.21961(4) 0.51370(2) 0.05127(16) Uani 1 1 d . . . . .
C25 C 0.6635(2) 0.5681(3) 0.65321(7) 0.0444(4) Uani 1 1 d . . . . .
C24 C 0.4748(2) 0.3611(3) 0.64860(7) 0.0443(5) Uani 1 1 d . . . . .
C30 C 0.7511(2) 0.4774(3) 0.68520(7) 0.0462(5) Uani 1 1 d . . . . .
C13 C 0.5484(3) 0.4778(3) 0.73865(8) 0.0509(5) Uani 1 1 d . . . . .
C18 C 0.4606(2) 0.5695(3) 0.70686(8) 0.0475(5) Uani 1 1 d . . . . .
C19 C 0.5618(3) 0.2690(3) 0.68052(8) 0.0469(5) Uani 1 1 d . . . . .
C26 C 0.7294(3) 0.6693(3) 0.62261(8) 0.0519(5) Uani 1 1 d . . . . .
H26 H 0.670380 0.730403 0.601532 0.062 Uiso 1 1 calc R . . . .
C1 C 0.9647(2) 1.0389(3) 0.51929(7) 0.0475(5) Uani 1 1 d . . . . .
C11 C 0.4960(2) 0.5399(3) 0.65595(7) 0.0445(5) Uani 1 1 d . . . . .
H11 H 0.434552 0.604063 0.633494 0.053 Uiso 1 1 calc R . . . .
C29 C 0.9060(3) 0.4886(3) 0.68639(8) 0.0565(6) Uani 1 1 d . . . . .
H29 H 0.965372 0.429067 0.707789 0.068 Uiso 1 1 calc R . . . .
C12 C 0.6581(3) 0.3697(3) 0.71523(8) 0.0503(5) Uani 1 1 d . . . . .
H12 H 0.719671 0.305684 0.737697 0.060 Uiso 1 1 calc R . . . .
C17 C 0.3523(3) 0.6704(3) 0.72249(10) 0.0599(6) Uani 1 1 d . . . . .
H17 H 0.294536 0.732694 0.701420 0.072 Uiso 1 1 calc R . . . .
C20 C 0.5537(3) 0.1054(3) 0.67897(8) 0.0558(6) Uani 1 1 d . . . . .
H20 H 0.611266 0.043817 0.700295 0.067 Uiso 1 1 calc R . . . .
C23 C 0.3800(3) 0.2900(3) 0.61496(9) 0.0518(5) Uani 1 1 d . . . . .
H23 H 0.322112 0.351495 0.593678 0.062 Uiso 1 1 calc R . . . .
C14 C 0.5281(3) 0.4873(4) 0.78632(9) 0.0652(7) Uani 1 1 d . . . . .
H14 H 0.587250 0.427326 0.807656 0.078 Uiso 1 1 calc R . . . .
C10 C 0.7570(3) 1.2637(3) 0.44463(9) 0.0602(6) Uani 1 1 d . . . . .
H10 H 0.792243 1.207342 0.419563 0.072 Uiso 1 1 calc R . . . .
C5 C 0.8291(3) 0.9945(4) 0.53897(10) 0.0703(8) Uani 1 1 d . . . . .
H5 H 0.768162 0.909259 0.529536 0.084 Uiso 1 1 calc R . . . .
C22 C 0.3720(3) 0.1249(3) 0.61327(9) 0.0602(6) Uani 1 1 d . . . . .
H22 H 0.308458 0.075601 0.590687 0.072 Uiso 1 1 calc R . . . .
C21 C 0.4576(3) 0.0340(3) 0.64482(9) 0.0604(6) Uani 1 1 d . . . . .
H21 H 0.451300 -0.076230 0.643335 0.073 Uiso 1 1 calc R . . . .
C2 C 1.0177(3) 1.1771(3) 0.54379(10) 0.0665(7) Uani 1 1 d . . . . .
H2 H 1.103965 1.233756 0.537942 0.080 Uiso 1 1 calc R . . . .
C27 C 0.8845(3) 0.6794(3) 0.62351(10) 0.0602(6) Uani 1 1 d . . . . .
H27 H 0.929894 0.746469 0.602746 0.072 Uiso 1 1 calc R . . . .
C28 C 0.9713(3) 0.5900(3) 0.65514(10) 0.0626(6) Uani 1 1 d . . . . .
H28 H 1.075254 0.597598 0.655587 0.075 Uiso 1 1 calc R . . . .
C9 C 0.8257(4) 1.3982(3) 0.46564(10) 0.0679(7) Uani 1 1 d . . . . .
H9 H 0.913189 1.446714 0.456835 0.081 Uiso 1 1 calc R . . . .
C16 C 0.3312(3) 0.6773(4) 0.77051(12) 0.0760(9) Uani 1 1 d . . . . .
H16 H 0.257369 0.743229 0.781390 0.091 Uiso 1 1 calc R . . . .
C8 C 0.7386(4) 1.4461(4) 0.50238(11) 0.0848(10) Uani 1 1 d . . . . .
H8 H 0.758474 1.531971 0.522310 0.102 Uiso 1 1 calc R . . . .
C6 C 0.6256(3) 1.2278(4) 0.46767(12) 0.0746(8) Uani 1 1 d . . . . .
H6 H 0.558610 1.145418 0.460519 0.089 Uiso 1 1 calc R . . . .
C15 C 0.4179(4) 0.5879(4) 0.80167(11) 0.0782(9) Uani 1 1 d . . . . .
H15 H 0.403001 0.594589 0.833531 0.094 Uiso 1 1 calc R . . . .
C4 C 0.8027(5) 1.1024(5) 0.57540(11) 0.1001(14) Uani 1 1 d . . . . .
H4 H 0.721592 1.099223 0.594278 0.120 Uiso 1 1 calc R . . . .
C7 C 0.6163(4) 1.3419(5) 0.50378(13) 0.0962(13) Uani 1 1 d . . . . .
H7 H 0.541409 1.346982 0.524933 0.115 Uiso 1 1 calc R . . . .
C3 C 0.9173(6) 1.2138(5) 0.57844(11) 0.0951(14) Uani 1 1 d . . . . .
H3 H 0.926429 1.297856 0.599589 0.114 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0600(3) 0.0484(3) 0.0456(2) 0.00292(14) 0.00520(16) 0.02156(15)
C25 0.0472(10) 0.0395(11) 0.0462(10) -0.0021(8) 0.0010(8) 0.0006(8)
C24 0.0456(10) 0.0393(11) 0.0482(11) 0.0039(8) 0.0036(8) -0.0009(8)
C30 0.0486(11) 0.0423(11) 0.0470(10) -0.0026(9) -0.0017(9) 0.0018(9)
C13 0.0559(12) 0.0487(12) 0.0483(11) 0.0000(9) 0.0046(9) -0.0080(10)
C18 0.0463(10) 0.0412(11) 0.0551(11) -0.0022(9) 0.0044(9) -0.0055(9)
C19 0.0521(12) 0.0419(12) 0.0468(11) 0.0053(9) 0.0045(9) 0.0025(9)
C26 0.0608(13) 0.0428(11) 0.0525(12) 0.0018(10) 0.0055(10) -0.0018(10)
C1 0.0557(12) 0.0401(11) 0.0463(10) 0.0061(9) -0.0010(9) 0.0156(9)
C11 0.0442(10) 0.0404(11) 0.0481(11) 0.0060(8) -0.0021(8) 0.0030(8)
C29 0.0509(12) 0.0552(14) 0.0622(13) -0.0117(11) -0.0071(10) 0.0080(10)
C12 0.0556(12) 0.0470(12) 0.0473(11) 0.0087(9) -0.0043(9) 0.0060(10)
C17 0.0475(12) 0.0502(13) 0.0824(17) -0.0116(12) 0.0076(11) -0.0048(10)
C20 0.0626(13) 0.0452(13) 0.0606(13) 0.0111(10) 0.0110(11) 0.0053(10)
C23 0.0500(12) 0.0518(14) 0.0530(13) 0.0008(9) -0.0006(10) -0.0024(9)
C14 0.0745(16) 0.0707(17) 0.0507(12) 0.0022(12) 0.0052(11) -0.0205(14)
C10 0.0681(15) 0.0630(15) 0.0480(13) 0.0074(11) -0.0077(11) 0.0143(12)
C5 0.0811(17) 0.0576(15) 0.0749(16) 0.0260(13) 0.0256(14) 0.0187(13)
C22 0.0617(14) 0.0530(14) 0.0658(14) -0.0098(11) 0.0029(11) -0.0086(11)
C21 0.0689(15) 0.0386(12) 0.0752(16) -0.0042(11) 0.0157(12) -0.0046(11)
C2 0.0754(17) 0.0569(15) 0.0637(15) -0.0104(12) -0.0224(13) 0.0192(13)
C27 0.0607(14) 0.0561(14) 0.0651(14) -0.0050(12) 0.0150(12) -0.0110(12)
C28 0.0477(12) 0.0645(16) 0.0763(16) -0.0162(13) 0.0094(11) -0.0090(11)
C9 0.0895(19) 0.0474(14) 0.0656(15) 0.0136(12) -0.0039(14) 0.0110(13)
C16 0.0592(15) 0.081(2) 0.090(2) -0.0348(17) 0.0278(15) -0.0169(15)
C8 0.120(3) 0.0542(17) 0.0798(18) -0.0008(14) 0.0007(19) 0.0445(19)
C6 0.0563(15) 0.088(2) 0.078(2) 0.0083(16) -0.0070(14) 0.0161(14)
C15 0.0778(18) 0.095(2) 0.0641(16) -0.0232(16) 0.0271(14) -0.0295(17)
C4 0.136(3) 0.107(3) 0.0618(17) 0.0356(19) 0.043(2) 0.065(3)
C7 0.083(2) 0.115(3) 0.093(2) 0.029(2) 0.0244(19) 0.061(2)
C3 0.143(4) 0.094(3) 0.0455(15) -0.0126(15) -0.0165(19) 0.059(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
Fe1 C1 2.053(2) . ?
Fe1 C10 2.035(3) . ?
Fe1 C5 2.029(3) . ?
Fe1 C2 2.027(3) . ?
Fe1 C9 2.045(3) . ?
Fe1 C8 2.029(3) . ?
Fe1 C6 2.044(3) . ?
Fe1 C4 2.024(3) . ?
Fe1 C7 2.019(3) . ?
Fe1 C3 2.030(3) . ?
C25 C30 1.393(3) . ?
C25 C26 1.378(3) . ?
C25 C11 1.522(3) . ?
C24 C19 1.396(3) . ?
C24 C11 1.528(3) . ?
C24 C23 1.377(3) . ?
C30 C29 1.385(3) . ?
C30 C12 1.528(3) . ?
C13 C18 1.395(3) . ?
C13 C12 1.522(3) . ?
C13 C14 1.387(3) . ?
C18 C11 1.528(3) . ?
C18 C17 1.382(3) . ?
C19 C12 1.528(3) . ?
C19 C20 1.378(3) . ?
C26 H26 0.9300 . ?
C26 C27 1.387(4) . ?
C1 C1 1.458(4) 3_776 ?
C1 C5 1.417(4) . ?
C1 C2 1.423(4) . ?
C11 H11 0.9800 . ?
C29 H29 0.9300 . ?
C29 C28 1.389(4) . ?
C12 H12 0.9800 . ?
C17 H17 0.9300 . ?
C17 C16 1.398(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.395(4) . ?
C23 H23 0.9300 . ?
C23 C22 1.391(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.389(4) . ?
C10 H10 0.9300 . ?
C10 C9 1.403(4) . ?
C10 C6 1.414(5) . ?
C5 H5 0.9300 . ?
C5 C4 1.411(5) . ?
C22 H22 0.9300 . ?
C22 C21 1.377(4) . ?
C21 H21 0.9300 . ?
C2 H2 0.9300 . ?
C2 C3 1.411(5) . ?
C27 H27 0.9300 . ?
C27 C28 1.377(4) . ?
C28 H28 0.9300 . ?
C9 H9 0.9300 . ?
C9 C8 1.404(4) . ?
C16 H16 0.9300 . ?
C16 C15 1.368(5) . ?
C8 H8 0.9300 . ?
C8 C7 1.403(6) . ?
C6 H6 0.9300 . ?
C6 C7 1.415(5) . ?
C15 H15 0.9300 . ?
C4 H4 0.9300 . ?
C4 C3 1.387(6) . ?
C7 H7 0.9300 . ?
C3 H3 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C10 Fe1 C1 108.98(10) . . ?
C10 Fe1 C9 40.24(11) . . ?
C10 Fe1 C6 40.56(13) . . ?
C5 Fe1 C1 40.62(10) . . ?
C5 Fe1 C10 121.63(13) . . ?
C5 Fe1 C9 156.33(12) . . ?
C5 Fe1 C6 107.85(14) . . ?
C5 Fe1 C3 68.24(16) . . ?
C2 Fe1 C1 40.80(10) . . ?
C2 Fe1 C10 126.51(13) . . ?
C2 Fe1 C5 68.32(13) . . ?
C2 Fe1 C9 108.35(14) . . ?
C2 Fe1 C8 120.25(15) . . ?
C2 Fe1 C6 163.40(13) . . ?
C2 Fe1 C3 40.70(15) . . ?
C9 Fe1 C1 121.44(11) . . ?
C8 Fe1 C1 155.64(14) . . ?
C8 Fe1 C10 67.79(12) . . ?
C8 Fe1 C5 162.03(14) . . ?
C8 Fe1 C9 40.32(12) . . ?
C8 Fe1 C6 68.45(15) . . ?
C8 Fe1 C3 107.09(15) . . ?
C6 Fe1 C1 125.89(12) . . ?
C6 Fe1 C9 68.27(14) . . ?
C4 Fe1 C1 68.30(11) . . ?
C4 Fe1 C10 156.21(18) . . ?
C4 Fe1 C5 40.75(14) . . ?
C4 Fe1 C2 67.90(16) . . ?
C4 Fe1 C9 161.70(16) . . ?
C4 Fe1 C8 124.70(14) . . ?
C4 Fe1 C6 120.51(19) . . ?
C4 Fe1 C3 40.02(17) . . ?
C7 Fe1 C1 162.76(17) . . ?
C7 Fe1 C10 67.98(13) . . ?
C7 Fe1 C5 125.26(16) . . ?
C7 Fe1 C2 154.64(16) . . ?
C7 Fe1 C9 68.02(15) . . ?
C7 Fe1 C8 40.58(16) . . ?
C7 Fe1 C6 40.76(16) . . ?
C7 Fe1 C4 107.23(15) . . ?
C7 Fe1 C3 119.49(16) . . ?
C3 Fe1 C1 68.56(11) . . ?
C3 Fe1 C10 162.99(19) . . ?
C3 Fe1 C9 125.52(18) . . ?
C3 Fe1 C6 154.52(19) . . ?
C30 C25 C11 113.24(19) . . ?
C26 C25 C30 120.7(2) . . ?
C26 C25 C11 126.1(2) . . ?
C19 C24 C11 113.40(19) . . ?
C23 C24 C19 120.5(2) . . ?
C23 C24 C11 126.1(2) . . ?
C25 C30 C12 112.96(19) . . ?
C29 C30 C25 119.9(2) . . ?
C29 C30 C12 127.1(2) . . ?
C18 C13 C12 113.28(19) . . ?
C14 C13 C18 120.3(2) . . ?
C14 C13 C12 126.4(2) . . ?
C13 C18 C11 112.85(19) . . ?
C17 C18 C13 120.4(2) . . ?
C17 C18 C11 126.8(2) . . ?
C24 C19 C12 112.60(19) . . ?
C20 C19 C24 120.5(2) . . ?
C20 C19 C12 126.9(2) . . ?
C25 C26 H26 120.3 . . ?
C25 C26 C27 119.4(2) . . ?
C27 C26 H26 120.3 . . ?
C1 C1 Fe1 126.43(19) 3_776 . ?
C5 C1 Fe1 68.78(14) . . ?
C5 C1 C1 127.0(3) . 3_776 ?
C5 C1 C2 106.6(2) . . ?
C2 C1 Fe1 68.59(13) . . ?
C2 C1 C1 126.3(3) . 3_776 ?
C25 C11 C24 105.10(17) . . ?
C25 C11 C18 106.61(17) . . ?
C25 C11 H11 113.1 . . ?
C24 C11 C18 105.07(17) . . ?
C24 C11 H11 113.1 . . ?
C18 C11 H11 113.1 . . ?
C30 C29 H29 120.5 . . ?
C30 C29 C28 119.0(2) . . ?
C28 C29 H29 120.5 . . ?
C30 C12 H12 113.0 . . ?
C13 C12 C30 106.30(18) . . ?
C13 C12 C19 105.34(18) . . ?
C13 C12 H12 113.0 . . ?
C19 C12 C30 105.54(17) . . ?
C19 C12 H12 113.0 . . ?
C18 C17 H17 120.6 . . ?
C18 C17 C16 118.9(3) . . ?
C16 C17 H17 120.6 . . ?
C19 C20 H20 120.6 . . ?
C19 C20 C21 118.8(2) . . ?
C21 C20 H20 120.6 . . ?
C24 C23 H23 120.5 . . ?
C24 C23 C22 119.0(2) . . ?
C22 C23 H23 120.5 . . ?
C13 C14 H14 120.5 . . ?
C13 C14 C15 118.9(3) . . ?
C15 C14 H14 120.5 . . ?
Fe1 C10 H10 125.7 . . ?
C9 C10 Fe1 70.30(15) . . ?
C9 C10 H10 125.5 . . ?
C9 C10 C6 109.1(3) . . ?
C6 C10 Fe1 70.08(17) . . ?
C6 C10 H10 125.5 . . ?
Fe1 C5 H5 125.6 . . ?
C1 C5 Fe1 70.60(14) . . ?
C1 C5 H5 126.0 . . ?
C4 C5 Fe1 69.43(17) . . ?
C4 C5 C1 108.1(3) . . ?
C4 C5 H5 126.0 . . ?
C23 C22 H22 119.8 . . ?
C21 C22 C23 120.4(2) . . ?
C21 C22 H22 119.8 . . ?
C20 C21 H21 119.6 . . ?
C22 C21 C20 120.8(2) . . ?
C22 C21 H21 119.6 . . ?
Fe1 C2 H2 125.5 . . ?
C1 C2 Fe1 70.61(14) . . ?
C1 C2 H2 125.7 . . ?
C3 C2 Fe1 69.76(19) . . ?
C3 C2 C1 108.5(3) . . ?
C3 C2 H2 125.7 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.0(2) . . ?
C28 C27 H27 120.0 . . ?
C29 C28 H28 119.5 . . ?
C27 C28 C29 121.0(2) . . ?
C27 C28 H28 119.5 . . ?
Fe1 C9 H9 126.7 . . ?
C10 C9 Fe1 69.47(15) . . ?
C10 C9 H9 126.2 . . ?
C10 C9 C8 107.6(3) . . ?
C8 C9 Fe1 69.19(16) . . ?
C8 C9 H9 126.2 . . ?
C17 C16 H16 119.7 . . ?
C15 C16 C17 120.7(3) . . ?
C15 C16 H16 119.7 . . ?
Fe1 C8 H8 125.8 . . ?
C9 C8 Fe1 70.48(15) . . ?
C9 C8 H8 125.9 . . ?
C7 C8 Fe1 69.33(18) . . ?
C7 C8 C9 108.1(3) . . ?
C7 C8 H8 125.9 . . ?
Fe1 C6 H6 126.8 . . ?
C10 C6 Fe1 69.36(16) . . ?
C10 C6 H6 126.8 . . ?
C10 C6 C7 106.4(3) . . ?
C7 C6 Fe1 68.65(19) . . ?
C7 C6 H6 126.8 . . ?
C14 C15 H15 119.6 . . ?
C16 C15 C14 120.9(3) . . ?
C16 C15 H15 119.6 . . ?
Fe1 C4 H4 126.0 . . ?
C5 C4 Fe1 69.82(15) . . ?
C5 C4 H4 125.6 . . ?
C3 C4 Fe1 70.20(19) . . ?
C3 C4 C5 108.9(3) . . ?
C3 C4 H4 125.6 . . ?
Fe1 C7 H7 125.3 . . ?
C8 C7 Fe1 70.10(17) . . ?
C8 C7 C6 108.7(3) . . ?
C8 C7 H7 125.6 . . ?
C6 C7 Fe1 70.59(17) . . ?
C6 C7 H7 125.6 . . ?
Fe1 C3 H3 126.2 . . ?
C2 C3 Fe1 69.53(16) . . ?
C2 C3 H3 126.1 . . ?
C4 C3 Fe1 69.8(2) . . ?
C4 C3 C2 107.9(3) . . ?
C4 C3 H3 126.1 . . ?
_shelx_res_file
;
TITL smm754_a.res in P2(1)/n
smm754.res
created by SHELXL-2018/3 at 00:39:19 on 26-Oct-2019
REM Old TITL SMM754 in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.170, Rweak 0.105, Alpha 0.039, Orientation as input
REM Formula found by SHELXT: C30 Fe
CELL 1.54184 8.9336 8.4105 28.5683 90 93.582 90
ZERR 2 0.0001 0.0001 0.0004 0 0.001 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Fe
UNIT 120 92 4
L.S. 40
PLAN 20
TEMP 19.85
BOND $H
LIST 6
fmap 2
acta 50
REM
REM
REM
WGHT 0.099000 0.178000
FVAR 0.43975
FE1 3 0.810067 1.219608 0.513704 11.00000 0.06004 0.04838 =
0.04564 0.00292 0.00520 0.02156
C25 1 0.663527 0.568120 0.653214 11.00000 0.04724 0.03954 =
0.04615 -0.00213 0.00101 0.00060
C24 1 0.474782 0.361143 0.648604 11.00000 0.04560 0.03931 =
0.04816 0.00387 0.00357 -0.00093
C30 1 0.751112 0.477365 0.685198 11.00000 0.04859 0.04235 =
0.04697 -0.00262 -0.00165 0.00182
C13 1 0.548395 0.477786 0.738650 11.00000 0.05589 0.04867 =
0.04832 0.00003 0.00462 -0.00803
C18 1 0.460616 0.569491 0.706857 11.00000 0.04627 0.04121 =
0.05506 -0.00219 0.00439 -0.00547
C19 1 0.561836 0.269004 0.680521 11.00000 0.05211 0.04190 =
0.04679 0.00529 0.00449 0.00250
C26 1 0.729433 0.669342 0.622608 11.00000 0.06082 0.04277 =
0.05246 0.00178 0.00554 -0.00179
AFIX 43
H26 2 0.670380 0.730403 0.601532 11.00000 -1.20000
AFIX 0
C1 1 0.964720 1.038900 0.519288 11.00000 0.05568 0.04010 =
0.04629 0.00613 -0.00099 0.01562
C11 1 0.495989 0.539861 0.655951 11.00000 0.04424 0.04040 =
0.04810 0.00598 -0.00214 0.00303
AFIX 13
H11 2 0.434552 0.604063 0.633494 11.00000 -1.20000
AFIX 0
C29 1 0.905995 0.488552 0.686389 11.00000 0.05091 0.05517 =
0.06223 -0.01168 -0.00711 0.00805
AFIX 43
H29 2 0.965372 0.429067 0.707789 11.00000 -1.20000
AFIX 0
C12 1 0.658103 0.369708 0.715228 11.00000 0.05557 0.04696 =
0.04734 0.00866 -0.00432 0.00599
AFIX 13
H12 2 0.719671 0.305684 0.737697 11.00000 -1.20000
AFIX 0
C17 1 0.352349 0.670394 0.722494 11.00000 0.04754 0.05019 =
0.08242 -0.01158 0.00757 -0.00481
AFIX 43
H17 2 0.294536 0.732694 0.701420 11.00000 -1.20000
AFIX 0
C20 1 0.553727 0.105435 0.678967 11.00000 0.06261 0.04517 =
0.06056 0.01112 0.01098 0.00529
AFIX 43
H20 2 0.611266 0.043817 0.700295 11.00000 -1.20000
AFIX 0
C23 1 0.379975 0.290021 0.614960 11.00000 0.05004 0.05180 =
0.05295 0.00083 -0.00063 -0.00245
AFIX 43
H23 2 0.322112 0.351495 0.593678 11.00000 -1.20000
AFIX 0
C14 1 0.528097 0.487302 0.786322 11.00000 0.07446 0.07066 =
0.05065 0.00218 0.00521 -0.02051
AFIX 43
H14 2 0.587250 0.427326 0.807656 11.00000 -1.20000
AFIX 0
C10 1 0.757016 1.263734 0.444628 11.00000 0.06813 0.06302 =
0.04796 0.00738 -0.00769 0.01431
AFIX 43
H10 2 0.792243 1.207342 0.419563 11.00000 -1.20000
AFIX 0
C5 1 0.829090 0.994527 0.538972 11.00000 0.08110 0.05762 =
0.07492 0.02604 0.02557 0.01869
AFIX 43
H5 2 0.768162 0.909259 0.529536 11.00000 -1.20000
AFIX 0
C22 1 0.372019 0.124907 0.613271 11.00000 0.06171 0.05305 =
0.06584 -0.00975 0.00286 -0.00858
AFIX 43
H22 2 0.308458 0.075601 0.590687 11.00000 -1.20000
AFIX 0
C21 1 0.457625 0.034046 0.644816 11.00000 0.06885 0.03861 =
0.07519 -0.00418 0.01567 -0.00456
AFIX 43
H21 2 0.451300 -0.076230 0.643335 11.00000 -1.20000
AFIX 0
C2 1 1.017692 1.177120 0.543788 11.00000 0.07541 0.05691 =
0.06373 -0.01041 -0.02241 0.01923
AFIX 43
H2 2 1.103965 1.233756 0.537942 11.00000 -1.20000
AFIX 0
C27 1 0.884513 0.679357 0.623510 11.00000 0.06065 0.05611 =
0.06509 -0.00500 0.01503 -0.01100
AFIX 43
H27 2 0.929894 0.746469 0.602746 11.00000 -1.20000
AFIX 0
C28 1 0.971320 0.589976 0.655136 11.00000 0.04766 0.06448 =
0.07627 -0.01624 0.00944 -0.00896
AFIX 43
H28 2 1.075254 0.597598 0.655587 11.00000 -1.20000
AFIX 0
C9 1 0.825744 1.398160 0.465643 11.00000 0.08954 0.04739 =
0.06557 0.01364 -0.00395 0.01095
AFIX 43
H9 2 0.913189 1.446714 0.456835 11.00000 -1.20000
AFIX 0
C16 1 0.331179 0.677258 0.770508 11.00000 0.05917 0.08138 =
0.09030 -0.03480 0.02785 -0.01690
AFIX 43
H16 2 0.257369 0.743229 0.781390 11.00000 -1.20000
AFIX 0
C8 1 0.738586 1.446095 0.502376 11.00000 0.11958 0.05416 =
0.07983 -0.00079 0.00069 0.04448
AFIX 43
H8 2 0.758474 1.531971 0.522310 11.00000 -1.20000
AFIX 0
C6 1 0.625634 1.227785 0.467673 11.00000 0.05628 0.08777 =
0.07822 0.00829 -0.00699 0.01606
AFIX 43
H6 2 0.558610 1.145418 0.460519 11.00000 -1.20000
AFIX 0
C15 1 0.417947 0.587903 0.801666 11.00000 0.07784 0.09542 =
0.06408 -0.02317 0.02712 -0.02945
AFIX 43
H15 2 0.403001 0.594589 0.833531 11.00000 -1.20000
AFIX 0
C4 1 0.802657 1.102367 0.575398 11.00000 0.13569 0.10732 =
0.06180 0.03559 0.04309 0.06495
AFIX 43
H4 2 0.721592 1.099223 0.594278 11.00000 -1.20000
AFIX 0
C7 1 0.616265 1.341891 0.503775 11.00000 0.08299 0.11493 =
0.09316 0.02860 0.02445 0.06093
AFIX 43
H7 2 0.541409 1.346982 0.524933 11.00000 -1.20000
AFIX 0
C3 1 0.917328 1.213821 0.578444 11.00000 0.14274 0.09434 =
0.04546 -0.01260 -0.01651 0.05900
AFIX 43
H3 2 0.926429 1.297856 0.599589 11.00000 -1.20000
AFIX 0
HKLF 4
REM smm754_a.res in P2(1)/n
REM wR2 = 0.1397, GooF = S = 1.042, Restrained GooF = 1.042 for all data
REM R1 = 0.0438 for 3679 Fo > 4sig(Fo) and 0.0497 for all 4112 data
REM 280 parameters refined using 0 restraints
END
WGHT 0.0988 0.1779
REM Highest difference peak 0.346, deepest hole -0.537, 1-sigma level 0.093
Q1 1 0.4752 0.5528 0.6844 11.00000 0.05 0.35
Q2 1 0.6028 0.4329 0.7273 11.00000 0.05 0.33
Q3 1 0.7140 0.4126 0.6995 11.00000 0.05 0.33
Q4 1 0.4863 0.4486 0.6524 11.00000 0.05 0.30
Q5 1 0.5792 0.5570 0.6549 11.00000 0.05 0.29
Q6 1 0.9478 0.5604 0.6837 11.00000 0.05 0.28
Q7 1 0.9178 0.5414 0.6884 11.00000 0.05 0.27
Q8 1 0.4717 0.5032 0.7183 11.00000 0.05 0.25
Q9 1 0.5407 0.5282 0.7680 11.00000 0.05 0.25
Q10 1 0.3608 0.5911 0.7817 11.00000 0.05 0.25
Q11 1 0.2968 0.6977 0.7828 11.00000 0.05 0.25
Q12 1 0.4629 0.4979 0.7824 11.00000 0.05 0.24
Q13 1 0.5195 0.4600 0.7560 11.00000 0.05 0.23
Q14 1 0.5631 0.1644 0.6742 11.00000 0.05 0.23
Q15 1 0.2248 0.7833 0.7650 11.00000 0.05 0.23
Q16 1 0.3332 0.6632 0.7436 11.00000 0.05 0.22
Q17 1 0.4516 0.6319 0.7169 11.00000 0.05 0.22
Q18 1 0.1733 0.6730 0.7815 11.00000 0.05 0.21
Q19 1 0.9201 0.4133 0.7150 11.00000 0.05 0.21
Q20 1 0.3782 0.5759 0.7169 11.00000 0.05 0.20
;
_shelx_res_checksum 85266
_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_2
_database_code_depnum_ccdc_archive 'CCDC 1586855'
loop_
_audit_author_name
_audit_author_address
'Ajeet Singh'
;Indian Institute of Technology Indore
India
;
_audit_update_record
;
2019-10-26 deposited with the CCDC. 2020-01-20 downloaded from the CCDC.
;
_audit_creation_date 2019-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic TripFccho
_chemical_formula_moiety 'C11 H10 Fe O, C20 H14'
_chemical_formula_sum 'C31 H24 Fe O'
_chemical_formula_weight 468.35
_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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.6767(12)
_cell_length_b 10.3972(12)
_cell_length_c 12.9455(15)
_cell_angle_alpha 70.641(10)
_cell_angle_beta 71.847(11)
_cell_angle_gamma 89.794(10)
_cell_volume 1160.4(3)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 2481
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 25.7440
_cell_measurement_theta_min 3.5150
_shelx_estimated_absorpt_T_max 0.829
_shelx_estimated_absorpt_T_min 0.785
_exptl_absorpt_coefficient_mu 0.671
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.23600
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour orange
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.340
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 488
_exptl_crystal_size_max 0.38
_exptl_crystal_size_mid 0.36
_exptl_crystal_size_min 0.29
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1015
_diffrn_reflns_av_unetI/netI 0.1430
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 15015
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 32.303
_diffrn_reflns_theta_min 3.171
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.0309
_diffrn_detector_type Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -5.00 93.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 77.0000 -150.0000 98
#__ type_ start__ end____ width___ exp.time_
2 omega -45.00 58.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 -26.0000 50.0000 103
#__ type_ start__ end____ width___ exp.time_
3 omega -47.00 47.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 -37.0000 -30.0000 94
#__ type_ start__ end____ width___ exp.time_
4 omega 1.00 77.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 77.0000 -60.0000 76
#__ type_ start__ end____ width___ exp.time_
5 omega 2.00 34.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 77.0000 30.0000 32
#__ type_ start__ end____ width___ exp.time_
6 omega 70.00 95.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 77.0000 30.0000 25
#__ type_ start__ end____ width___ exp.time_
7 omega -13.00 37.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 -99.0000 -180.0000 50
#__ type_ start__ end____ width___ exp.time_
8 omega 14.00 67.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ frames
- 25.3597 -99.0000 90.0000 53
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 0.0345819000
_diffrn_orient_matrix_UB_12 0.0665759000
_diffrn_orient_matrix_UB_13 -0.0144064000
_diffrn_orient_matrix_UB_21 0.0584845000
_diffrn_orient_matrix_UB_22 -0.0293396000
_diffrn_orient_matrix_UB_23 0.0182131000
_diffrn_orient_matrix_UB_31 0.0375294000
_diffrn_orient_matrix_UB_32 0.0010955000
_diffrn_orient_matrix_UB_33 -0.0569438000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2885
_reflns_number_total 7481
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 30.44
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.467
_refine_diff_density_min -0.815
_refine_diff_density_rms 0.132
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.961
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 298
_refine_ls_number_reflns 7481
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.2121
_refine_ls_R_factor_gt 0.1203
_refine_ls_restrained_S_all 0.961
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.3157
_refine_ls_wR_factor_ref 0.3924
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Ternary CH refined with riding coordinates:
C11(H11), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
C29(H29), C20(H20), C26(H26), C23(H23), C14(H14), C5(H5), C21(H21), C2(H2),
C17(H17), C8(H8), C27(H27), C28(H28), C15(H15), C3(H3), C22(H22), C4(H4),
C16(H16), C6(H6), C7(H7), C9(H9), C10(H10), C31(H31)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 1.15719(8) 0.76059(9) 0.20196(6) 0.0557(3) Uani 1 1 d . . . . .
C29 C 0.5996(6) 0.4235(6) 0.1876(5) 0.0542(13) Uani 1 1 d . . . . .
H29 H 0.666472 0.423134 0.118301 0.065 Uiso 1 1 calc R . . . .
C11 C 0.2435(6) 0.2215(6) 0.3923(4) 0.0511(12) Uani 1 1 d . . . . .
H11 H 0.170900 0.222446 0.464270 0.061 Uiso 1 1 calc R . . . .
C18 C 0.2832(6) 0.2448(5) 0.1903(4) 0.0466(11) Uani 1 1 d . . . . .
C30 C 0.4757(6) 0.3313(6) 0.2423(4) 0.0476(11) Uani 1 1 d . . . . .
C12 C 0.4343(6) 0.2205(6) 0.2007(4) 0.0484(12) Uani 1 1 d . . . . .
H12 H 0.506795 0.219710 0.128573 0.058 Uiso 1 1 calc R . . . .
C13 C 0.1802(6) 0.2450(6) 0.2936(5) 0.0546(13) Uani 1 1 d . . . . .
C20 C 0.2867(7) -0.0226(6) 0.5087(5) 0.0583(14) Uani 1 1 d . . . . .
H20 H 0.218501 -0.022683 0.577613 0.070 Uiso 1 1 calc R . . . .
C25 C 0.3723(6) 0.3337(5) 0.3448(4) 0.0488(12) Uani 1 1 d . . . . .
C24 C 0.4137(6) 0.0862(5) 0.3026(4) 0.0473(11) Uani 1 1 d . . . . .
C19 C 0.3100(6) 0.0883(5) 0.4061(4) 0.0479(12) Uani 1 1 d . . . . .
C26 C 0.3964(8) 0.4245(6) 0.3953(6) 0.0639(16) Uani 1 1 d . . . . .
H26 H 0.330013 0.425654 0.464599 0.077 Uiso 1 1 calc R . . . .
C23 C 0.4945(7) -0.0241(6) 0.3020(5) 0.0585(14) Uani 1 1 d . . . . .
H23 H 0.563395 -0.025206 0.233792 0.070 Uiso 1 1 calc R . . . .
C14 C 0.0375(7) 0.2678(7) 0.2994(6) 0.0678(17) Uani 1 1 d . . . . .
H14 H -0.031234 0.268979 0.367745 0.081 Uiso 1 1 calc R . . . .
C1 C 0.9548(7) 0.8021(8) 0.2794(5) 0.0690(18) Uani 1 1 d . . . . .
C5 C 1.0616(10) 0.8612(10) 0.3113(7) 0.094(3) Uani 1 1 d . . . . .
H5 H 1.083855 0.953388 0.298146 0.113 Uiso 1 1 calc R . . . .
C21 C 0.3677(8) -0.1339(6) 0.5059(6) 0.0650(17) Uani 1 1 d . . . . .
H21 H 0.351616 -0.209534 0.573324 0.078 Uiso 1 1 calc R . . . .
C2 C 0.9616(8) 0.6579(7) 0.3159(6) 0.0723(19) Uani 1 1 d . . . . .
H2 H 0.904951 0.593542 0.306251 0.087 Uiso 1 1 calc R . . . .
C17 C 0.2450(7) 0.2662(7) 0.0930(5) 0.0674(17) Uani 1 1 d . . . . .
H17 H 0.314121 0.266564 0.024388 0.081 Uiso 1 1 calc R . . . .
C8 C 1.3123(10) 0.6644(8) 0.1195(6) 0.085(2) Uani 1 1 d . . . . .
H8 H 1.333942 0.576034 0.152503 0.102 Uiso 1 1 calc R . . . .
C27 C 0.5264(8) 0.5165(6) 0.3380(7) 0.073(2) Uani 1 1 d . . . . .
H27 H 0.545401 0.578540 0.370933 0.087 Uiso 1 1 calc R . . . .
C28 C 0.6236(8) 0.5171(7) 0.2370(6) 0.0671(17) Uani 1 1 d . . . . .
H28 H 0.706776 0.580380 0.200659 0.081 Uiso 1 1 calc R . . . .
C15 C -0.0007(8) 0.2892(9) 0.1993(7) 0.091(3) Uani 1 1 d . . . . .
H15 H -0.095932 0.304833 0.200984 0.109 Uiso 1 1 calc R . . . .
O1 O 0.7916(8) 0.8321(8) 0.1719(7) 0.130(3) Uani 1 1 d . . . . .
C3 C 1.0684(9) 0.6313(12) 0.3684(6) 0.100(3) Uani 1 1 d . . . . .
H3 H 1.095914 0.544926 0.399652 0.120 Uiso 1 1 calc R . . . .
C22 C 0.4703(9) -0.1325(7) 0.4052(7) 0.0733(19) Uani 1 1 d . . . . .
H22 H 0.525211 -0.206218 0.405984 0.088 Uiso 1 1 calc R . . . .
C4 C 1.1257(9) 0.7482(15) 0.3672(7) 0.109(4) Uani 1 1 d . . . . .
H4 H 1.198209 0.754670 0.399027 0.130 Uiso 1 1 calc R . . . .
C16 C 0.1023(8) 0.2873(9) 0.0984(7) 0.081(2) Uani 1 1 d . . . . .
H16 H 0.075207 0.300314 0.033064 0.097 Uiso 1 1 calc R . . . .
C6 C 1.3125(14) 0.8905(9) 0.0594(10) 0.129(5) Uani 1 1 d . . . . .
H6 H 1.333918 0.983013 0.045598 0.155 Uiso 1 1 calc R . . . .
C7 C 1.3777(9) 0.7835(12) 0.1169(7) 0.097(3) Uani 1 1 d . . . . .
H7 H 1.451034 0.790698 0.147697 0.117 Uiso 1 1 calc R . . . .
C9 C 1.2094(10) 0.6990(13) 0.0646(7) 0.102(3) Uani 1 1 d . . . . .
H9 H 1.147941 0.638712 0.054856 0.122 Uiso 1 1 calc R . . . .
C10 C 1.2144(13) 0.8383(15) 0.0274(6) 0.132(6) Uani 1 1 d . . . . .
H10 H 1.157683 0.889196 -0.014241 0.158 Uiso 1 1 calc R . . . .
C31 C 0.8745(9) 0.8801(9) 0.2068(8) 0.088(2) Uani 1 1 d . . . . .
H31 H 0.887364 0.975084 0.184998 0.106 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0488(5) 0.0615(6) 0.0397(4) -0.0116(4) 0.0021(3) -0.0054(4)
C29 0.049(3) 0.052(3) 0.051(3) -0.010(2) -0.009(2) -0.003(2)
C11 0.046(3) 0.051(3) 0.042(2) -0.012(2) 0.000(2) 0.002(2)
C18 0.052(3) 0.044(3) 0.040(2) -0.013(2) -0.012(2) 0.001(2)
C30 0.047(3) 0.049(3) 0.043(2) -0.013(2) -0.013(2) 0.005(2)
C12 0.045(3) 0.053(3) 0.040(2) -0.016(2) -0.004(2) 0.005(2)
C13 0.038(3) 0.057(3) 0.052(3) -0.009(2) -0.004(2) 0.002(2)
C20 0.063(4) 0.050(3) 0.046(3) -0.005(2) -0.010(2) -0.008(3)
C25 0.049(3) 0.046(3) 0.048(3) -0.015(2) -0.012(2) 0.015(2)
C24 0.045(3) 0.046(3) 0.049(3) -0.021(2) -0.010(2) 0.004(2)
C19 0.044(3) 0.052(3) 0.043(2) -0.015(2) -0.009(2) 0.000(2)
C26 0.084(5) 0.055(4) 0.061(3) -0.025(3) -0.029(3) 0.022(3)
C23 0.054(3) 0.062(4) 0.062(3) -0.028(3) -0.013(3) 0.007(3)
C14 0.052(3) 0.065(4) 0.072(4) -0.016(3) -0.009(3) 0.005(3)
C1 0.051(3) 0.081(5) 0.057(3) -0.022(3) 0.005(3) 0.006(3)
C5 0.086(6) 0.097(6) 0.080(5) -0.056(5) 0.025(4) -0.022(5)
C21 0.078(4) 0.045(3) 0.065(4) -0.004(3) -0.032(3) -0.006(3)
C2 0.061(4) 0.064(4) 0.067(4) -0.007(3) -0.004(3) -0.009(3)
C17 0.058(4) 0.074(4) 0.056(3) -0.008(3) -0.014(3) -0.005(3)
C8 0.102(6) 0.071(5) 0.056(4) -0.013(3) 0.000(4) 0.022(4)
C27 0.094(5) 0.046(3) 0.105(5) -0.033(3) -0.060(5) 0.017(3)
C28 0.075(4) 0.057(4) 0.063(4) -0.013(3) -0.023(3) -0.010(3)
C15 0.048(4) 0.102(6) 0.100(6) -0.007(5) -0.024(4) 0.006(4)
O1 0.101(5) 0.132(6) 0.160(7) -0.041(5) -0.058(5) 0.029(5)
C3 0.067(5) 0.143(8) 0.044(3) 0.008(4) 0.002(3) 0.002(5)
C22 0.091(5) 0.042(3) 0.102(5) -0.028(3) -0.050(4) 0.016(3)
C4 0.063(5) 0.219(13) 0.054(4) -0.073(6) -0.003(3) -0.008(7)
C16 0.073(5) 0.093(5) 0.072(4) -0.014(4) -0.035(4) 0.000(4)
C6 0.128(9) 0.052(5) 0.111(8) -0.013(5) 0.074(7) -0.020(5)
C7 0.054(4) 0.143(9) 0.075(5) -0.053(5) 0.022(3) -0.018(5)
C9 0.076(5) 0.167(10) 0.070(5) -0.066(6) -0.010(4) -0.006(6)
C10 0.119(9) 0.169(12) 0.038(3) 0.015(5) 0.013(4) 0.081(8)
C31 0.075(5) 0.066(5) 0.114(6) -0.034(4) -0.015(5) 0.020(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C1 2.021(6) . ?
Fe1 C5 2.028(8) . ?
Fe1 C2 2.032(6) . ?
Fe1 C8 2.023(8) . ?
Fe1 C3 2.030(7) . ?
Fe1 C4 2.025(7) . ?
Fe1 C6 2.030(7) . ?
Fe1 C7 2.046(7) . ?
Fe1 C9 2.004(8) . ?
Fe1 C10 2.020(8) . ?
C29 H29 0.9300 . ?
C29 C30 1.374(7) . ?
C29 C28 1.384(9) . ?
C11 H11 0.9800 . ?
C11 C13 1.532(8) . ?
C11 C25 1.533(8) . ?
C11 C19 1.505(8) . ?
C18 C12 1.522(7) . ?
C18 C13 1.397(7) . ?
C18 C17 1.370(8) . ?
C30 C12 1.525(8) . ?
C30 C25 1.399(7) . ?
C12 H12 0.9800 . ?
C12 C24 1.533(7) . ?
C13 C14 1.383(8) . ?
C20 H20 0.9300 . ?
C20 C19 1.394(7) . ?
C20 C21 1.399(9) . ?
C25 C26 1.372(8) . ?
C24 C19 1.408(7) . ?
C24 C23 1.386(8) . ?
C26 H26 0.9300 . ?
C26 C27 1.415(9) . ?
C23 H23 0.9300 . ?
C23 C22 1.386(9) . ?
C14 H14 0.9300 . ?
C14 C15 1.405(11) . ?
C1 C5 1.434(12) . ?
C1 C2 1.423(10) . ?
C1 C31 1.446(11) . ?
C5 H5 0.9300 . ?
C5 C4 1.414(14) . ?
C21 H21 0.9300 . ?
C21 C22 1.366(10) . ?
C2 H2 0.9300 . ?
C2 C3 1.384(11) . ?
C17 H17 0.9300 . ?
C17 C16 1.381(10) . ?
C8 H8 0.9300 . ?
C8 C7 1.378(12) . ?
C8 C9 1.376(13) . ?
C27 H27 0.9300 . ?
C27 C28 1.350(10) . ?
C28 H28 0.9300 . ?
C15 H15 0.9300 . ?
C15 C16 1.381(11) . ?
O1 C31 1.214(11) . ?
C3 H3 0.9300 . ?
C3 C4 1.332(14) . ?
C22 H22 0.9300 . ?
C4 H4 0.9300 . ?
C16 H16 0.9300 . ?
C6 H6 0.9300 . ?
C6 C7 1.389(15) . ?
C6 C10 1.329(17) . ?
C7 H7 0.9300 . ?
C9 H9 0.9300 . ?
C9 C10 1.361(16) . ?
C10 H10 0.9300 . ?
C31 H31 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 C5 41.5(3) . . ?
C1 Fe1 C2 41.1(3) . . ?
C1 Fe1 C8 158.2(4) . . ?
C1 Fe1 C3 67.8(3) . . ?
C1 Fe1 C4 67.7(3) . . ?
C1 Fe1 C6 126.5(4) . . ?
C1 Fe1 C7 161.4(4) . . ?
C5 Fe1 C2 69.1(3) . . ?
C5 Fe1 C3 67.8(4) . . ?
C5 Fe1 C6 109.9(4) . . ?
C5 Fe1 C7 123.5(4) . . ?
C2 Fe1 C7 155.7(4) . . ?
C8 Fe1 C5 158.1(4) . . ?
C8 Fe1 C2 121.3(3) . . ?
C8 Fe1 C3 106.9(4) . . ?
C8 Fe1 C4 122.1(4) . . ?
C8 Fe1 C6 66.3(4) . . ?
C8 Fe1 C7 39.6(4) . . ?
C3 Fe1 C2 39.9(3) . . ?
C3 Fe1 C6 157.4(6) . . ?
C3 Fe1 C7 121.1(4) . . ?
C4 Fe1 C5 40.8(4) . . ?
C4 Fe1 C2 66.3(3) . . ?
C4 Fe1 C3 38.3(4) . . ?
C4 Fe1 C6 125.2(6) . . ?
C4 Fe1 C7 108.2(4) . . ?
C6 Fe1 C2 162.3(5) . . ?
C6 Fe1 C7 39.8(4) . . ?
C9 Fe1 C1 124.0(4) . . ?
C9 Fe1 C5 160.5(5) . . ?
C9 Fe1 C2 108.5(4) . . ?
C9 Fe1 C8 40.0(4) . . ?
C9 Fe1 C3 123.6(5) . . ?
C9 Fe1 C4 157.4(5) . . ?
C9 Fe1 C6 66.1(4) . . ?
C9 Fe1 C7 66.8(4) . . ?
C9 Fe1 C10 39.5(5) . . ?
C10 Fe1 C1 111.7(3) . . ?
C10 Fe1 C5 125.5(5) . . ?
C10 Fe1 C2 127.0(5) . . ?
C10 Fe1 C8 66.0(3) . . ?
C10 Fe1 C3 160.9(6) . . ?
C10 Fe1 C4 160.6(6) . . ?
C10 Fe1 C6 38.3(5) . . ?
C10 Fe1 C7 65.7(4) . . ?
C30 C29 H29 120.4 . . ?
C30 C29 C28 119.2(6) . . ?
C28 C29 H29 120.4 . . ?
C13 C11 H11 112.9 . . ?
C13 C11 C25 105.2(4) . . ?
C25 C11 H11 112.9 . . ?
C19 C11 H11 112.9 . . ?
C19 C11 C13 106.3(5) . . ?
C19 C11 C25 105.8(4) . . ?
C13 C18 C12 112.8(4) . . ?
C17 C18 C12 126.4(5) . . ?
C17 C18 C13 120.8(6) . . ?
C29 C30 C12 125.7(5) . . ?
C29 C30 C25 120.8(5) . . ?
C25 C30 C12 113.4(5) . . ?
C18 C12 C30 106.0(4) . . ?
C18 C12 H12 113.1 . . ?
C18 C12 C24 106.2(4) . . ?
C30 C12 H12 113.1 . . ?
C30 C12 C24 104.7(4) . . ?
C24 C12 H12 113.1 . . ?
C18 C13 C11 113.3(5) . . ?
C14 C13 C11 126.0(5) . . ?
C14 C13 C18 120.6(6) . . ?
C19 C20 H20 120.6 . . ?
C19 C20 C21 118.8(6) . . ?
C21 C20 H20 120.6 . . ?
C30 C25 C11 112.6(5) . . ?
C26 C25 C11 127.0(5) . . ?
C26 C25 C30 120.3(5) . . ?
C19 C24 C12 112.8(5) . . ?
C23 C24 C12 126.2(5) . . ?
C23 C24 C19 120.7(5) . . ?
C20 C19 C11 127.1(5) . . ?
C20 C19 C24 119.7(6) . . ?
C24 C19 C11 113.1(4) . . ?
C25 C26 H26 121.3 . . ?
C25 C26 C27 117.4(6) . . ?
C27 C26 H26 121.3 . . ?
C24 C23 H23 120.7 . . ?
C24 C23 C22 118.6(6) . . ?
C22 C23 H23 120.7 . . ?
C13 C14 H14 120.9 . . ?
C13 C14 C15 118.1(6) . . ?
C15 C14 H14 120.9 . . ?
C5 C1 Fe1 69.5(4) . . ?
C5 C1 C31 124.5(8) . . ?
C2 C1 Fe1 69.9(4) . . ?
C2 C1 C5 107.5(7) . . ?
C2 C1 C31 127.3(8) . . ?
C31 C1 Fe1 118.4(5) . . ?
Fe1 C5 H5 125.5 . . ?
C1 C5 Fe1 69.0(4) . . ?
C1 C5 H5 127.6 . . ?
C4 C5 Fe1 69.5(5) . . ?
C4 C5 C1 104.7(8) . . ?
C4 C5 H5 127.6 . . ?
C20 C21 H21 119.7 . . ?
C22 C21 C20 120.6(5) . . ?
C22 C21 H21 119.7 . . ?
Fe1 C2 H2 126.1 . . ?
C1 C2 Fe1 69.0(4) . . ?
C1 C2 H2 126.4 . . ?
C3 C2 Fe1 70.0(4) . . ?
C3 C2 C1 107.2(8) . . ?
C3 C2 H2 126.4 . . ?
C18 C17 H17 120.5 . . ?
C18 C17 C16 119.0(7) . . ?
C16 C17 H17 120.5 . . ?
Fe1 C8 H8 125.2 . . ?
C7 C8 Fe1 71.1(5) . . ?
C7 C8 H8 125.9 . . ?
C9 C8 Fe1 69.3(5) . . ?
C9 C8 H8 125.9 . . ?
C9 C8 C7 108.1(8) . . ?
C26 C27 H27 118.9 . . ?
C28 C27 C26 122.2(6) . . ?
C28 C27 H27 118.9 . . ?
C29 C28 H28 120.0 . . ?
C27 C28 C29 120.0(6) . . ?
C27 C28 H28 120.0 . . ?
C14 C15 H15 119.8 . . ?
C16 C15 C14 120.4(7) . . ?
C16 C15 H15 119.8 . . ?
Fe1 C3 H3 125.7 . . ?
C2 C3 Fe1 70.1(4) . . ?
C2 C3 H3 125.2 . . ?
C4 C3 Fe1 70.6(5) . . ?
C4 C3 C2 109.6(9) . . ?
C4 C3 H3 125.2 . . ?
C23 C22 H22 119.2 . . ?
C21 C22 C23 121.6(6) . . ?
C21 C22 H22 119.2 . . ?
Fe1 C4 H4 126.4 . . ?
C5 C4 Fe1 69.7(4) . . ?
C5 C4 H4 124.5 . . ?
C3 C4 Fe1 71.1(4) . . ?
C3 C4 C5 111.0(8) . . ?
C3 C4 H4 124.5 . . ?
C17 C16 H16 119.5 . . ?
C15 C16 C17 121.0(7) . . ?
C15 C16 H16 119.5 . . ?
Fe1 C6 H6 124.7 . . ?
C7 C6 Fe1 70.7(4) . . ?
C7 C6 H6 125.8 . . ?
C10 C6 Fe1 70.4(5) . . ?
C10 C6 H6 125.8 . . ?
C10 C6 C7 108.4(9) . . ?
Fe1 C7 H7 126.1 . . ?
C8 C7 Fe1 69.3(4) . . ?
C8 C7 C6 106.5(9) . . ?
C8 C7 H7 126.7 . . ?
C6 C7 Fe1 69.5(5) . . ?
C6 C7 H7 126.7 . . ?
Fe1 C9 H9 123.6 . . ?
C8 C9 Fe1 70.7(5) . . ?
C8 C9 H9 126.5 . . ?
C10 C9 Fe1 70.8(6) . . ?
C10 C9 C8 107.1(9) . . ?
C10 C9 H9 126.5 . . ?
Fe1 C10 H10 125.6 . . ?
C6 C10 Fe1 71.3(6) . . ?
C6 C10 C9 109.8(9) . . ?
C6 C10 H10 125.1 . . ?
C9 C10 Fe1 69.6(4) . . ?
C9 C10 H10 125.1 . . ?
C1 C31 H31 117.2 . . ?
O1 C31 C1 125.5(9) . . ?
O1 C31 H31 117.2 . . ?
_shelx_res_file
;
TITL smm577_a.res in P-1
smm577.res
created by SHELXL-2018/3 at 14:02:48 on 26-Oct-2019
REM Old TITL smm577_a.res in P-1
REM SHELXT solution in P-1
REM R1 0.257, Rweak 0.047, Alpha 0.091, Orientation as input
REM Formula found by SHELXT: C31 Fe O
CELL 0.71073 9.6767 10.3972 12.9455 70.641 71.847 89.794
ZERR 2 0.0012 0.0012 0.0015 0.01 0.011 0.01
LATT 1
SFAC C H Fe O
UNIT 62 48 2 2
L.S. 10
PLAN 10
SIZE 0.38 0.36 0.29
BOND $H
list 4
fmap 2
acta 52
REM
REM
REM
WGHT 0.200000
FVAR 0.73803
FE1 3 1.157191 0.760595 0.201961 11.00000 0.04880 0.06150 =
0.03971 -0.01163 0.00206 -0.00539
C29 1 0.599587 0.423533 0.187629 11.00000 0.04852 0.05183 =
0.05051 -0.00975 -0.00886 -0.00269
AFIX 43
H29 2 0.666472 0.423134 0.118301 11.00000 -1.20000
AFIX 0
C11 1 0.243519 0.221502 0.392278 11.00000 0.04569 0.05062 =
0.04240 -0.01166 0.00042 0.00164
AFIX 13
H11 2 0.170900 0.222446 0.464270 11.00000 -1.20000
AFIX 0
C18 1 0.283232 0.244824 0.190318 11.00000 0.05203 0.04424 =
0.03997 -0.01321 -0.01162 0.00096
C30 1 0.475693 0.331266 0.242289 11.00000 0.04705 0.04894 =
0.04319 -0.01323 -0.01302 0.00546
C12 1 0.434299 0.220541 0.200658 11.00000 0.04461 0.05280 =
0.03981 -0.01558 -0.00365 0.00515
AFIX 13
H12 2 0.506795 0.219710 0.128573 11.00000 -1.20000
AFIX 0
C13 1 0.180201 0.245038 0.293572 11.00000 0.03781 0.05744 =
0.05230 -0.00892 -0.00376 0.00168
C20 1 0.286694 -0.022627 0.508658 11.00000 0.06339 0.05015 =
0.04572 -0.00455 -0.00967 -0.00795
AFIX 43
H20 2 0.218501 -0.022683 0.577613 11.00000 -1.20000
AFIX 0
C25 1 0.372349 0.333674 0.344794 11.00000 0.04872 0.04585 =
0.04802 -0.01534 -0.01211 0.01455
C24 1 0.413699 0.086166 0.302642 11.00000 0.04524 0.04634 =
0.04902 -0.02055 -0.00951 0.00401
C19 1 0.310046 0.088320 0.406131 11.00000 0.04352 0.05174 =
0.04311 -0.01486 -0.00874 0.00010
C26 1 0.396447 0.424526 0.395348 11.00000 0.08416 0.05452 =
0.06077 -0.02522 -0.02894 0.02214
AFIX 43
H26 2 0.330013 0.425654 0.464599 11.00000 -1.20000
AFIX 0
C23 1 0.494458 -0.024052 0.302009 11.00000 0.05353 0.06153 =
0.06155 -0.02805 -0.01340 0.00708
AFIX 43
H23 2 0.563395 -0.025206 0.233792 11.00000 -1.20000
AFIX 0
C14 1 0.037495 0.267845 0.299432 11.00000 0.05191 0.06519 =
0.07155 -0.01581 -0.00877 0.00457
AFIX 43
H14 2 -0.031234 0.268979 0.367745 11.00000 -1.20000
AFIX 0
C1 1 0.954818 0.802069 0.279425 11.00000 0.05072 0.08139 =
0.05660 -0.02238 0.00518 0.00593
C5 1 1.061628 0.861169 0.311321 11.00000 0.08577 0.09723 =
0.08037 -0.05601 0.02520 -0.02172
AFIX 43
H5 2 1.083855 0.953388 0.298146 11.00000 -1.20000
AFIX 0
C21 1 0.367733 -0.133917 0.505934 11.00000 0.07839 0.04543 =
0.06523 -0.00404 -0.03187 -0.00598
AFIX 43
H21 2 0.351616 -0.209534 0.573324 11.00000 -1.20000
AFIX 0
C2 1 0.961644 0.657901 0.315885 11.00000 0.06123 0.06393 =
0.06671 -0.00698 -0.00409 -0.00913
AFIX 43
H2 2 0.904951 0.593542 0.306251 11.00000 -1.20000
AFIX 0
C17 1 0.245000 0.266218 0.093049 11.00000 0.05753 0.07416 =
0.05567 -0.00812 -0.01380 -0.00526
AFIX 43
H17 2 0.314121 0.266564 0.024388 11.00000 -1.20000
AFIX 0
C8 1 1.312288 0.664403 0.119473 11.00000 0.10207 0.07102 =
0.05562 -0.01269 -0.00024 0.02248
AFIX 43
H8 2 1.333942 0.576034 0.152503 11.00000 -1.20000
AFIX 0
C27 1 0.526372 0.516461 0.337976 11.00000 0.09369 0.04568 =
0.10456 -0.03310 -0.05970 0.01660
AFIX 43
H27 2 0.545401 0.578540 0.370933 11.00000 -1.20000
AFIX 0
C28 1 0.623602 0.517076 0.237036 11.00000 0.07497 0.05742 =
0.06263 -0.01264 -0.02271 -0.01012
AFIX 43
H28 2 0.706776 0.580380 0.200659 11.00000 -1.20000
AFIX 0
C15 1 -0.000693 0.289242 0.199311 11.00000 0.04757 0.10240 =
0.10040 -0.00702 -0.02382 0.00560
AFIX 43
H15 2 -0.095932 0.304833 0.200984 11.00000 -1.20000
AFIX 0
O1 4 0.791573 0.832061 0.171932 11.00000 0.10128 0.13196 =
0.15960 -0.04073 -0.05792 0.02870
C3 1 1.068409 0.631256 0.368384 11.00000 0.06696 0.14306 =
0.04448 0.00773 0.00162 0.00152
AFIX 43
H3 2 1.095914 0.544926 0.399652 11.00000 -1.20000
AFIX 0
C22 1 0.470272 -0.132543 0.405247 11.00000 0.09134 0.04245 =
0.10171 -0.02764 -0.05020 0.01619
AFIX 43
H22 2 0.525211 -0.206218 0.405984 11.00000 -1.20000
AFIX 0
C4 1 1.125687 0.748187 0.367247 11.00000 0.06289 0.21911 =
0.05352 -0.07348 -0.00346 -0.00757
AFIX 43
H4 2 1.198209 0.754670 0.399027 11.00000 -1.20000
AFIX 0
C16 1 0.102323 0.287268 0.098413 11.00000 0.07299 0.09293 =
0.07187 -0.01368 -0.03456 0.00047
AFIX 43
H16 2 0.075207 0.300314 0.033064 11.00000 -1.20000
AFIX 0
C6 1 1.312513 0.890480 0.059387 11.00000 0.12838 0.05204 =
0.11126 -0.01270 0.07397 -0.02046
AFIX 43
H6 2 1.333918 0.983013 0.045598 11.00000 -1.20000
AFIX 0
C7 1 1.377669 0.783450 0.116924 11.00000 0.05375 0.14318 =
0.07539 -0.05289 0.02199 -0.01785
AFIX 43
H7 2 1.451034 0.790698 0.147697 11.00000 -1.20000
AFIX 0
C9 1 1.209362 0.699047 0.064626 11.00000 0.07621 0.16704 =
0.07048 -0.06612 -0.00962 -0.00612
AFIX 43
H9 2 1.147941 0.638712 0.054856 11.00000 -1.20000
AFIX 0
C10 1 1.214402 0.838265 0.027374 11.00000 0.11852 0.16918 =
0.03797 0.01517 0.01253 0.08074
AFIX 43
H10 2 1.157683 0.889196 -0.014241 11.00000 -1.20000
AFIX 0
C31 1 0.874466 0.880086 0.206821 11.00000 0.07498 0.06593 =
0.11358 -0.03361 -0.01508 0.02031
AFIX 43
H31 2 0.887364 0.975084 0.184998 11.00000 -1.20000
AFIX 0
HKLF 4
REM smm577_a.res in P-1
REM wR2 = 0.3924, GooF = S = 0.961, Restrained GooF = 0.961 for all data
REM R1 = 0.1203 for 2885 Fo > 4sig(Fo) and 0.2121 for all 7481 data
REM 298 parameters refined using 0 restraints
END
WGHT 0.2000 0.0000
REM Highest difference peak 1.467, deepest hole -0.815, 1-sigma level 0.132
Q1 1 1.0726 0.7857 0.1491 11.00000 0.05 1.47
Q2 1 0.5159 0.4854 0.1264 11.00000 0.05 1.40
Q3 1 0.1762 -0.0254 0.4633 11.00000 0.05 1.25
Q4 1 1.2321 0.7452 0.2550 11.00000 0.05 1.16
Q5 1 0.7555 0.9091 0.0677 11.00000 0.05 0.61
Q6 1 1.1877 0.7284 0.4326 11.00000 0.05 0.56
Q7 1 1.1106 0.4841 0.5328 11.00000 0.05 0.55
Q8 1 0.1938 0.2641 0.1296 11.00000 0.05 0.49
Q9 1 1.4833 0.7511 0.1601 11.00000 0.05 0.46
Q10 1 1.2529 0.6867 0.0727 11.00000 0.05 0.45
;
_shelx_res_checksum 77159
_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_4
_database_code_depnum_ccdc_archive 'CCDC 1586856'
loop_
_audit_author_name
_audit_author_address
'Ajeet Singh'
;Indian Institute of Technology Indore
India
;
_audit_update_record
;
2019-10-26 deposited with the CCDC. 2020-01-20 downloaded from the CCDC.
;
_audit_creation_date 2019-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic TripPCPfc
_chemical_formula_moiety 'C28 H24 Fe, C20 H14'
_chemical_formula_sum 'C48 H38 Fe'
_chemical_formula_weight 670.63
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 7.9500(4)
_cell_length_b 28.507(2)
_cell_length_c 15.5007(8)
_cell_angle_alpha 90
_cell_angle_beta 104.262(5)
_cell_angle_gamma 90
_cell_volume 3404.6(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 3195
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 65.6080
_cell_measurement_theta_min 4.2690
_shelx_estimated_absorpt_T_max 0.376
_shelx_estimated_absorpt_T_min 0.312
_exptl_absorpt_coefficient_mu 3.800
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.67892
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour orange
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.308
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1408
_exptl_crystal_preparation CHCl3Hexane
_exptl_crystal_recrystallization_method CHCl3hexane
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.34
_exptl_crystal_size_min 0.32
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0946
_diffrn_reflns_av_unetI/netI 0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 34
_diffrn_reflns_limit_k_min -34
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 23737
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full 66.9682
_diffrn_reflns_theta_max 72.124
_diffrn_reflns_theta_min 5.509
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.0309
_diffrn_detector_type Eos
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega 17.00 61.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 57.0000 -90.0000 44
#__ type_ start__ end____ width___ exp.time_
2 omega 51.00 91.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 37.0000 -180.0000 40
#__ type_ start__ end____ width___ exp.time_
3 omega 38.00 69.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -37.0000 -180.0000 31
#__ type_ start__ end____ width___ exp.time_
4 omega 47.00 104.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -50.0000 -150.0000 57
#__ type_ start__ end____ width___ exp.time_
5 omega 91.00 116.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -111.0000 -60.0000 25
#__ type_ start__ end____ width___ exp.time_
6 omega 101.00 134.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -77.0000 -30.0000 33
#__ type_ start__ end____ width___ exp.time_
7 omega 74.00 102.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -50.0000 60.0000 28
#__ type_ start__ end____ width___ exp.time_
8 omega 65.00 92.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -25.0000 0.0000 27
#__ type_ start__ end____ width___ exp.time_
9 omega 66.00 93.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -77.0000 -30.0000 27
#__ type_ start__ end____ width___ exp.time_
10 omega 50.00 98.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -50.0000 -60.0000 48
#__ type_ start__ end____ width___ exp.time_
11 omega 52.00 93.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -25.0000 -120.0000 41
#__ type_ start__ end____ width___ exp.time_
12 omega 79.00 178.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 25.0000 -60.0000 99
#__ type_ start__ end____ width___ exp.time_
13 omega 122.00 171.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 63.0000 -150.0000 49
#__ type_ start__ end____ width___ exp.time_
14 omega 145.00 173.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 111.0000 -180.0000 28
#__ type_ start__ end____ width___ exp.time_
15 omega 102.00 175.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 111.0000 -60.0000 73
#__ type_ start__ end____ width___ exp.time_
16 omega 95.00 172.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 50.0000 0.0000 77
#__ type_ start__ end____ width___ exp.time_
17 omega 57.00 85.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -37.0000 120.0000 28
#__ type_ start__ end____ width___ exp.time_
18 omega 38.00 81.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -37.0000 60.0000 43
#__ type_ start__ end____ width___ exp.time_
19 omega 40.00 81.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -25.0000 -30.0000 41
#__ type_ start__ end____ width___ exp.time_
20 omega 32.00 121.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 37.0000 -120.0000 89
#__ type_ start__ end____ width___ exp.time_
21 omega 48.00 146.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -91.0000 -150.0000 98
#__ type_ start__ end____ width___ exp.time_
22 omega 45.00 105.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 -125.0000 30.0000 60
#__ type_ start__ end____ width___ exp.time_
23 omega 53.00 107.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -111.0000 60.0000 54
#__ type_ start__ end____ width___ exp.time_
24 omega 51.00 116.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 108.0000 -111.0000 150.0000 65
#__ type_ start__ end____ width___ exp.time_
25 omega 16.00 65.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 -57.0000 90.0000 49
#__ type_ start__ end____ width___ exp.time_
26 omega -12.00 36.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 -77.0000 -60.0000 48
#__ type_ start__ end____ width___ exp.time_
27 omega 38.00 77.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 -125.0000 -90.0000 39
#__ type_ start__ end____ width___ exp.time_
28 omega -15.00 79.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 -37.0000 -60.0000 94
#__ type_ start__ end____ width___ exp.time_
29 omega 38.00 118.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 54.0000 57.0000 90.0000 80
#__ type_ start__ end____ width___ exp.time_
30 omega -19.00 9.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -77.0000 -180.0000 28
#__ type_ start__ end____ width___ exp.time_
31 omega -26.00 30.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -77.0000 -60.0000 56
#__ type_ start__ end____ width___ exp.time_
32 omega -18.00 15.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 57.0000 -90.0000 33
#__ type_ start__ end____ width___ exp.time_
33 omega -40.00 9.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 103.0000 79.0000 49
#__ type_ start__ end____ width___ exp.time_
34 omega -66.00 -37.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -77.0000 -60.0000 29
#__ type_ start__ end____ width___ exp.time_
35 omega -67.00 -38.00 1.0000 9.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -77.0000 -180.0000 29
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 0.0483958000
_diffrn_orient_matrix_UB_12 -0.0454596000
_diffrn_orient_matrix_UB_13 -0.0137459000
_diffrn_orient_matrix_UB_21 -0.0902845000
_diffrn_orient_matrix_UB_22 -0.0252047000
_diffrn_orient_matrix_UB_23 -0.0307435000
_diffrn_orient_matrix_UB_31 -0.0044848000
_diffrn_orient_matrix_UB_32 0.0149850000
_diffrn_orient_matrix_UB_33 -0.0941992000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3490
_reflns_number_total 6536
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.031
_refine_diff_density_min -0.592
_refine_diff_density_rms 0.079
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.027
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 442
_refine_ls_number_reflns 6536
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1747
_refine_ls_R_factor_gt 0.1158
_refine_ls_restrained_S_all 1.027
_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^)+(0.1683P)^2^+5.1133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.3075
_refine_ls_wR_factor_ref 0.3614
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
C12(H12), C11(H11), C8(H8), C6(H6), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
C48(H48A,H48B), C47(H47A,H47B), C39(H39A,H39B), C40(H40A,H40B)
2.c Aromatic/amide H refined with riding coordinates:
C26(H26), C20(H20), C38(H38), C23(H23), C45(H45), C21(H21), C29(H29),
C35(H35), C22(H22), C14(H14), C27(H27), C46(H46), C42(H42), C17(H17), C43(H43),
C28(H28), C36(H36), C15(H15), C5(H5), C3(H3), C16(H16), C2(H2), C9(H9),
C4(H4), C10(H10)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.64005(15) 0.91007(5) 0.81606(8) 0.0736(5) Uani 1 1 d . . . . .
C19 C 0.3827(8) 0.5814(3) 0.6634(5) 0.0625(17) Uani 1 1 d . . . . .
C25 C 0.5935(8) 0.6419(3) 0.7156(5) 0.0647(18) Uani 1 1 d . . . . .
C30 C 0.5024(8) 0.6549(3) 0.7791(5) 0.0643(18) Uani 1 1 d . . . . .
C18 C 0.5493(9) 0.5772(3) 0.8443(5) 0.071(2) Uani 1 1 d . . . . .
C24 C 0.2928(9) 0.5931(3) 0.7250(5) 0.0646(18) Uani 1 1 d . . . . .
C12 C 0.4101(9) 0.6143(3) 0.8106(5) 0.0670(19) Uani 1 1 d . . . . .
H12 H 0.346657 0.623366 0.854808 0.080 Uiso 1 1 calc R . . . .
C34 C 0.1501(10) 0.8391(3) 0.4593(5) 0.072(2) Uani 1 1 d . . . . .
C33 C 0.3020(9) 0.8186(3) 0.5103(4) 0.0670(19) Uani 1 1 d . . . . .
C13 C 0.6386(8) 0.5649(3) 0.7807(5) 0.0653(18) Uani 1 1 d . . . . .
C26 C 0.6807(9) 0.6764(3) 0.6799(5) 0.0681(19) Uani 1 1 d . . . . .
H26 H 0.742193 0.668432 0.638146 0.082 Uiso 1 1 calc R . . . .
C11 C 0.5764(8) 0.5911(2) 0.6944(5) 0.0602(17) Uani 1 1 d . . . . .
H11 H 0.639156 0.581919 0.649996 0.072 Uiso 1 1 calc R . . . .
C20 C 0.2954(9) 0.5636(3) 0.5805(5) 0.0682(19) Uani 1 1 d . . . . .
H20 H 0.355011 0.556363 0.537554 0.082 Uiso 1 1 calc R . . . .
C38 C 0.3276(9) 0.7713(3) 0.5056(5) 0.075(2) Uani 1 1 d . . . . .
H38 H 0.427642 0.758051 0.541345 0.090 Uiso 1 1 calc R . . . .
C23 C 0.1155(9) 0.5868(3) 0.7083(6) 0.072(2) Uani 1 1 d . . . . .
H23 H 0.055127 0.595567 0.750029 0.087 Uiso 1 1 calc R . . . .
C45 C 0.0808(9) 0.7989(3) 0.6446(5) 0.072(2) Uani 1 1 d . . . . .
H45 H 0.149983 0.814530 0.693253 0.087 Uiso 1 1 calc R . . . .
C21 C 0.1158(9) 0.5568(3) 0.5638(5) 0.073(2) Uani 1 1 d . . . . .
H21 H 0.055171 0.545258 0.508834 0.088 Uiso 1 1 calc R . . . .
C29 C 0.4953(9) 0.7012(3) 0.8034(5) 0.074(2) Uani 1 1 d . . . . .
H29 H 0.431735 0.709696 0.843935 0.088 Uiso 1 1 calc R . . . .
C35 C 0.0560(10) 0.8124(4) 0.3897(5) 0.079(2) Uani 1 1 d . . . . .
H35 H -0.029252 0.826634 0.345506 0.094 Uiso 1 1 calc R . . . .
C22 C 0.0289(9) 0.5670(3) 0.6267(6) 0.074(2) Uani 1 1 d . . . . .
H22 H -0.089301 0.560718 0.615565 0.089 Uiso 1 1 calc R . . . .
C14 C 0.7687(9) 0.5311(3) 0.8010(6) 0.076(2) Uani 1 1 d . . . . .
H14 H 0.830024 0.522888 0.759295 0.091 Uiso 1 1 calc R . . . .
C27 C 0.6753(10) 0.7224(3) 0.7067(6) 0.076(2) Uani 1 1 d . . . . .
H27 H 0.735143 0.745160 0.683316 0.091 Uiso 1 1 calc R . . . .
C44 C -0.0417(10) 0.8233(3) 0.5810(5) 0.075(2) Uani 1 1 d . . . . .
C1 C 0.6570(11) 0.8921(4) 0.6921(5) 0.088(3) Uani 1 1 d . . . . .
C46 C 0.0984(10) 0.7507(3) 0.6341(6) 0.080(2) Uani 1 1 d . . . . .
H46 H 0.179504 0.734077 0.676589 0.096 Uiso 1 1 calc R . . . .
C42 C -0.1477(10) 0.7510(4) 0.5135(6) 0.083(2) Uani 1 1 d . . . . .
H42 H -0.233191 0.734310 0.473390 0.099 Uiso 1 1 calc R . . . .
C17 C 0.5882(11) 0.5556(3) 0.9260(5) 0.084(2) Uani 1 1 d . . . . .
H17 H 0.526927 0.563749 0.967659 0.101 Uiso 1 1 calc R . . . .
C41 C -0.0016(12) 0.7276(3) 0.5625(6) 0.080(2) Uani 1 1 d . . . . .
C43 C -0.1669(9) 0.7979(3) 0.5236(5) 0.075(2) Uani 1 1 d . . . . .
H43 H -0.266382 0.812911 0.491210 0.090 Uiso 1 1 calc R . . . .
C28 C 0.5835(10) 0.7352(3) 0.7673(5) 0.074(2) Uani 1 1 d . . . . .
H28 H 0.580177 0.766467 0.784084 0.089 Uiso 1 1 calc R . . . .
C36 C 0.0861(10) 0.7650(4) 0.3847(5) 0.080(2) Uani 1 1 d . . . . .
H36 H 0.021894 0.747851 0.336714 0.096 Uiso 1 1 calc R . . . .
C15 C 0.8064(11) 0.5097(3) 0.8850(7) 0.088(3) Uani 1 1 d . . . . .
H15 H 0.892965 0.487047 0.898834 0.105 Uiso 1 1 calc R . . . .
C37 C 0.2095(10) 0.7425(3) 0.4493(5) 0.078(2) Uani 1 1 d . . . . .
C5 C 0.6663(13) 0.9416(4) 0.7020(7) 0.095(3) Uani 1 1 d . . . . .
H5 H 0.590308 0.963202 0.668112 0.115 Uiso 1 1 calc R . . . .
C3 C 0.8896(11) 0.9106(4) 0.8046(7) 0.097(3) Uani 1 1 d . . . . .
H3 H 0.989130 0.908371 0.850827 0.116 Uiso 1 1 calc R . . . .
C16 C 0.7170(12) 0.5219(3) 0.9473(7) 0.094(3) Uani 1 1 d . . . . .
H16 H 0.742810 0.507644 1.003031 0.112 Uiso 1 1 calc R . . . .
C2 C 0.7988(12) 0.8732(4) 0.7582(7) 0.093(3) Uani 1 1 d . . . . .
H2 H 0.825290 0.841540 0.768336 0.112 Uiso 1 1 calc R . . . .
C9 C 0.6317(15) 0.8958(5) 0.9422(6) 0.104(3) Uani 1 1 d . . . . .
H9 H 0.727090 0.885621 0.985988 0.124 Uiso 1 1 calc R . . . .
C4 C 0.8078(15) 0.9519(4) 0.7706(7) 0.103(3) Uani 1 1 d . . . . .
H4 H 0.842915 0.981887 0.791031 0.124 Uiso 1 1 calc R . . . .
C48 C 0.0771(13) 0.8829(3) 0.4874(7) 0.095(3) Uani 1 1 d . . . . .
H48A H -0.006744 0.895970 0.436732 0.114 Uiso 1 1 calc R . . . .
H48B H 0.169780 0.905627 0.506045 0.114 Uiso 1 1 calc R . . . .
C47 C -0.0135(13) 0.8749(3) 0.5655(7) 0.096(3) Uani 1 1 d . . . . .
H47A H 0.057734 0.888482 0.619653 0.115 Uiso 1 1 calc R . . . .
H47B H -0.124561 0.890882 0.551823 0.115 Uiso 1 1 calc R . . . .
C8 C 0.588(2) 0.9393(4) 0.9267(9) 0.116(4) Uani 1 1 d . . . . .
H8 H 0.650438 0.966034 0.959327 0.139 Uiso 1 1 calc R . . . .
C39 C 0.1955(14) 0.6910(3) 0.4718(8) 0.102(3) Uani 1 1 d . . . . .
H39A H 0.307666 0.679846 0.505544 0.123 Uiso 1 1 calc R . . . .
H39B H 0.162686 0.672961 0.417238 0.123 Uiso 1 1 calc R . . . .
C10 C 0.524(2) 0.8680(4) 0.8883(11) 0.138(5) Uani 1 1 d . . . . .
H10 H 0.528209 0.835378 0.888830 0.166 Uiso 1 1 calc R . . . .
C6 C 0.4017(15) 0.8953(11) 0.8297(9) 0.209(12) Uani 1 1 d . . . . .
H6 H 0.299875 0.884990 0.784063 0.251 Uiso 1 1 calc R . . . .
C7 C 0.451(2) 0.9427(7) 0.8594(11) 0.151(7) Uani 1 1 d . . . . .
H7 H 0.391292 0.971627 0.835360 0.181 Uiso 1 1 calc R . . . .
C40 C 0.0576(15) 0.6833(4) 0.5275(8) 0.114(4) Uani 1 1 d . . . . .
H40A H -0.042409 0.667481 0.490487 0.136 Uiso 1 1 calc R . . . .
H40B H 0.107032 0.662836 0.577312 0.136 Uiso 1 1 calc R . . . .
C32 C 0.4202(16) 0.8446(4) 0.5742(8) 0.116(4) Uani 1 1 d . . . . .
C31 C 0.5287(14) 0.8670(5) 0.6309(8) 0.119(4) 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
Fe1 0.0598(7) 0.0971(10) 0.0653(7) -0.0006(6) 0.0180(5) -0.0058(6)
C19 0.049(3) 0.071(5) 0.067(4) 0.007(3) 0.014(3) 0.001(3)
C25 0.048(3) 0.084(5) 0.062(4) -0.003(4) 0.014(3) -0.004(3)
C30 0.046(3) 0.085(5) 0.061(4) -0.003(4) 0.011(3) -0.001(3)
C18 0.057(4) 0.094(6) 0.059(4) 0.001(4) 0.006(3) -0.015(4)
C24 0.054(4) 0.081(5) 0.062(4) -0.001(4) 0.019(3) -0.002(3)
C12 0.054(4) 0.092(6) 0.059(4) -0.005(4) 0.021(3) -0.004(3)
C34 0.073(5) 0.085(6) 0.059(4) 0.008(4) 0.020(4) -0.011(4)
C33 0.053(4) 0.101(6) 0.047(4) -0.003(4) 0.012(3) -0.014(4)
C13 0.048(3) 0.076(5) 0.068(4) -0.001(4) 0.009(3) -0.003(3)
C26 0.052(4) 0.097(6) 0.054(4) 0.001(4) 0.011(3) -0.004(4)
C11 0.050(3) 0.078(5) 0.056(4) 0.000(3) 0.019(3) 0.001(3)
C20 0.066(4) 0.076(5) 0.062(4) 0.001(4) 0.015(3) -0.003(4)
C38 0.053(4) 0.121(7) 0.052(4) 0.007(4) 0.016(3) 0.003(4)
C23 0.054(4) 0.091(6) 0.078(5) 0.004(4) 0.029(4) 0.004(4)
C45 0.055(4) 0.103(7) 0.061(4) 0.002(4) 0.019(3) -0.002(4)
C21 0.058(4) 0.087(6) 0.064(4) 0.007(4) -0.004(4) -0.002(4)
C29 0.060(4) 0.093(6) 0.065(4) -0.006(4) 0.011(4) -0.006(4)
C35 0.063(4) 0.110(7) 0.059(4) 0.010(4) 0.009(4) -0.006(4)
C22 0.050(4) 0.082(5) 0.089(6) 0.004(4) 0.012(4) -0.005(3)
C14 0.052(4) 0.081(5) 0.090(6) -0.003(4) 0.008(4) -0.009(4)
C27 0.065(4) 0.078(6) 0.077(5) 0.007(4) 0.000(4) -0.010(4)
C44 0.073(5) 0.088(6) 0.067(5) 0.007(4) 0.025(4) 0.009(4)
C1 0.072(5) 0.139(9) 0.055(5) -0.023(5) 0.017(4) -0.028(5)
C46 0.062(4) 0.112(7) 0.068(5) 0.023(5) 0.019(4) 0.004(4)
C42 0.059(4) 0.113(8) 0.080(6) -0.003(5) 0.022(4) -0.017(4)
C17 0.078(5) 0.105(7) 0.065(5) 0.002(4) 0.009(4) -0.016(5)
C41 0.085(6) 0.078(6) 0.081(6) 0.010(4) 0.027(5) -0.005(4)
C43 0.050(4) 0.101(7) 0.072(5) 0.005(4) 0.013(4) 0.001(4)
C28 0.070(4) 0.092(6) 0.059(4) -0.002(4) 0.012(4) -0.004(4)
C36 0.065(4) 0.122(8) 0.053(4) -0.009(4) 0.016(4) -0.015(5)
C15 0.065(5) 0.088(6) 0.094(7) 0.012(5) -0.011(5) -0.003(4)
C37 0.067(5) 0.107(7) 0.065(5) -0.006(4) 0.025(4) 0.000(4)
C5 0.088(6) 0.116(8) 0.089(6) 0.028(6) 0.036(5) 0.005(6)
C3 0.051(4) 0.157(10) 0.087(6) -0.024(7) 0.027(4) -0.012(5)
C16 0.084(6) 0.095(7) 0.085(6) 0.018(5) -0.011(5) -0.012(5)
C2 0.089(6) 0.102(7) 0.096(7) -0.014(5) 0.038(5) -0.005(5)
C9 0.113(8) 0.153(11) 0.051(5) 0.007(6) 0.032(5) 0.021(8)
C4 0.111(8) 0.116(9) 0.097(7) -0.019(6) 0.053(7) -0.038(7)
C48 0.100(7) 0.086(7) 0.095(7) 0.013(5) 0.016(5) 0.009(5)
C47 0.099(7) 0.096(7) 0.100(7) 0.007(5) 0.036(5) 0.010(5)
C8 0.174(12) 0.085(8) 0.121(9) -0.011(7) 0.097(10) -0.001(8)
C39 0.106(7) 0.090(7) 0.118(8) -0.010(6) 0.041(6) 0.008(5)
C10 0.217(16) 0.093(8) 0.139(11) -0.026(8) 0.108(12) -0.062(10)
C6 0.051(5) 0.51(4) 0.069(7) -0.065(14) 0.027(5) -0.091(12)
C7 0.127(11) 0.232(18) 0.123(11) 0.095(11) 0.088(9) 0.104(12)
C40 0.130(9) 0.086(7) 0.140(10) -0.005(6) 0.061(8) -0.009(6)
C32 0.113(8) 0.135(10) 0.092(7) 0.015(7) 0.008(7) 0.000(7)
C31 0.089(7) 0.159(11) 0.100(8) -0.015(7) 0.005(6) -0.011(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
Fe1 C1 2.025(8) . ?
Fe1 C5 2.039(9) . ?
Fe1 C3 2.035(8) . ?
Fe1 C2 2.015(9) . ?
Fe1 C9 2.015(8) . ?
Fe1 C4 2.039(9) . ?
Fe1 C8 2.039(10) . ?
Fe1 C10 2.013(10) . ?
Fe1 C6 2.003(10) . ?
Fe1 C7 2.015(11) . ?
C19 C24 1.369(10) . ?
C19 C11 1.522(9) . ?
C19 C20 1.397(10) . ?
C25 C30 1.408(9) . ?
C25 C26 1.394(10) . ?
C25 C11 1.485(10) . ?
C30 C12 1.514(10) . ?
C30 C29 1.378(10) . ?
C18 C12 1.527(11) . ?
C18 C13 1.394(11) . ?
C18 C17 1.372(11) . ?
C24 C12 1.544(10) . ?
C24 C23 1.380(10) . ?
C12 H12 0.9800 . ?
C34 C33 1.399(11) . ?
C34 C35 1.380(11) . ?
C34 C48 1.486(12) . ?
C33 C38 1.369(11) . ?
C33 C32 1.399(14) . ?
C13 C11 1.505(10) . ?
C13 C14 1.390(10) . ?
C26 H26 0.9300 . ?
C26 C27 1.379(11) . ?
C11 H11 0.9800 . ?
C20 H20 0.9300 . ?
C20 C21 1.400(10) . ?
C38 H38 0.9300 . ?
C38 C37 1.383(11) . ?
C23 H23 0.9300 . ?
C23 C22 1.401(11) . ?
C45 H45 0.9300 . ?
C45 C44 1.388(11) . ?
C45 C46 1.395(12) . ?
C21 H21 0.9300 . ?
C21 C22 1.358(11) . ?
C29 H29 0.9300 . ?
C29 C28 1.393(11) . ?
C35 H35 0.9300 . ?
C35 C36 1.379(12) . ?
C22 H22 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.402(12) . ?
C27 H27 0.9300 . ?
C27 C28 1.374(11) . ?
C44 C43 1.367(11) . ?
C44 C47 1.517(12) . ?
C1 C5 1.418(14) . ?
C1 C2 1.431(13) . ?
C1 C31 1.406(13) . ?
C46 H46 0.9300 . ?
C46 C41 1.366(12) . ?
C42 H42 0.9300 . ?
C42 C41 1.391(12) . ?
C42 C43 1.361(12) . ?
C17 H17 0.9300 . ?
C17 C16 1.383(13) . ?
C41 C40 1.494(13) . ?
C43 H43 0.9300 . ?
C28 H28 0.9300 . ?
C36 H36 0.9300 . ?
C36 C37 1.375(12) . ?
C15 H15 0.9300 . ?
C15 C16 1.378(13) . ?
C37 C39 1.517(13) . ?
C5 H5 0.9300 . ?
C5 C4 1.376(14) . ?
C3 H3 0.9300 . ?
C3 C2 1.386(13) . ?
C3 C4 1.384(14) . ?
C16 H16 0.9300 . ?
C2 H2 0.9300 . ?
C9 H9 0.9300 . ?
C9 C8 1.296(15) . ?
C9 C10 1.307(16) . ?
C4 H4 0.9300 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C48 C47 1.571(12) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C8 H8 0.9800 . ?
C8 C7 1.310(19) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.568(13) . ?
C10 H10 0.9300 . ?
C10 C6 1.39(2) . ?
C6 H6 0.9800 . ?
C6 C7 1.45(2) . ?
C7 H7 0.9800 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C32 C31 1.244(15) . ?
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 C5 40.8(4) . . ?
C1 Fe1 C3 68.0(4) . . ?
C1 Fe1 C4 67.6(4) . . ?
C1 Fe1 C8 167.5(6) . . ?
C5 Fe1 C4 39.4(4) . . ?
C3 Fe1 C5 67.1(4) . . ?
C3 Fe1 C4 39.7(4) . . ?
C3 Fe1 C8 118.4(5) . . ?
C2 Fe1 C1 41.5(4) . . ?
C2 Fe1 C5 68.6(4) . . ?
C2 Fe1 C3 40.0(4) . . ?
C2 Fe1 C4 67.5(5) . . ?
C2 Fe1 C8 150.1(6) . . ?
C2 Fe1 C7 171.2(7) . . ?
C9 Fe1 C1 153.6(5) . . ?
C9 Fe1 C5 164.9(5) . . ?
C9 Fe1 C3 110.6(5) . . ?
C9 Fe1 C2 120.0(5) . . ?
C9 Fe1 C4 129.4(5) . . ?
C9 Fe1 C8 37.3(4) . . ?
C9 Fe1 C7 64.2(5) . . ?
C8 Fe1 C5 129.4(5) . . ?
C8 Fe1 C4 109.7(5) . . ?
C10 Fe1 C1 121.6(5) . . ?
C10 Fe1 C5 154.6(6) . . ?
C10 Fe1 C3 130.1(7) . . ?
C10 Fe1 C2 111.1(5) . . ?
C10 Fe1 C9 37.9(5) . . ?
C10 Fe1 C4 165.6(7) . . ?
C10 Fe1 C8 63.9(5) . . ?
C10 Fe1 C7 67.0(6) . . ?
C6 Fe1 C1 109.5(4) . . ?
C6 Fe1 C5 119.1(7) . . ?
C6 Fe1 C3 168.3(10) . . ?
C6 Fe1 C2 130.6(8) . . ?
C6 Fe1 C9 66.2(5) . . ?
C6 Fe1 C4 151.1(10) . . ?
C6 Fe1 C8 66.6(6) . . ?
C6 Fe1 C10 40.6(7) . . ?
C6 Fe1 C7 42.3(7) . . ?
C7 Fe1 C1 131.4(6) . . ?
C7 Fe1 C5 109.2(4) . . ?
C7 Fe1 C3 147.9(8) . . ?
C7 Fe1 C4 116.7(7) . . ?
C7 Fe1 C8 37.7(6) . . ?
C24 C19 C11 113.4(6) . . ?
C24 C19 C20 120.3(7) . . ?
C20 C19 C11 126.3(7) . . ?
C30 C25 C11 112.1(6) . . ?
C26 C25 C30 119.0(7) . . ?
C26 C25 C11 128.9(7) . . ?
C25 C30 C12 113.5(7) . . ?
C29 C30 C25 120.4(7) . . ?
C29 C30 C12 126.0(7) . . ?
C13 C18 C12 112.6(6) . . ?
C17 C18 C12 127.3(8) . . ?
C17 C18 C13 120.0(8) . . ?
C19 C24 C12 112.8(6) . . ?
C19 C24 C23 121.4(7) . . ?
C23 C24 C12 125.8(7) . . ?
C30 C12 C18 105.8(6) . . ?
C30 C12 C24 105.1(6) . . ?
C30 C12 H12 113.4 . . ?
C18 C12 C24 104.9(6) . . ?
C18 C12 H12 113.4 . . ?
C24 C12 H12 113.4 . . ?
C33 C34 C48 122.1(8) . . ?
C35 C34 C33 115.9(8) . . ?
C35 C34 C48 121.1(8) . . ?
C34 C33 C32 121.0(9) . . ?
C38 C33 C34 120.1(7) . . ?
C38 C33 C32 118.6(8) . . ?
C18 C13 C11 113.0(6) . . ?
C14 C13 C18 119.7(8) . . ?
C14 C13 C11 127.4(7) . . ?
C25 C26 H26 120.2 . . ?
C27 C26 C25 119.7(7) . . ?
C27 C26 H26 120.2 . . ?
C19 C11 H11 112.3 . . ?
C25 C11 C19 106.1(6) . . ?
C25 C11 C13 107.2(6) . . ?
C25 C11 H11 112.3 . . ?
C13 C11 C19 106.1(6) . . ?
C13 C11 H11 112.3 . . ?
C19 C20 H20 120.9 . . ?
C19 C20 C21 118.2(7) . . ?
C21 C20 H20 120.9 . . ?
C33 C38 H38 118.9 . . ?
C33 C38 C37 122.2(7) . . ?
C37 C38 H38 118.9 . . ?
C24 C23 H23 120.8 . . ?
C24 C23 C22 118.3(7) . . ?
C22 C23 H23 120.8 . . ?
C44 C45 H45 120.6 . . ?
C44 C45 C46 118.8(8) . . ?
C46 C45 H45 120.6 . . ?
C20 C21 H21 119.5 . . ?
C22 C21 C20 120.9(7) . . ?
C22 C21 H21 119.5 . . ?
C30 C29 H29 120.0 . . ?
C30 C29 C28 119.9(8) . . ?
C28 C29 H29 120.0 . . ?
C34 C35 H35 119.4 . . ?
C36 C35 C34 121.1(8) . . ?
C36 C35 H35 119.4 . . ?
C23 C22 H22 119.7 . . ?
C21 C22 C23 120.7(7) . . ?
C21 C22 H22 119.7 . . ?
C13 C14 H14 120.4 . . ?
C13 C14 C15 119.2(9) . . ?
C15 C14 H14 120.4 . . ?
C26 C27 H27 119.3 . . ?
C28 C27 C26 121.4(8) . . ?
C28 C27 H27 119.3 . . ?
C45 C44 C47 119.4(8) . . ?
C43 C44 C45 118.0(8) . . ?
C43 C44 C47 121.5(8) . . ?
C5 C1 Fe1 70.1(5) . . ?
C5 C1 C2 106.7(8) . . ?
C2 C1 Fe1 68.9(5) . . ?
C31 C1 Fe1 124.2(7) . . ?
C31 C1 C5 126.2(11) . . ?
C31 C1 C2 127.2(11) . . ?
C45 C46 H46 119.5 . . ?
C41 C46 C45 121.0(8) . . ?
C41 C46 H46 119.5 . . ?
C41 C42 H42 119.7 . . ?
C43 C42 H42 119.7 . . ?
C43 C42 C41 120.7(8) . . ?
C18 C17 H17 119.4 . . ?
C18 C17 C16 121.2(9) . . ?
C16 C17 H17 119.4 . . ?
C46 C41 C42 116.9(8) . . ?
C46 C41 C40 122.0(9) . . ?
C42 C41 C40 120.1(9) . . ?
C44 C43 H43 119.6 . . ?
C42 C43 C44 120.7(8) . . ?
C42 C43 H43 119.6 . . ?
C29 C28 H28 120.2 . . ?
C27 C28 C29 119.6(8) . . ?
C27 C28 H28 120.2 . . ?
C35 C36 H36 119.4 . . ?
C37 C36 C35 121.3(8) . . ?
C37 C36 H36 119.4 . . ?
C14 C15 H15 119.6 . . ?
C16 C15 C14 120.9(9) . . ?
C16 C15 H15 119.6 . . ?
C38 C37 C39 120.4(8) . . ?
C36 C37 C38 115.7(9) . . ?
C36 C37 C39 122.6(8) . . ?
Fe1 C5 H5 126.2 . . ?
C1 C5 Fe1 69.1(5) . . ?
C1 C5 H5 126.0 . . ?
C4 C5 Fe1 70.3(6) . . ?
C4 C5 C1 107.9(9) . . ?
C4 C5 H5 126.0 . . ?
Fe1 C3 H3 126.5 . . ?
C2 C3 Fe1 69.2(5) . . ?
C2 C3 H3 125.6 . . ?
C4 C3 Fe1 70.3(5) . . ?
C4 C3 H3 125.6 . . ?
C4 C3 C2 108.8(9) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 C17 119.1(9) . . ?
C15 C16 H16 120.5 . . ?
Fe1 C2 H2 124.9 . . ?
C1 C2 Fe1 69.6(5) . . ?
C1 C2 H2 126.3 . . ?
C3 C2 Fe1 70.8(5) . . ?
C3 C2 C1 107.4(9) . . ?
C3 C2 H2 126.3 . . ?
Fe1 C9 H9 123.7 . . ?
C8 C9 Fe1 72.4(6) . . ?
C8 C9 H9 124.5 . . ?
C8 C9 C10 110.9(13) . . ?
C10 C9 Fe1 71.0(6) . . ?
C10 C9 H9 124.5 . . ?
Fe1 C4 H4 126.0 . . ?
C5 C4 Fe1 70.3(5) . . ?
C5 C4 C3 109.2(10) . . ?
C5 C4 H4 125.4 . . ?
C3 C4 Fe1 70.0(5) . . ?
C3 C4 H4 125.4 . . ?
C34 C48 H48A 109.0 . . ?
C34 C48 H48B 109.0 . . ?
C34 C48 C47 112.9(8) . . ?
H48A C48 H48B 107.8 . . ?
C47 C48 H48A 109.0 . . ?
C47 C48 H48B 109.0 . . ?
C44 C47 C48 112.2(8) . . ?
C44 C47 H47A 109.2 . . ?
C44 C47 H47B 109.2 . . ?
C48 C47 H47A 109.2 . . ?
C48 C47 H47B 109.2 . . ?
H47A C47 H47B 107.9 . . ?
Fe1 C8 H8 124.7 . . ?
C9 C8 Fe1 70.4(6) . . ?
C9 C8 H8 124.7 . . ?
C9 C8 C7 110.5(13) . . ?
C7 C8 Fe1 70.2(7) . . ?
C7 C8 H8 124.7 . . ?
C37 C39 H39A 109.4 . . ?
C37 C39 H39B 109.4 . . ?
C37 C39 C40 111.3(8) . . ?
H39A C39 H39B 108.0 . . ?
C40 C39 H39A 109.4 . . ?
C40 C39 H39B 109.4 . . ?
Fe1 C10 H10 125.5 . . ?
C9 C10 Fe1 71.2(6) . . ?
C9 C10 H10 125.7 . . ?
C9 C10 C6 108.7(13) . . ?
C6 C10 Fe1 69.3(7) . . ?
C6 C10 H10 125.7 . . ?
Fe1 C6 H6 128.4 . . ?
C10 C6 Fe1 70.1(6) . . ?
C10 C6 H6 128.4 . . ?
C10 C6 C7 102.9(9) . . ?
C7 C6 Fe1 69.3(7) . . ?
C7 C6 H6 128.4 . . ?
Fe1 C7 H7 126.5 . . ?
C8 C7 Fe1 72.1(6) . . ?
C8 C7 C6 107.0(13) . . ?
C8 C7 H7 126.5 . . ?
C6 C7 Fe1 68.4(7) . . ?
C6 C7 H7 126.5 . . ?
C41 C40 C39 114.0(8) . . ?
C41 C40 H40A 108.8 . . ?
C41 C40 H40B 108.8 . . ?
C39 C40 H40A 108.8 . . ?
C39 C40 H40B 108.8 . . ?
H40A C40 H40B 107.7 . . ?
C31 C32 C33 178.3(14) . . ?
C32 C31 C1 177.2(13) . . ?
_shelx_res_file
;
TITL smm743a_a.res in P2(1)/c
smm743a.res
created by SHELXL-2018/3 at 14:07:56 on 26-Oct-2019
REM Old TITL smm743a_a.res in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.239, Rweak 0.064, Alpha 0.086, Orientation as input
REM Formula found by SHELXT: C49 Fe
CELL 1.54184 7.95 28.5068 15.5007 90 104.262 90
ZERR 4 0.0004 0.0021 0.0008 0 0.005 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Fe
UNIT 192 152 4
L.S. 40
PLAN 20
SIZE 0.4 0.34 0.32
BOND $H
list 4
fmap 2
acta 52
OMIT 0 2 0
OMIT -1 3 1
OMIT -3 9 5
OMIT 0 2 1
OMIT -2 1 3
OMIT 5 2 7
OMIT 0 1 8
OMIT 4 0 8
OMIT 0 1 1
OMIT 0 4 4
REM
REM
REM
WGHT 0.168300 5.113300
FVAR 0.29050
FE1 3 0.640049 0.910067 0.816063 11.00000 0.05981 0.09710 =
0.06527 -0.00061 0.01803 -0.00578
C19 1 0.382669 0.581387 0.663364 11.00000 0.04941 0.07071 =
0.06722 0.00665 0.01427 0.00070
C25 1 0.593523 0.641913 0.715619 11.00000 0.04784 0.08442 =
0.06228 -0.00280 0.01411 -0.00375
C30 1 0.502447 0.654877 0.779144 11.00000 0.04636 0.08474 =
0.06073 -0.00316 0.01140 -0.00107
C18 1 0.549277 0.577176 0.844320 11.00000 0.05661 0.09446 =
0.05875 0.00061 0.00581 -0.01518
C24 1 0.292794 0.593133 0.725034 11.00000 0.05391 0.08104 =
0.06165 -0.00095 0.01949 -0.00199
C12 1 0.410082 0.614303 0.810617 11.00000 0.05410 0.09191 =
0.05866 -0.00545 0.02101 -0.00398
AFIX 13
H12 2 0.346657 0.623366 0.854808 11.00000 -1.20000
AFIX 0
C34 1 0.150070 0.839126 0.459293 11.00000 0.07315 0.08469 =
0.05927 0.00799 0.01997 -0.01120
C33 1 0.301991 0.818602 0.510328 11.00000 0.05316 0.10055 =
0.04735 -0.00271 0.01237 -0.01373
C13 1 0.638576 0.564856 0.780707 11.00000 0.04845 0.07637 =
0.06820 -0.00063 0.00879 -0.00258
C26 1 0.680700 0.676392 0.679884 11.00000 0.05205 0.09716 =
0.05402 0.00113 0.01084 -0.00427
AFIX 43
H26 2 0.742193 0.668432 0.638146 11.00000 -1.20000
AFIX 0
C11 1 0.576423 0.591057 0.694437 11.00000 0.05001 0.07787 =
0.05556 0.00033 0.01869 0.00127
AFIX 13
H11 2 0.639156 0.581919 0.649996 11.00000 -1.20000
AFIX 0
C20 1 0.295425 0.563568 0.580492 11.00000 0.06626 0.07575 =
0.06188 0.00072 0.01450 -0.00286
AFIX 43
H20 2 0.355011 0.556363 0.537554 11.00000 -1.20000
AFIX 0
C38 1 0.327568 0.771263 0.505576 11.00000 0.05284 0.12113 =
0.05204 0.00744 0.01647 0.00265
AFIX 43
H38 2 0.427642 0.758051 0.541345 11.00000 -1.20000
AFIX 0
C23 1 0.115540 0.586847 0.708259 11.00000 0.05441 0.09072 =
0.07845 0.00352 0.02882 0.00415
AFIX 43
H23 2 0.055127 0.595567 0.750029 11.00000 -1.20000
AFIX 0
C45 1 0.080826 0.798946 0.644557 11.00000 0.05536 0.10256 =
0.06104 0.00243 0.01856 -0.00183
AFIX 43
H45 2 0.149983 0.814530 0.693253 11.00000 -1.20000
AFIX 0
C21 1 0.115814 0.556844 0.563794 11.00000 0.05813 0.08692 =
0.06413 0.00686 -0.00415 -0.00205
AFIX 43
H21 2 0.055171 0.545258 0.508834 11.00000 -1.20000
AFIX 0
C29 1 0.495330 0.701178 0.803442 11.00000 0.06013 0.09344 =
0.06483 -0.00631 0.01093 -0.00557
AFIX 43
H29 2 0.431735 0.709696 0.843935 11.00000 -1.20000
AFIX 0
C35 1 0.055971 0.812402 0.389742 11.00000 0.06344 0.10990 =
0.05889 0.01047 0.00864 -0.00580
AFIX 43
H35 2 -0.029252 0.826634 0.345506 11.00000 -1.20000
AFIX 0
C22 1 0.028897 0.566999 0.626714 11.00000 0.05038 0.08153 =
0.08888 0.00428 0.01232 -0.00467
AFIX 43
H22 2 -0.089301 0.560718 0.615565 11.00000 -1.20000
AFIX 0
C14 1 0.768734 0.531143 0.800957 11.00000 0.05227 0.08062 =
0.08961 -0.00276 0.00798 -0.00938
AFIX 43
H14 2 0.830024 0.522888 0.759295 11.00000 -1.20000
AFIX 0
C27 1 0.675322 0.722371 0.706725 11.00000 0.06469 0.07834 =
0.07661 0.00741 0.00029 -0.00988
AFIX 43
H27 2 0.735143 0.745160 0.683316 11.00000 -1.20000
AFIX 0
C44 1 -0.041712 0.823261 0.580998 11.00000 0.07337 0.08751 =
0.06689 0.00650 0.02523 0.00939
C1 1 0.656976 0.892110 0.692058 11.00000 0.07210 0.13863 =
0.05541 -0.02294 0.01716 -0.02811
C46 1 0.098432 0.750719 0.634113 11.00000 0.06194 0.11177 =
0.06822 0.02326 0.01930 0.00419
AFIX 43
H46 2 0.179504 0.734077 0.676589 11.00000 -1.20000
AFIX 0
C42 1 -0.147733 0.750951 0.513489 11.00000 0.05853 0.11278 =
0.07955 -0.00290 0.02184 -0.01739
AFIX 43
H42 2 -0.233191 0.734310 0.473390 11.00000 -1.20000
AFIX 0
C17 1 0.588231 0.555581 0.925953 11.00000 0.07817 0.10529 =
0.06520 0.00236 0.00868 -0.01646
AFIX 43
H17 2 0.526927 0.563749 0.967659 11.00000 -1.20000
AFIX 0
C41 1 -0.001575 0.727579 0.562467 11.00000 0.08525 0.07786 =
0.08119 0.00951 0.02716 -0.00459
C43 1 -0.166940 0.797907 0.523650 11.00000 0.04984 0.10095 =
0.07212 0.00455 0.01329 0.00103
AFIX 43
H43 2 -0.266382 0.812911 0.491210 11.00000 -1.20000
AFIX 0
C28 1 0.583483 0.735225 0.767302 11.00000 0.06957 0.09189 =
0.05942 -0.00206 0.01161 -0.00353
AFIX 43
H28 2 0.580177 0.766467 0.784084 11.00000 -1.20000
AFIX 0
C36 1 0.086144 0.764956 0.384709 11.00000 0.06453 0.12224 =
0.05331 -0.00941 0.01609 -0.01521
AFIX 43
H36 2 0.021894 0.747851 0.336714 11.00000 -1.20000
AFIX 0
C15 1 0.806445 0.509740 0.885002 11.00000 0.06534 0.08762 =
0.09438 0.01194 -0.01109 -0.00308
AFIX 43
H15 2 0.892965 0.487047 0.898834 11.00000 -1.20000
AFIX 0
C37 1 0.209455 0.742458 0.449327 11.00000 0.06651 0.10654 =
0.06542 -0.00552 0.02491 0.00022
C5 1 0.666331 0.941572 0.701994 11.00000 0.08848 0.11603 =
0.08917 0.02780 0.03587 0.00473
AFIX 43
H5 2 0.590308 0.963202 0.668112 11.00000 -1.20000
AFIX 0
C3 1 0.889604 0.910611 0.804558 11.00000 0.05149 0.15706 =
0.08741 -0.02429 0.02693 -0.01228
AFIX 43
H3 2 0.989130 0.908371 0.850827 11.00000 -1.20000
AFIX 0
C16 1 0.716979 0.521894 0.947345 11.00000 0.08428 0.09482 =
0.08536 0.01827 -0.01062 -0.01207
AFIX 43
H16 2 0.742810 0.507644 1.003031 11.00000 -1.20000
AFIX 0
C2 1 0.798845 0.873159 0.758246 11.00000 0.08926 0.10164 =
0.09622 -0.01416 0.03781 -0.00508
AFIX 43
H2 2 0.825290 0.841540 0.768336 11.00000 -1.20000
AFIX 0
C9 1 0.631703 0.895751 0.942243 11.00000 0.11303 0.15322 =
0.05092 0.00660 0.03249 0.02071
AFIX 43
H9 2 0.727090 0.885621 0.985988 11.00000 -1.20000
AFIX 0
C4 1 0.807814 0.951902 0.770647 11.00000 0.11129 0.11603 =
0.09737 -0.01883 0.05317 -0.03752
AFIX 43
H4 2 0.842915 0.981887 0.791031 11.00000 -1.20000
AFIX 0
C48 1 0.077102 0.882912 0.487354 11.00000 0.10048 0.08646 =
0.09515 0.01329 0.01631 0.00870
AFIX 23
H48A 2 -0.006744 0.895970 0.436732 11.00000 -1.20000
H48B 2 0.169780 0.905627 0.506045 11.00000 -1.20000
AFIX 0
C47 1 -0.013455 0.874883 0.565510 11.00000 0.09921 0.09553 =
0.09951 0.00712 0.03629 0.01029
AFIX 23
H47A 2 0.057734 0.888482 0.619653 11.00000 -1.20000
H47B 2 -0.124561 0.890882 0.551823 11.00000 -1.20000
AFIX 0
C8 1 0.587858 0.939302 0.926669 11.00000 0.17417 0.08545 =
0.12086 -0.01144 0.09685 -0.00099
AFIX 13
H8 2 0.650438 0.966034 0.959327 11.00000 -1.20000
AFIX 0
C39 1 0.195454 0.691035 0.471834 11.00000 0.10631 0.08973 =
0.11803 -0.01044 0.04096 0.00805
AFIX 23
H39A 2 0.307666 0.679846 0.505544 11.00000 -1.20000
H39B 2 0.162686 0.672961 0.417238 11.00000 -1.20000
AFIX 0
C10 1 0.523977 0.867982 0.888268 11.00000 0.21688 0.09316 =
0.13885 -0.02565 0.10771 -0.06163
AFIX 43
H10 2 0.528209 0.835378 0.888830 11.00000 -1.20000
AFIX 0
C6 1 0.401671 0.895332 0.829712 11.00000 0.05055 0.51443 =
0.06946 -0.06465 0.02713 -0.09075
AFIX 13
H6 2 0.299875 0.884990 0.784063 11.00000 -1.20000
AFIX 0
C7 1 0.451344 0.942671 0.859391 11.00000 0.12718 0.23202 =
0.12279 0.09514 0.08773 0.10395
AFIX 13
H7 2 0.391292 0.971627 0.835360 11.00000 -1.20000
AFIX 0
C40 1 0.057647 0.683307 0.527528 11.00000 0.12950 0.08624 =
0.13989 -0.00471 0.06070 -0.00883
AFIX 23
H40A 2 -0.042409 0.667481 0.490487 11.00000 -1.20000
H40B 2 0.107032 0.662836 0.577312 11.00000 -1.20000
AFIX 0
C32 1 0.420226 0.844635 0.574244 11.00000 0.11260 0.13539 =
0.09206 0.01514 0.00832 -0.00041
C31 1 0.528742 0.866969 0.630860 11.00000 0.08874 0.15906 =
0.09980 -0.01468 0.00472 -0.01126
HKLF 4
REM smm743a_a.res in P2(1)/c
REM wR2 = 0.3614, GooF = S = 1.027, Restrained GooF = 1.027 for all data
REM R1 = 0.1158 for 3490 Fo > 4sig(Fo) and 0.1747 for all 6536 data
REM 442 parameters refined using 0 restraints
END
WGHT 0.1679 5.1549
REM Highest difference peak 1.031, deepest hole -0.592, 1-sigma level 0.079
Q1 1 0.2914 0.8473 0.7631 11.00000 0.05 1.03
Q2 1 0.2052 0.8283 0.7129 11.00000 0.05 1.01
Q3 1 0.6701 0.9087 0.7684 11.00000 0.05 0.46
Q4 1 0.4489 0.8692 0.8217 11.00000 0.05 0.34
Q5 1 0.6235 0.8677 0.8804 11.00000 0.05 0.33
Q6 1 0.3902 0.9223 0.8086 11.00000 0.05 0.33
Q7 1 0.5389 0.8606 0.7643 11.00000 0.05 0.28
Q8 1 0.1480 0.6133 0.5934 11.00000 0.05 0.28
Q9 1 0.7414 0.9510 0.8809 11.00000 0.05 0.28
Q10 1 0.6430 0.8670 0.8188 11.00000 0.05 0.26
Q11 1 0.6802 0.8306 0.8185 11.00000 0.05 0.25
Q12 1 0.5110 0.9526 0.7536 11.00000 0.05 0.25
Q13 1 -0.2276 0.7201 0.4480 11.00000 0.05 0.25
Q14 1 0.6074 0.5629 0.5721 11.00000 0.05 0.23
Q15 1 0.6094 0.9307 0.9406 11.00000 0.05 0.23
Q16 1 0.1768 0.7618 0.3797 11.00000 0.05 0.23
Q17 1 0.5081 0.9175 0.6818 11.00000 0.05 0.22
Q18 1 0.6441 0.9615 0.8177 11.00000 0.05 0.22
Q19 1 0.6551 0.9367 0.8917 11.00000 0.05 0.21
Q20 1 0.6812 0.8182 0.9427 11.00000 0.05 0.21
;
_shelx_res_checksum 52529
_olex2_submission_special_instructions 'No special instructions were received'