# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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.
#
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data_exp_2079
_database_code_depnum_ccdc_archive 'CCDC 1952454'
loop_
_audit_author_name
_audit_author_address
'Marta Feliz'
;Instituto de Tecnologia Quimica
Spain
;
_audit_update_record
;
2019-09-09 deposited with the CCDC. 2020-03-20 downloaded from the CCDC.
;
_audit_creation_date 2019-08-22
_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 trans-[FeCl2{(R,R)-Me-DuPhos}2]
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H56 Cl2 Fe P4'
_chemical_formula_sum 'C36 H56 Cl2 Fe P4'
_chemical_formula_weight 739.43
_chemical_absolute_configuration rm
_chemical_melting_point ?
_chemical_oxdiff_formula ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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 tetragonal
_space_group_IT_number 92
_space_group_name_H-M_alt 'P 41 21 2'
_space_group_name_Hall 'P 4abw 2nw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x+1/2, z+1/4'
'-x, -y, z+1/2'
'y+1/2, -x+1/2, z+3/4'
'x+1/2, -y+1/2, -z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'
_cell_length_a 11.05922(16)
_cell_length_b 11.05922(16)
_cell_length_c 30.7432(7)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3760.09(14)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 8041
_cell_measurement_temperature 180.00(10)
_cell_measurement_theta_max 27.3840
_cell_measurement_theta_min 3.6950
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.738
_exptl_absorpt_correction_T_max 0.977
_exptl_absorpt_correction_T_min 0.956
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb 1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour orange
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.306
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1568
_exptl_crystal_size_max 0.2219
_exptl_crystal_size_mid 0.1503
_exptl_crystal_size_min 0.0949
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0326
_diffrn_reflns_av_unetI/netI 0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 37
_diffrn_reflns_limit_l_min -37
_diffrn_reflns_number 14568
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.608
_diffrn_reflns_theta_min 2.923
_diffrn_ambient_temperature 180.00(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 0.0302183000
_diffrn_orient_matrix_UB_12 0.0540682000
_diffrn_orient_matrix_UB_13 0.0059645000
_diffrn_orient_matrix_UB_21 0.0560033000
_diffrn_orient_matrix_UB_22 -0.0312807000
_diffrn_orient_matrix_UB_23 -0.0001279000
_diffrn_orient_matrix_UB_31 0.0077812000
_diffrn_orient_matrix_UB_32 0.0146409000
_diffrn_orient_matrix_UB_33 -0.0222891000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.629
_reflns_Friedel_fraction_full 0.999
_reflns_Friedel_fraction_max 0.857
_reflns_number_gt 3617
_reflns_number_total 3945
_reflns_odcompleteness_completeness 99.44
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 24.66
_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 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb 1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb 1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb 1 2013,16:14:44)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.261
_refine_diff_density_min -0.187
_refine_diff_density_rms 0.046
_refine_ls_abs_structure_details
;
Flack x determined using 1315 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack -0.001(9)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.083
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 199
_refine_ls_number_reflns 3945
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0323
_refine_ls_R_factor_gt 0.0266
_refine_ls_restrained_S_all 1.083
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.1415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0576
_refine_ls_wR_factor_ref 0.0604
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C6(H6), C8(H8), C10(H10), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
C7(H7A,H7B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C12(H12)
2.d Idealised Me refined as rotating group:
C9(H9A,H9B,H9C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.58101(3) 0.58101(3) 0.000000 0.01716(12) Uani 1 2 d S T P . .
P1 P 0.63840(6) 0.74343(6) 0.05781(2) 0.02151(16) Uani 1 1 d . . . . .
P2 P 0.41932(6) 0.54556(6) 0.05930(2) 0.01860(14) Uani 1 1 d . . . . .
Cl1 Cl 0.70387(6) 0.44497(6) 0.04033(2) 0.02766(16) Uani 1 1 d . . . . .
C1 C 0.5609(2) 0.7070(2) 0.10897(7) 0.0206(5) Uani 1 1 d . . . . .
C2 C 0.4693(2) 0.6192(2) 0.11030(7) 0.0207(5) Uani 1 1 d . . . . .
C3 C 0.4164(2) 0.5919(2) 0.15048(7) 0.0261(5) Uani 1 1 d . . . . .
H3 H 0.354828 0.534835 0.151882 0.031 Uiso 1 1 calc R . . . .
C4 C 0.5957(2) 0.7649(2) 0.14773(7) 0.0260(6) Uani 1 1 d . . . . .
H4 H 0.654970 0.824479 0.146840 0.031 Uiso 1 1 calc R . . . .
C5 C 0.5435(3) 0.7351(3) 0.18701(8) 0.0293(6) Uani 1 1 d . . . . .
H5 H 0.568459 0.773240 0.212426 0.035 Uiso 1 1 calc R . . . .
C6 C 0.6284(3) 0.9130(3) 0.05571(8) 0.0357(7) Uani 1 1 d . . . . .
H6 H 0.605743 0.940741 0.084866 0.043 Uiso 1 1 calc R . . . .
C8 C 0.2648(2) 0.6102(3) 0.05044(8) 0.0293(7) Uani 1 1 d . . . . .
H8 H 0.243826 0.593791 0.020031 0.035 Uiso 1 1 calc R . . . .
C7 C 0.2219(3) 0.4034(3) 0.07411(9) 0.0401(8) Uani 1 1 d . . . . .
H7A H 0.198213 0.371758 0.045942 0.048 Uiso 1 1 calc R . . . .
H7B H 0.183653 0.354489 0.096385 0.048 Uiso 1 1 calc R . . . .
C10 C 0.8046(2) 0.7442(3) 0.07117(8) 0.0311(7) Uani 1 1 d . . . . .
H10 H 0.845872 0.715637 0.044906 0.037 Uiso 1 1 calc R . . . .
C9 C 0.4154(3) 0.2865(2) 0.05680(8) 0.0368(7) Uani 1 1 d . . . . .
H9A H 0.399260 0.289995 0.026149 0.055 Uiso 1 1 calc GR . . . .
H9B H 0.380669 0.214189 0.068715 0.055 Uiso 1 1 calc GR . . . .
H9C H 0.501208 0.286074 0.061551 0.055 Uiso 1 1 calc GR . . . .
C12 C 0.4548(3) 0.6490(3) 0.18834(8) 0.0321(6) Uani 1 1 d . . . . .
H12 H 0.419746 0.628440 0.214834 0.038 Uiso 1 1 calc R . . . .
C11 C 0.3602(2) 0.3962(2) 0.07895(8) 0.0262(6) Uani 1 1 d . . . . .
H11 H 0.378377 0.390218 0.110076 0.031 Uiso 1 1 calc R . . . .
C14 C 0.2517(3) 0.7456(3) 0.05683(9) 0.0427(8) Uani 1 1 d . . . . .
H14A H 0.274350 0.766387 0.086031 0.064 Uiso 1 1 calc GR . . . .
H14B H 0.169252 0.768744 0.051823 0.064 Uiso 1 1 calc GR . . . .
H14C H 0.303346 0.787199 0.036681 0.064 Uiso 1 1 calc GR . . . .
C13 C 0.1801(3) 0.5325(3) 0.07826(9) 0.0403(8) Uani 1 1 d . . . . .
H13A H 0.183380 0.558137 0.108412 0.048 Uiso 1 1 calc R . . . .
H13B H 0.097394 0.540313 0.068089 0.048 Uiso 1 1 calc R . . . .
C15 C 0.7595(3) 0.9531(3) 0.04778(9) 0.0469(9) Uani 1 1 d . . . . .
H15A H 0.780738 0.941690 0.017443 0.056 Uiso 1 1 calc R . . . .
H15B H 0.768764 1.038049 0.054867 0.056 Uiso 1 1 calc R . . . .
C16 C 0.8407(3) 0.8773(3) 0.07641(9) 0.0443(8) Uani 1 1 d . . . . .
H16A H 0.831931 0.901731 0.106542 0.053 Uiso 1 1 calc R . . . .
H16B H 0.924478 0.888328 0.067982 0.053 Uiso 1 1 calc R . . . .
C17 C 0.8486(3) 0.6629(3) 0.10804(8) 0.0407(8) Uani 1 1 d . . . . .
H17A H 0.819148 0.693418 0.135294 0.061 Uiso 1 1 calc GR . . . .
H17B H 0.935376 0.662008 0.108379 0.061 Uiso 1 1 calc GR . . . .
H17C H 0.818915 0.582275 0.103644 0.061 Uiso 1 1 calc GR . . . .
C18 C 0.5369(3) 0.9649(3) 0.02422(9) 0.0496(9) Uani 1 1 d . . . . .
H18A H 0.551129 0.932452 -0.004290 0.074 Uiso 1 1 calc GR . . . .
H18B H 0.544824 1.051288 0.023417 0.074 Uiso 1 1 calc GR . . . .
H18C H 0.456835 0.943789 0.033565 0.074 Uiso 1 1 calc GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.01888(16) 0.01888(16) 0.0137(2) 0.00120(13) -0.00120(13) -0.0007(2)
P1 0.0254(4) 0.0211(3) 0.0180(3) -0.0018(3) -0.0009(3) -0.0048(3)
P2 0.0186(3) 0.0213(3) 0.0158(3) 0.0010(2) -0.0002(3) -0.0011(3)
Cl1 0.0281(3) 0.0317(4) 0.0232(3) 0.0036(3) -0.0056(3) 0.0070(3)
C1 0.0229(14) 0.0211(13) 0.0176(11) -0.0013(10) -0.0014(10) 0.0055(11)
C2 0.0209(13) 0.0253(14) 0.0159(11) 0.0015(10) -0.0016(10) 0.0060(10)
C3 0.0283(14) 0.0293(14) 0.0206(12) 0.0005(11) 0.0027(11) 0.0022(12)
C4 0.0245(14) 0.0296(15) 0.0237(12) -0.0068(11) -0.0047(11) 0.0013(11)
C5 0.0350(16) 0.0347(16) 0.0183(12) -0.0082(11) -0.0058(11) 0.0091(13)
C6 0.058(2) 0.0211(14) 0.0283(14) -0.0050(12) 0.0023(14) -0.0075(14)
C8 0.0214(14) 0.0452(18) 0.0214(13) -0.0019(12) -0.0025(11) 0.0040(12)
C7 0.0310(17) 0.060(2) 0.0294(14) 0.0037(14) 0.0031(13) -0.0213(15)
C10 0.0245(14) 0.0434(18) 0.0253(13) -0.0079(12) 0.0021(12) -0.0102(13)
C9 0.0521(19) 0.0258(15) 0.0323(14) 0.0037(12) -0.0005(14) -0.0091(14)
C12 0.0409(17) 0.0405(16) 0.0149(12) 0.0020(11) 0.0038(11) 0.0108(14)
C11 0.0316(15) 0.0270(16) 0.0200(12) 0.0031(11) 0.0013(11) -0.0101(12)
C14 0.0409(19) 0.050(2) 0.0375(15) -0.0006(15) -0.0026(14) 0.0209(15)
C13 0.0199(15) 0.070(2) 0.0313(15) 0.0006(15) 0.0037(12) -0.0007(15)
C15 0.070(2) 0.0324(17) 0.0385(17) -0.0081(14) 0.0103(16) -0.0270(17)
C16 0.044(2) 0.051(2) 0.0378(16) -0.0117(15) 0.0016(15) -0.0257(16)
C17 0.0277(17) 0.059(2) 0.0349(15) -0.0079(14) -0.0085(13) 0.0005(15)
C18 0.079(3) 0.0236(16) 0.0462(17) 0.0037(14) -0.0028(17) 0.0038(16)
_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 P1 2.6055(7) . ?
Fe1 P1 2.6054(7) 7 ?
Fe1 P2 2.5836(7) . ?
Fe1 P2 2.5837(7) 7 ?
Fe1 Cl1 2.3763(6) . ?
Fe1 Cl1 2.3763(6) 7 ?
P1 C1 1.836(2) . ?
P1 C6 1.880(3) . ?
P1 C10 1.883(3) . ?
P2 C2 1.851(2) . ?
P2 C8 1.872(3) . ?
P2 C11 1.877(3) . ?
C1 C2 1.405(3) . ?
C1 C4 1.406(3) . ?
C2 C3 1.399(3) . ?
C3 C12 1.390(3) . ?
C4 C5 1.378(4) . ?
C5 C12 1.368(4) . ?
C6 C15 1.536(4) . ?
C6 C18 1.513(4) . ?
C8 C14 1.517(4) . ?
C8 C13 1.532(4) . ?
C7 C11 1.539(4) . ?
C7 C13 1.506(4) . ?
C10 C16 1.534(4) . ?
C10 C17 1.526(4) . ?
C9 C11 1.519(4) . ?
C15 C16 1.511(5) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Fe1 P1 97.44(3) 7 . ?
P2 Fe1 P1 174.57(2) . 7 ?
P2 Fe1 P1 77.99(2) 7 7 ?
P2 Fe1 P1 174.56(2) 7 . ?
P2 Fe1 P1 77.99(2) . . ?
P2 Fe1 P2 106.73(3) . 7 ?
Cl1 Fe1 P1 86.63(2) . . ?
Cl1 Fe1 P1 96.66(2) . 7 ?
Cl1 Fe1 P1 86.64(2) 7 7 ?
Cl1 Fe1 P1 96.66(2) 7 . ?
Cl1 Fe1 P2 86.07(2) . . ?
Cl1 Fe1 P2 90.96(2) 7 . ?
Cl1 Fe1 P2 86.07(2) 7 7 ?
Cl1 Fe1 P2 90.96(2) . 7 ?
Cl1 Fe1 Cl1 175.03(4) . 7 ?
C1 P1 Fe1 108.64(8) . . ?
C1 P1 C6 102.75(12) . . ?
C1 P1 C10 105.63(11) . . ?
C6 P1 Fe1 130.53(9) . . ?
C6 P1 C10 93.49(13) . . ?
C10 P1 Fe1 112.92(9) . . ?
C2 P2 Fe1 108.93(8) . . ?
C2 P2 C8 103.15(11) . . ?
C2 P2 C11 102.63(11) . . ?
C8 P2 Fe1 118.10(8) . . ?
C8 P2 C11 93.73(12) . . ?
C11 P2 Fe1 127.00(8) . . ?
C2 C1 P1 120.89(17) . . ?
C2 C1 C4 119.2(2) . . ?
C4 C1 P1 119.92(19) . . ?
C1 C2 P2 119.67(17) . . ?
C3 C2 P2 121.9(2) . . ?
C3 C2 C1 118.4(2) . . ?
C12 C3 C2 120.9(3) . . ?
C5 C4 C1 121.3(3) . . ?
C12 C5 C4 119.5(2) . . ?
C15 C6 P1 103.8(2) . . ?
C18 C6 P1 116.1(2) . . ?
C18 C6 C15 114.8(2) . . ?
C14 C8 P2 116.4(2) . . ?
C14 C8 C13 115.0(2) . . ?
C13 C8 P2 105.23(18) . . ?
C13 C7 C11 110.3(2) . . ?
C16 C10 P1 106.3(2) . . ?
C17 C10 P1 118.09(19) . . ?
C17 C10 C16 113.8(2) . . ?
C5 C12 C3 120.6(2) . . ?
C7 C11 P2 105.60(19) . . ?
C9 C11 P2 114.74(18) . . ?
C9 C11 C7 113.5(2) . . ?
C7 C13 C8 107.2(2) . . ?
C16 C15 C6 108.0(2) . . ?
C15 C16 C10 108.5(2) . . ?
_shelx_res_file
;
TITL CF solution in P43212
exp_2079.res
created by SHELXL-2018/3 at 10:34:26 on 22-Aug-2019
CELL 0.71073 11.059219 11.059219 30.743235 90 90 90
ZERR 4 0.000161 0.000161 0.000702 0 0 0
LATT -1
SYMM 0.5-Y,0.5+X,0.25+Z
SYMM -X,-Y,0.5+Z
SYMM 0.5+Y,0.5-X,0.75+Z
SYMM 0.5+X,0.5-Y,0.75-Z
SYMM 0.5-X,0.5+Y,0.25-Z
SYMM +Y,+X,-Z
SYMM -Y,-X,0.5-Z
SFAC C H Cl Fe P
UNIT 144 224 8 4 16
L.S. 15
PLAN 10
BOND
fmap 2
acta
REM
REM
REM
WGHT 0.026700 0.141500
FVAR 1.09016
FE1 4 0.581015 0.581015 0.000000 10.50000 0.01888 0.01888 =
0.01372 0.00120 -0.00120 -0.00072
P1 5 0.638404 0.743434 0.057814 11.00000 0.02544 0.02106 =
0.01803 -0.00184 -0.00090 -0.00480
P2 5 0.419318 0.545559 0.059299 11.00000 0.01864 0.02135 =
0.01582 0.00096 -0.00018 -0.00110
CL1 3 0.703873 0.444972 0.040329 11.00000 0.02812 0.03166 =
0.02320 0.00364 -0.00559 0.00703
C1 1 0.560943 0.707039 0.108974 11.00000 0.02291 0.02115 =
0.01765 -0.00134 -0.00144 0.00552
C2 1 0.469259 0.619211 0.110300 11.00000 0.02089 0.02528 =
0.01587 0.00147 -0.00159 0.00603
C3 1 0.416439 0.591937 0.150485 11.00000 0.02831 0.02935 =
0.02061 0.00050 0.00265 0.00219
AFIX 43
H3 2 0.354828 0.534835 0.151882 11.00000 -1.20000
AFIX 0
C4 1 0.595660 0.764915 0.147725 11.00000 0.02452 0.02963 =
0.02370 -0.00677 -0.00468 0.00129
AFIX 43
H4 2 0.654970 0.824479 0.146840 11.00000 -1.20000
AFIX 0
C5 1 0.543498 0.735092 0.187007 11.00000 0.03502 0.03475 =
0.01826 -0.00815 -0.00580 0.00912
AFIX 43
H5 2 0.568459 0.773240 0.212426 11.00000 -1.20000
AFIX 0
C6 1 0.628370 0.912999 0.055706 11.00000 0.05778 0.02111 =
0.02828 -0.00503 0.00234 -0.00747
AFIX 13
H6 2 0.605743 0.940741 0.084866 11.00000 -1.20000
AFIX 0
C8 1 0.264784 0.610205 0.050435 11.00000 0.02138 0.04518 =
0.02139 -0.00192 -0.00248 0.00405
AFIX 13
H8 2 0.243826 0.593791 0.020031 11.00000 -1.20000
AFIX 0
C7 1 0.221863 0.403448 0.074105 11.00000 0.03098 0.05989 =
0.02938 0.00367 0.00314 -0.02131
AFIX 23
H7A 2 0.198213 0.371758 0.045942 11.00000 -1.20000
H7B 2 0.183653 0.354489 0.096385 11.00000 -1.20000
AFIX 0
C10 1 0.804557 0.744156 0.071175 11.00000 0.02453 0.04340 =
0.02529 -0.00792 0.00206 -0.01019
AFIX 13
H10 2 0.845872 0.715637 0.044906 11.00000 -1.20000
AFIX 0
C9 1 0.415413 0.286520 0.056804 11.00000 0.05210 0.02583 =
0.03234 0.00368 -0.00052 -0.00910
AFIX 137
H9A 2 0.399260 0.289995 0.026149 11.00000 -1.50000
H9B 2 0.380669 0.214189 0.068715 11.00000 -1.50000
H9C 2 0.501208 0.286074 0.061551 11.00000 -1.50000
AFIX 0
C12 1 0.454766 0.648997 0.188344 11.00000 0.04089 0.04046 =
0.01486 0.00197 0.00377 0.01081
AFIX 43
H12 2 0.419746 0.628440 0.214834 11.00000 -1.20000
AFIX 0
C11 1 0.360204 0.396152 0.078950 11.00000 0.03159 0.02700 =
0.02000 0.00309 0.00125 -0.01013
AFIX 13
H11 2 0.378377 0.390218 0.110076 11.00000 -1.20000
AFIX 0
C14 1 0.251736 0.745551 0.056829 11.00000 0.04085 0.04983 =
0.03747 -0.00065 -0.00259 0.02091
AFIX 137
H14A 2 0.274350 0.766387 0.086031 11.00000 -1.50000
H14B 2 0.169252 0.768744 0.051823 11.00000 -1.50000
H14C 2 0.303346 0.787199 0.036681 11.00000 -1.50000
AFIX 0
C13 1 0.180053 0.532507 0.078261 11.00000 0.01991 0.06966 =
0.03130 0.00057 0.00372 -0.00072
AFIX 23
H13A 2 0.183380 0.558137 0.108412 11.00000 -1.20000
H13B 2 0.097394 0.540313 0.068089 11.00000 -1.20000
AFIX 0
C15 1 0.759487 0.953086 0.047779 11.00000 0.06980 0.03245 =
0.03849 -0.00810 0.01035 -0.02703
AFIX 23
H15A 2 0.780738 0.941690 0.017443 11.00000 -1.20000
H15B 2 0.768764 1.038049 0.054867 11.00000 -1.20000
AFIX 0
C16 1 0.840682 0.877253 0.076408 11.00000 0.04379 0.05136 =
0.03784 -0.01172 0.00156 -0.02567
AFIX 23
H16A 2 0.831931 0.901731 0.106542 11.00000 -1.20000
H16B 2 0.924478 0.888328 0.067982 11.00000 -1.20000
AFIX 0
C17 1 0.848581 0.662933 0.108041 11.00000 0.02771 0.05950 =
0.03485 -0.00794 -0.00851 0.00053
AFIX 137
H17A 2 0.819148 0.693418 0.135294 11.00000 -1.50000
H17B 2 0.935376 0.662008 0.108379 11.00000 -1.50000
H17C 2 0.818915 0.582275 0.103644 11.00000 -1.50000
AFIX 0
C18 1 0.536937 0.964870 0.024224 11.00000 0.07893 0.02360 =
0.04625 0.00366 -0.00284 0.00379
AFIX 137
H18A 2 0.551129 0.932452 -0.004290 11.00000 -1.50000
H18B 2 0.544824 1.051288 0.023417 11.00000 -1.50000
H18C 2 0.456835 0.943789 0.033565 11.00000 -1.50000
AFIX 0
HKLF 4
REM CF solution in P43212
REM wR2 = 0.0604, GooF = S = 1.083, Restrained GooF = 1.083 for all data
REM R1 = 0.0266 for 3617 Fo > 4sig(Fo) and 0.0323 for all 3945 data
REM 199 parameters refined using 0 restraints
END
WGHT 0.0267 0.1415
REM Highest difference peak 0.261, deepest hole -0.187, 1-sigma level 0.046
Q1 1 0.3793 0.4643 0.0664 11.00000 0.05 0.26
Q2 1 0.3340 0.5759 0.0579 11.00000 0.05 0.25
Q3 1 0.6036 0.8341 0.0584 11.00000 0.05 0.22
Q4 1 0.6452 0.6452 0.0000 10.50000 0.05 0.20
Q5 1 0.5671 0.7412 0.1271 11.00000 0.05 0.19
Q6 1 0.6135 0.6706 -0.0011 11.00000 0.05 0.19
Q7 1 0.4965 0.5820 0.0604 11.00000 0.05 0.19
Q8 1 0.8334 0.7169 0.0910 11.00000 0.05 0.18
Q9 1 0.7245 0.7745 0.0669 11.00000 0.05 0.17
Q10 1 0.2572 0.5673 0.0747 11.00000 0.05 0.17
;
_shelx_res_checksum 2425
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6 -12 -20 0.0474 -6.0000 -12.0000 -20.0000 -0.9494 0.0419 0.2234
6 12 20 0.0474 6.0000 12.0000 20.0000 0.9494 -0.0419 -0.2234
-6 -12 22 0.0832 -6.0000 -12.0000 22.0001 -0.6989 0.0365 -0.7127
7 14 -7 0.0595 7.0000 14.0000 -7.0000 0.9267 -0.0450 0.4155
9 -10 23 0.0616 9.0000 -10.0000 23.0001 -0.1315 0.8139 -0.5890
-11 6 24 0.0602 -11.0000 6.0000 24.0001 0.1352 -0.8068 -0.5327
-12 10 -4 0.0706 -12.0000 10.0000 -4.0000 0.1542 -0.9843 0.1422
1 4 -42 0.0995 1.0000 4.0000 -42.0001 -0.0040 -0.0637 1.0025
12 -10 -2 0.0746 12.0000 -10.0000 -2.0000 -0.1900 0.9851 -0.0085
-7 -13 -9 0.0431 -7.0000 -13.0000 -9.0000 -0.9681 0.0158 -0.0442
14 5 11 0.0581 14.0000 5.0000 11.0000 0.7590 0.6262 -0.0630
-14 -4 -15 0.0569 -14.0000 -4.0000 -15.0000 -0.7288 -0.6570 0.1668
-3 15 11 0.0464 -3.0000 15.0000 11.0000 0.7860 -0.6386 -0.0489
3 -10 -31 0.0800 3.0000 -10.0000 -31.0001 -0.6349 0.4848 0.5679
_olex2_date_sample_data_collection 2013-09-18
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane'
#######################################################################
#
# 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_str1816
_database_code_depnum_ccdc_archive 'CCDC 1952456'
loop_
_audit_author_name
_audit_author_address
'Marta Feliz'
;Instituto de Tecnologia Quimica
Spain
;
_audit_update_record
;
2019-09-09 deposited with the CCDC. 2020-03-20 downloaded from the CCDC.
;
_audit_creation_date 2019-08-26
_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 '[FeCl{(R,R)-Me-DuPhos}2](BF4)'
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H56 Cl Fe P4, B F4'
_chemical_formula_sum 'C36 H56 B Cl F4 Fe P4'
_chemical_formula_weight 790.79
_chemical_absolute_configuration rm
_chemical_melting_point ?
_chemical_oxdiff_formula 'C36 H96 P12 B F4 I Fe '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
_cell_length_a 14.8107(3)
_cell_length_b 16.8676(4)
_cell_length_c 15.5365(3)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3881.34(15)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 17631
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 28.5710
_cell_measurement_theta_min 3.2120
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.667
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.40968
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.353
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1664
_exptl_crystal_size_max 0.3475
_exptl_crystal_size_mid 0.2515
_exptl_crystal_size_min 0.1435
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0467
_diffrn_reflns_av_unetI/netI 0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 33898
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 23.998
_diffrn_reflns_theta_max 23.998
_diffrn_reflns_theta_min 2.779
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -46.00 24.00 0.7000 25.0000
omega____ theta____ kappa____ phi______ frames
- -11.1253 80.0000 136.0000 100
#__ type_ start__ end____ width___ exp.time_
2 omega -100.00 -55.90 0.7000 25.0000
omega____ theta____ kappa____ phi______ frames
- -11.1253 178.0000 120.0000 63
#__ type_ start__ end____ width___ exp.time_
3 omega -20.00 29.70 0.7000 25.0000
omega____ theta____ kappa____ phi______ frames
- -11.1253 -99.0000 -30.0000 71
#__ type_ start__ end____ width___ exp.time_
4 omega -20.00 29.70 0.7000 25.0000
omega____ theta____ kappa____ phi______ frames
- -11.1253 -99.0000 150.0000 71
#__ type_ start__ end____ width___ exp.time_
5 omega 34.00 99.10 0.7000 25.0000
omega____ theta____ kappa____ phi______ frames
- 12.0628 -178.0000 -60.0000 93
#__ type_ start__ end____ width___ exp.time_
6 omega -14.00 87.50 0.7000 25.0000
omega____ theta____ kappa____ phi______ frames
- 12.0628 37.0000 90.0000 145
#__ type_ start__ end____ width___ exp.time_
7 omega 35.00 81.20 0.7000 25.0000
omega____ theta____ kappa____ phi______ frames
- 12.0628 178.0000 90.0000 66
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 0.0436310000
_diffrn_orient_matrix_UB_12 -0.0089887000
_diffrn_orient_matrix_UB_13 -0.0160604000
_diffrn_orient_matrix_UB_21 -0.0171894000
_diffrn_orient_matrix_UB_22 -0.0349345000
_diffrn_orient_matrix_UB_23 -0.0194453000
_diffrn_orient_matrix_UB_31 -0.0096349000
_diffrn_orient_matrix_UB_32 0.0216353000
_diffrn_orient_matrix_UB_33 -0.0380587000
_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 0.786
_reflns_Friedel_fraction_full 1.000
_reflns_Friedel_fraction_max 1.000
_reflns_number_gt 5728
_reflns_number_total 6074
_reflns_odcompleteness_completeness 99.75
_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 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.523
_refine_diff_density_min -0.418
_refine_diff_density_rms 0.060
_refine_ls_abs_structure_details
;
Flack x determined using 2405 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.000(8)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.057
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 423
_refine_ls_number_reflns 6074
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0464
_refine_ls_R_factor_gt 0.0425
_refine_ls_restrained_S_all 1.057
_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^)+(0.0612P)^2^+3.6528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1096
_refine_ls_wR_factor_ref 0.1142
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Others
Fixed Sof: F1(0.61) F2(0.59) F3(0.63) F4(0.41) F5(0.7) F0AA(0.37) F6(0.3)
F7(0.39)
3.a Ternary CH refined with riding coordinates:
C6(H6), C7(H7), C10(H10), C11(H11), C14(H14), C16(H16), C19(H19), C22(H22)
3.b Secondary CH2 refined with riding coordinates:
C9(H9A,H9B), C8(H8A,H8B), C12(H12A,H12B), C13(H13A,H13B), C17(H17A,H17B),
C18(H18A,H18B), C20(H20A,H20B), C21(H21A,H21B)
3.c Aromatic/amide H refined with riding coordinates:
C5(H5), C2AA(H2AA), C4(H4), C15(H15), C28(H28), C31(H31), C29(H29), C30(H30)
3.d Idealised Me refined as rotating group:
C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C32(H32A,H32B,
H32C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C35(H35A,
H35B,H35C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.37006(5) 0.13555(4) 0.20662(5) 0.0303(2) Uani 1 1 d . . . . .
P1 P 0.32517(10) 0.23282(8) 0.29903(10) 0.0335(3) Uani 1 1 d . . . . .
P2 P 0.41196(10) 0.10503(9) 0.06871(9) 0.0323(3) Uani 1 1 d . . . . .
P3 P 0.21800(9) 0.11605(8) 0.18664(9) 0.0327(3) Uani 1 1 d . . . . .
P4 P 0.52260(10) 0.14634(9) 0.23253(9) 0.0345(3) Uani 1 1 d . . . . .
Cl1 Cl 0.37468(14) 0.01920(11) 0.27949(15) 0.0759(6) Uani 1 1 d . . . . .
C0AA C 0.5829(4) 0.0987(3) 0.1436(4) 0.0374(13) Uani 1 1 d . . . . .
C1AA C 0.5336(4) 0.0852(3) 0.0675(4) 0.0353(13) Uani 1 1 d . . . . .
C5 C 0.6750(4) 0.0827(4) 0.1427(4) 0.0468(16) Uani 1 1 d . . . . .
H5 H 0.708786 0.091023 0.192312 0.056 Uiso 1 1 calc R . . . .
C2AA C 0.5777(4) 0.0577(4) -0.0058(4) 0.0427(14) Uani 1 1 d . . . . .
H2AA H 0.545218 0.049809 -0.056327 0.051 Uiso 1 1 calc R . . . .
C4 C 0.7170(4) 0.0549(4) 0.0701(5) 0.0536(17) Uani 1 1 d . . . . .
H4 H 0.778651 0.044657 0.071168 0.064 Uiso 1 1 calc R . . . .
C6 C 0.3586(4) 0.0171(3) 0.0168(4) 0.0397(13) Uani 1 1 d . . . . .
H6 H 0.296466 0.015215 0.038435 0.048 Uiso 1 1 calc R . . . .
C9 C 0.4018(5) 0.3679(4) 0.3584(4) 0.0516(16) Uani 1 1 d . . . . .
H9A H 0.464516 0.360119 0.342352 0.062 Uiso 1 1 calc R . . . .
H9B H 0.392854 0.423798 0.370476 0.062 Uiso 1 1 calc R . . . .
C8 C 0.3801(5) 0.3195(4) 0.4375(4) 0.0536(17) Uani 1 1 d . . . . .
H8A H 0.322732 0.335855 0.461706 0.064 Uiso 1 1 calc R . . . .
H8B H 0.426635 0.326417 0.480799 0.064 Uiso 1 1 calc R . . . .
C7 C 0.3757(4) 0.2322(4) 0.4087(4) 0.0414(13) Uani 1 1 d . . . . .
H7 H 0.438144 0.213942 0.402312 0.050 Uiso 1 1 calc R . . . .
C10 C 0.3406(4) 0.3424(3) 0.2847(4) 0.0436(14) Uani 1 1 d . . . . .
H10 H 0.281604 0.366648 0.295764 0.052 Uiso 1 1 calc R . . . .
C11 C 0.1618(4) 0.1649(4) 0.0936(4) 0.0404(14) Uani 1 1 d . . . . .
H11 H 0.202612 0.159523 0.044291 0.049 Uiso 1 1 calc R . . . .
C12 C 0.0787(4) 0.1149(4) 0.0740(4) 0.0544(17) Uani 1 1 d . . . . .
H12A H 0.029764 0.129148 0.112502 0.065 Uiso 1 1 calc R . . . .
H12B H 0.059067 0.123872 0.015304 0.065 Uiso 1 1 calc R . . . .
C14 C 0.1538(4) 0.0200(4) 0.1718(4) 0.0430(14) Uani 1 1 d . . . . .
H14 H 0.106919 0.020303 0.216290 0.052 Uiso 1 1 calc R . . . .
C13 C 0.1035(5) 0.0298(4) 0.0863(4) 0.0543(17) Uani 1 1 d . . . . .
H13A H 0.141549 0.012366 0.039145 0.065 Uiso 1 1 calc R . . . .
H13B H 0.049310 -0.002536 0.086493 0.065 Uiso 1 1 calc R . . . .
C16 C 0.5885(4) 0.1130(4) 0.3309(4) 0.0484(15) Uani 1 1 d . . . . .
H16 H 0.636016 0.077745 0.309517 0.058 Uiso 1 1 calc R . . . .
C19 C 0.5767(4) 0.2460(4) 0.2322(4) 0.0450(15) Uani 1 1 d . . . . .
H19 H 0.534945 0.282385 0.261147 0.054 Uiso 1 1 calc R . . . .
C17 C 0.6368(6) 0.1880(5) 0.3634(5) 0.067(2) Uani 1 1 d . . . . .
H17A H 0.597747 0.216687 0.402647 0.080 Uiso 1 1 calc R . . . .
H17B H 0.691226 0.173282 0.394282 0.080 Uiso 1 1 calc R . . . .
C15 C 0.6690(4) 0.0420(4) -0.0043(4) 0.0484(16) Uani 1 1 d . . . . .
H15 H 0.697867 0.022805 -0.053245 0.058 Uiso 1 1 calc R . . . .
C18 C 0.6607(5) 0.2399(4) 0.2887(5) 0.0606(19) Uani 1 1 d . . . . .
H18A H 0.710348 0.216997 0.256420 0.073 Uiso 1 1 calc R . . . .
H18B H 0.678766 0.292047 0.308686 0.073 Uiso 1 1 calc R . . . .
C22 C 0.3975(4) 0.1697(4) -0.0288(4) 0.0444(15) Uani 1 1 d . . . . .
H22 H 0.456593 0.171455 -0.057098 0.053 Uiso 1 1 calc R . . . .
C20 C 0.3515(5) 0.0354(4) -0.0791(4) 0.0524(17) Uani 1 1 d . . . . .
H20A H 0.407023 0.020533 -0.108046 0.063 Uiso 1 1 calc R . . . .
H20B H 0.302249 0.005561 -0.104393 0.063 Uiso 1 1 calc R . . . .
C21 C 0.3349(5) 0.1230(4) -0.0897(4) 0.0543(17) Uani 1 1 d . . . . .
H21A H 0.272361 0.135019 -0.076460 0.065 Uiso 1 1 calc R . . . .
H21B H 0.346437 0.138464 -0.148796 0.065 Uiso 1 1 calc R . . . .
C23 C 0.2039(4) 0.2239(3) 0.3184(4) 0.0383(13) Uani 1 1 d . . . . .
C24 C 0.1577(4) 0.1641(3) 0.2759(4) 0.0381(13) Uani 1 1 d . . . . .
C25 C 0.3710(5) 0.3722(3) 0.1964(4) 0.0548(16) Uani 1 1 d . . . . .
H25A H 0.428962 0.350117 0.182755 0.082 Uiso 1 1 calc GR . . . .
H25B H 0.375127 0.429005 0.197325 0.082 Uiso 1 1 calc GR . . . .
H25C H 0.327862 0.356237 0.153622 0.082 Uiso 1 1 calc GR . . . .
C26 C 0.3693(5) 0.2544(4) -0.0163(4) 0.0547(17) Uani 1 1 d . . . . .
H26A H 0.312035 0.255974 0.012691 0.082 Uiso 1 1 calc GR . . . .
H26B H 0.363974 0.279848 -0.071321 0.082 Uiso 1 1 calc GR . . . .
H26C H 0.413683 0.281472 0.017745 0.082 Uiso 1 1 calc GR . . . .
C27 C 0.5947(5) 0.2801(4) 0.1431(5) 0.0600(19) Uani 1 1 d . . . . .
H27A H 0.643703 0.251885 0.116692 0.090 Uiso 1 1 calc GR . . . .
H27B H 0.610305 0.335190 0.148125 0.090 Uiso 1 1 calc GR . . . .
H27C H 0.541522 0.274851 0.108244 0.090 Uiso 1 1 calc GR . . . .
C28 C 0.0654(4) 0.1541(4) 0.2910(4) 0.0485(15) Uani 1 1 d . . . . .
H28 H 0.034158 0.113586 0.263448 0.058 Uiso 1 1 calc R . . . .
C31 C 0.1568(5) 0.2741(4) 0.3739(4) 0.0552(18) Uani 1 1 d . . . . .
H31 H 0.187387 0.314750 0.401931 0.066 Uiso 1 1 calc R . . . .
C29 C 0.0205(4) 0.2042(5) 0.3466(5) 0.0594(19) Uani 1 1 d . . . . .
H29 H -0.040941 0.197173 0.356343 0.071 Uiso 1 1 calc R . . . .
C30 C 0.0657(5) 0.2642(5) 0.3875(5) 0.063(2) Uani 1 1 d . . . . .
H30 H 0.034854 0.298111 0.424384 0.076 Uiso 1 1 calc R . . . .
C32 C 0.1428(5) 0.2526(4) 0.1043(5) 0.0571(18) Uani 1 1 d . . . . .
H32A H 0.094386 0.259760 0.144675 0.086 Uiso 1 1 calc GR . . . .
H32B H 0.125893 0.274851 0.049750 0.086 Uiso 1 1 calc GR . . . .
H32C H 0.195970 0.278779 0.125252 0.086 Uiso 1 1 calc GR . . . .
C34 C 0.2009(5) -0.0603(3) 0.1805(4) 0.0496(16) Uani 1 1 d . . . . .
H34A H 0.241989 -0.067467 0.133391 0.074 Uiso 1 1 calc GR . . . .
H34B H 0.156516 -0.101801 0.179790 0.074 Uiso 1 1 calc GR . . . .
H34C H 0.233599 -0.062030 0.233803 0.074 Uiso 1 1 calc GR . . . .
C33 C 0.3998(5) -0.0622(4) 0.0379(5) 0.0537(17) Uani 1 1 d . . . . .
H33A H 0.459659 -0.064852 0.014377 0.081 Uiso 1 1 calc GR . . . .
H33B H 0.363446 -0.103584 0.013458 0.081 Uiso 1 1 calc GR . . . .
H33C H 0.402523 -0.068641 0.099216 0.081 Uiso 1 1 calc GR . . . .
C36 C 0.5422(5) 0.0681(5) 0.4048(5) 0.062(2) Uani 1 1 d . . . . .
H36A H 0.492675 0.099002 0.426290 0.093 Uiso 1 1 calc GR . . . .
H36B H 0.584922 0.059108 0.450214 0.093 Uiso 1 1 calc GR . . . .
H36C H 0.520122 0.018144 0.383975 0.093 Uiso 1 1 calc GR . . . .
C35 C 0.3303(5) 0.1768(5) 0.4737(4) 0.0610(19) Uani 1 1 d . . . . .
H35A H 0.273080 0.198576 0.490471 0.091 Uiso 1 1 calc GR . . . .
H35B H 0.368196 0.171437 0.523510 0.091 Uiso 1 1 calc GR . . . .
H35C H 0.321286 0.125718 0.447894 0.091 Uiso 1 1 calc GR . . . .
B1 B 0.8835(10) 0.0045(8) 0.2490(9) 0.100(4) Uiso 1 1 d . . . . .
F1 F 0.9655(7) -0.0360(6) 0.2801(6) 0.092(3) Uiso 0.61 1 d . . P A .
F2 F 0.8821(8) 0.0789(7) 0.2161(8) 0.111(3) Uiso 0.59 1 d . . P A 1
F3 F 0.8182(9) -0.0498(8) 0.2662(8) 0.129(4) Uiso 0.63 1 d . . P A 1
F4 F 0.8540(15) 0.0635(12) 0.3017(14) 0.154(7) Uiso 0.41 1 d . . P A 2
F5 F 0.8857(9) -0.0399(8) 0.1638(8) 0.158(4) Uiso 0.7 1 d . . P A 1
F0AA F 0.7982(10) -0.0056(9) 0.2866(10) 0.087(4) Uiso 0.37 1 d . . P A 2
F6 F 0.9055(11) 0.0456(10) 0.1803(11) 0.077(4) Uiso 0.3 1 d . . P A 2
F7 F 0.9490(8) -0.0009(8) 0.3018(8) 0.070(3) Uiso 0.39 1 d . . P A .
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 0.0301(4) 0.0310(4) 0.0299(4) -0.0012(3) -0.0003(3) -0.0010(3)
P1 0.0349(7) 0.0307(7) 0.0349(7) -0.0021(6) -0.0016(6) -0.0025(6)
P2 0.0309(7) 0.0377(7) 0.0285(7) -0.0007(6) -0.0026(6) -0.0012(6)
P3 0.0324(7) 0.0349(7) 0.0308(7) 0.0003(6) -0.0009(6) -0.0023(6)
P4 0.0335(8) 0.0368(7) 0.0331(7) -0.0016(6) -0.0016(6) -0.0022(6)
Cl1 0.0726(12) 0.0576(10) 0.0977(15) 0.0353(10) -0.0390(12) -0.0214(9)
C0AA 0.039(3) 0.034(3) 0.039(3) 0.000(3) -0.003(3) 0.001(3)
C1AA 0.034(3) 0.033(3) 0.039(3) 0.002(2) -0.004(3) -0.001(2)
C5 0.033(3) 0.057(4) 0.051(4) -0.011(3) -0.003(3) 0.000(3)
C2AA 0.041(4) 0.049(4) 0.038(3) -0.003(3) 0.003(3) -0.001(3)
C4 0.035(3) 0.061(4) 0.065(4) -0.004(4) 0.002(3) 0.005(3)
C6 0.036(3) 0.044(3) 0.039(3) -0.006(3) -0.003(3) -0.002(3)
C9 0.059(4) 0.037(3) 0.059(4) -0.011(3) 0.002(3) -0.009(3)
C8 0.062(4) 0.051(4) 0.047(4) -0.014(3) -0.005(3) -0.015(3)
C7 0.041(3) 0.046(3) 0.037(3) -0.001(3) -0.004(3) -0.008(3)
C10 0.055(4) 0.026(3) 0.050(4) -0.001(3) 0.004(3) 0.004(2)
C11 0.040(3) 0.046(3) 0.036(3) 0.005(3) -0.005(3) 0.003(3)
C12 0.045(4) 0.072(5) 0.046(4) 0.007(3) -0.014(3) 0.002(3)
C14 0.047(4) 0.040(3) 0.042(3) -0.005(3) 0.001(3) -0.009(3)
C13 0.050(4) 0.063(4) 0.050(4) -0.008(3) -0.008(3) -0.013(3)
C16 0.047(4) 0.059(4) 0.040(3) 0.004(3) -0.008(3) 0.002(3)
C19 0.043(3) 0.043(3) 0.049(3) -0.009(3) 0.003(3) -0.011(3)
C17 0.058(5) 0.087(5) 0.055(4) -0.009(4) -0.020(4) -0.014(4)
C15 0.046(4) 0.051(4) 0.048(4) -0.003(3) 0.011(3) 0.003(3)
C18 0.045(4) 0.064(4) 0.073(5) -0.012(4) -0.012(3) -0.015(3)
C22 0.042(4) 0.057(4) 0.034(3) 0.008(3) 0.000(3) 0.002(3)
C20 0.048(4) 0.072(5) 0.037(3) -0.018(3) -0.001(3) -0.002(3)
C21 0.054(4) 0.076(5) 0.033(3) 0.006(3) -0.002(3) 0.005(4)
C23 0.038(3) 0.039(3) 0.037(3) 0.000(3) 0.000(2) 0.001(3)
C24 0.041(3) 0.041(3) 0.032(3) 0.001(2) 0.004(2) -0.002(2)
C25 0.066(4) 0.037(3) 0.061(4) 0.012(3) 0.003(4) 0.003(3)
C26 0.062(4) 0.052(4) 0.051(4) 0.021(3) 0.001(3) 0.006(4)
C27 0.063(5) 0.049(4) 0.068(5) 0.006(3) 0.009(4) -0.014(3)
C28 0.042(3) 0.061(4) 0.042(3) -0.003(3) 0.005(3) -0.008(3)
C31 0.049(4) 0.060(4) 0.057(4) -0.023(3) 0.004(3) 0.000(3)
C29 0.032(3) 0.083(5) 0.063(4) -0.011(4) 0.013(3) -0.003(3)
C30 0.047(4) 0.081(5) 0.062(4) -0.025(4) 0.014(3) 0.009(4)
C32 0.061(4) 0.051(4) 0.059(4) 0.015(3) -0.004(4) 0.010(3)
C34 0.066(4) 0.037(3) 0.046(4) -0.001(3) 0.001(3) -0.006(3)
C33 0.048(4) 0.046(4) 0.067(4) -0.015(3) -0.005(3) -0.003(3)
C36 0.067(5) 0.070(5) 0.049(4) 0.011(4) -0.005(4) 0.011(4)
C35 0.071(5) 0.069(5) 0.043(4) 0.008(3) -0.005(4) -0.014(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 P1 2.2793(16) . ?
Fe1 P2 2.2893(16) . ?
Fe1 P3 2.2971(16) . ?
Fe1 P4 2.3021(16) . ?
Fe1 Cl1 2.2666(18) . ?
P1 C7 1.861(6) . ?
P1 C10 1.876(5) . ?
P1 C23 1.828(6) . ?
P2 C1AA 1.833(6) . ?
P2 C6 1.863(6) . ?
P2 C22 1.879(6) . ?
P3 C11 1.860(6) . ?
P3 C14 1.893(6) . ?
P3 C24 1.837(6) . ?
P4 C0AA 1.830(6) . ?
P4 C16 1.899(6) . ?
P4 C19 1.863(6) . ?
C0AA C1AA 1.409(8) . ?
C0AA C5 1.391(9) . ?
C1AA C2AA 1.392(8) . ?
C5 C4 1.371(9) . ?
C2AA C15 1.377(9) . ?
C4 C15 1.374(9) . ?
C6 C20 1.526(9) . ?
C6 C33 1.506(9) . ?
C9 C8 1.511(9) . ?
C9 C10 1.522(9) . ?
C8 C7 1.540(8) . ?
C7 C35 1.531(9) . ?
C10 C25 1.529(9) . ?
C11 C12 1.523(9) . ?
C11 C32 1.515(9) . ?
C12 C13 1.493(10) . ?
C14 C13 1.533(9) . ?
C14 C34 1.529(9) . ?
C16 C17 1.540(10) . ?
C16 C36 1.536(10) . ?
C19 C18 1.527(9) . ?
C19 C27 1.522(9) . ?
C17 C18 1.496(11) . ?
C22 C21 1.541(9) . ?
C22 C26 1.501(9) . ?
C20 C21 1.506(10) . ?
C23 C24 1.386(8) . ?
C23 C31 1.395(8) . ?
C24 C28 1.398(9) . ?
C28 C29 1.379(9) . ?
C31 C30 1.377(10) . ?
C29 C30 1.369(10) . ?
B1 F1 1.473(17) . ?
B1 F2 1.356(17) . ?
B1 F3 1.359(17) . ?
B1 F4 1.36(2) . ?
B1 F5 1.521(18) . ?
B1 F0AA 1.40(2) . ?
B1 F6 1.31(2) . ?
B1 F7 1.273(17) . ?
F1 F7 0.724(13) . ?
F4 F0AA 1.45(2) . ?
F4 F7 1.78(2) . ?
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
P1 Fe1 P2 146.15(6) . . ?
P1 Fe1 P3 84.39(6) . . ?
P1 Fe1 P4 96.85(6) . . ?
P2 Fe1 P3 96.14(6) . . ?
P2 Fe1 P4 85.15(6) . . ?
P3 Fe1 P4 175.68(6) . . ?
Cl1 Fe1 P1 108.51(8) . . ?
Cl1 Fe1 P2 105.34(8) . . ?
Cl1 Fe1 P3 88.46(7) . . ?
Cl1 Fe1 P4 87.22(7) . . ?
C7 P1 Fe1 117.1(2) . . ?
C7 P1 C10 93.7(3) . . ?
C10 P1 Fe1 126.8(2) . . ?
C23 P1 Fe1 109.33(19) . . ?
C23 P1 C7 104.1(3) . . ?
C23 P1 C10 102.8(3) . . ?
C1AA P2 Fe1 108.51(19) . . ?
C1AA P2 C6 105.5(3) . . ?
C1AA P2 C22 102.1(3) . . ?
C6 P2 Fe1 118.0(2) . . ?
C6 P2 C22 93.7(3) . . ?
C22 P2 Fe1 126.4(2) . . ?
C11 P3 Fe1 118.7(2) . . ?
C11 P3 C14 93.4(3) . . ?
C14 P3 Fe1 129.1(2) . . ?
C24 P3 Fe1 108.12(19) . . ?
C24 P3 C11 100.0(3) . . ?
C24 P3 C14 103.0(3) . . ?
C0AA P4 Fe1 108.17(19) . . ?
C0AA P4 C16 103.1(3) . . ?
C0AA P4 C19 100.6(3) . . ?
C16 P4 Fe1 128.4(2) . . ?
C19 P4 Fe1 119.5(2) . . ?
C19 P4 C16 92.8(3) . . ?
C1AA C0AA P4 116.9(4) . . ?
C5 C0AA P4 124.9(5) . . ?
C5 C0AA C1AA 117.9(6) . . ?
C0AA C1AA P2 118.1(4) . . ?
C2AA C1AA P2 122.1(4) . . ?
C2AA C1AA C0AA 119.9(5) . . ?
C4 C5 C0AA 121.3(6) . . ?
C15 C2AA C1AA 120.7(6) . . ?
C5 C4 C15 120.8(6) . . ?
C20 C6 P2 106.9(4) . . ?
C33 C6 P2 116.2(4) . . ?
C33 C6 C20 114.8(5) . . ?
C8 C9 C10 109.4(5) . . ?
C9 C8 C7 106.9(5) . . ?
C8 C7 P1 106.1(4) . . ?
C35 C7 P1 115.5(4) . . ?
C35 C7 C8 114.2(5) . . ?
C9 C10 P1 105.2(4) . . ?
C9 C10 C25 114.0(5) . . ?
C25 C10 P1 117.8(4) . . ?
C12 C11 P3 105.7(4) . . ?
C32 C11 P3 115.5(5) . . ?
C32 C11 C12 114.4(5) . . ?
C13 C12 C11 108.0(5) . . ?
C13 C14 P3 104.9(4) . . ?
C34 C14 P3 121.3(4) . . ?
C34 C14 C13 113.2(5) . . ?
C12 C13 C14 109.5(5) . . ?
C17 C16 P4 105.0(5) . . ?
C36 C16 P4 121.2(5) . . ?
C36 C16 C17 111.6(6) . . ?
C18 C19 P4 106.7(5) . . ?
C27 C19 P4 114.8(4) . . ?
C27 C19 C18 113.9(6) . . ?
C18 C17 C16 109.7(6) . . ?
C4 C15 C2AA 119.4(6) . . ?
C17 C18 C19 107.0(6) . . ?
C21 C22 P2 105.5(4) . . ?
C26 C22 P2 118.7(4) . . ?
C26 C22 C21 113.5(5) . . ?
C21 C20 C6 108.4(5) . . ?
C20 C21 C22 109.6(5) . . ?
C24 C23 P1 117.8(4) . . ?
C24 C23 C31 119.4(5) . . ?
C31 C23 P1 122.9(5) . . ?
C23 C24 P3 116.2(4) . . ?
C23 C24 C28 119.3(5) . . ?
C28 C24 P3 123.3(5) . . ?
C29 C28 C24 120.2(6) . . ?
C30 C31 C23 120.7(6) . . ?
C30 C29 C28 120.5(6) . . ?
C29 C30 C31 119.9(7) . . ?
F1 B1 F5 92.3(10) . . ?
F2 B1 F1 124.4(12) . . ?
F2 B1 F3 133.4(14) . . ?
F2 B1 F5 97.3(11) . . ?
F3 B1 F1 102.1(11) . . ?
F3 B1 F5 81.6(11) . . ?
F4 B1 F1 114.0(15) . . ?
F4 B1 F0AA 63.2(13) . . ?
F0AA B1 F1 123.4(12) . . ?
F6 B1 F1 107.8(13) . . ?
F6 B1 F4 100.5(15) . . ?
F6 B1 F0AA 128.7(15) . . ?
F7 B1 F1 29.4(7) . . ?
F7 B1 F2 108.7(13) . . ?
F7 B1 F3 111.6(13) . . ?
F7 B1 F4 84.8(15) . . ?
F7 B1 F5 120.6(13) . . ?
F7 B1 F0AA 114.2(13) . . ?
F7 B1 F6 111.8(14) . . ?
F7 F1 B1 59.8(14) . . ?
B1 F4 F0AA 59.8(12) . . ?
B1 F4 F7 45.5(10) . . ?
F0AA F4 F7 87.7(13) . . ?
B1 F0AA F4 57.0(11) . . ?
B1 F7 F4 49.7(10) . . ?
F1 F7 B1 90.8(17) . . ?
F1 F7 F4 140.0(19) . . ?
_shelx_res_file
;
TITL str1816 in P212121 #19
str1816.res
created by SHELXL-2018/3 at 11:03:26 on 26-Aug-2019
REM reset to P212121 #19
CELL 0.71073 14.810725 16.867568 15.536488 90 90 90
ZERR 4 0.000337 0.000372 0.000318 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z
SFAC C H B Cl F Fe P
UNIT 144 224 4 4 16 4 16
L.S. 25 0 0
PLAN 20
BOND
fmap 2
acta
OMIT -4 48
REM
REM
REM
WGHT 0.061200 3.652800
FVAR 1.55460
FE1 6 0.370060 0.135551 0.206625 11.00000 0.03005 0.03098 =
0.02995 -0.00118 -0.00032 -0.00099
P1 7 0.325165 0.232822 0.299034 11.00000 0.03493 0.03074 =
0.03492 -0.00214 -0.00156 -0.00247
P2 7 0.411956 0.105027 0.068714 11.00000 0.03086 0.03768 =
0.02851 -0.00072 -0.00256 -0.00116
P3 7 0.218000 0.116052 0.186641 11.00000 0.03238 0.03488 =
0.03080 0.00030 -0.00093 -0.00233
P4 7 0.522604 0.146345 0.232534 11.00000 0.03346 0.03679 =
0.03312 -0.00157 -0.00165 -0.00225
CL1 4 0.374679 0.019203 0.279490 11.00000 0.07256 0.05758 =
0.09767 0.03533 -0.03901 -0.02145
C0AA 1 0.582862 0.098671 0.143649 11.00000 0.03911 0.03384 =
0.03940 0.00016 -0.00307 0.00118
C1AA 1 0.533633 0.085166 0.067464 11.00000 0.03412 0.03284 =
0.03901 0.00170 -0.00403 -0.00109
C5 1 0.674983 0.082686 0.142686 11.00000 0.03335 0.05664 =
0.05050 -0.01065 -0.00279 0.00046
AFIX 43
H5 2 0.708786 0.091023 0.192312 11.00000 -1.20000
AFIX 0
C2AA 1 0.577723 0.057666 -0.005828 11.00000 0.04068 0.04917 =
0.03823 -0.00275 0.00322 -0.00083
AFIX 43
H2AA 2 0.545218 0.049809 -0.056327 11.00000 -1.20000
AFIX 0
C4 1 0.716961 0.054893 0.070070 11.00000 0.03519 0.06095 =
0.06465 -0.00383 0.00184 0.00483
AFIX 43
H4 2 0.778651 0.044657 0.071168 11.00000 -1.20000
AFIX 0
C6 1 0.358599 0.017141 0.016846 11.00000 0.03615 0.04446 =
0.03850 -0.00587 -0.00307 -0.00162
AFIX 13
H6 2 0.296466 0.015215 0.038435 11.00000 -1.20000
AFIX 0
C9 1 0.401845 0.367937 0.358372 11.00000 0.05892 0.03684 =
0.05891 -0.01056 0.00221 -0.00918
AFIX 23
H9A 2 0.464516 0.360119 0.342352 11.00000 -1.20000
H9B 2 0.392854 0.423798 0.370476 11.00000 -1.20000
AFIX 0
C8 1 0.380135 0.319457 0.437486 11.00000 0.06249 0.05107 =
0.04724 -0.01386 -0.00464 -0.01468
AFIX 23
H8A 2 0.322732 0.335855 0.461706 11.00000 -1.20000
H8B 2 0.426635 0.326417 0.480799 11.00000 -1.20000
AFIX 0
C7 1 0.375680 0.232190 0.408674 11.00000 0.04061 0.04627 =
0.03719 -0.00101 -0.00441 -0.00766
AFIX 13
H7 2 0.438144 0.213942 0.402312 11.00000 -1.20000
AFIX 0
C10 1 0.340610 0.342399 0.284736 11.00000 0.05469 0.02634 =
0.04968 -0.00111 0.00420 0.00426
AFIX 13
H10 2 0.281604 0.366648 0.295764 11.00000 -1.20000
AFIX 0
C11 1 0.161822 0.164899 0.093613 11.00000 0.03981 0.04577 =
0.03572 0.00519 -0.00506 0.00287
AFIX 13
H11 2 0.202612 0.159523 0.044291 11.00000 -1.20000
AFIX 0
C12 1 0.078732 0.114870 0.074050 11.00000 0.04496 0.07209 =
0.04602 0.00681 -0.01358 0.00151
AFIX 23
H12A 2 0.029764 0.129148 0.112502 11.00000 -1.20000
H12B 2 0.059067 0.123872 0.015304 11.00000 -1.20000
AFIX 0
C14 1 0.153837 0.019987 0.171814 11.00000 0.04717 0.03950 =
0.04218 -0.00463 0.00112 -0.00933
AFIX 13
H14 2 0.106919 0.020303 0.216290 11.00000 -1.20000
AFIX 0
C13 1 0.103455 0.029817 0.086266 11.00000 0.05000 0.06280 =
0.05022 -0.00766 -0.00817 -0.01332
AFIX 23
H13A 2 0.141549 0.012366 0.039145 11.00000 -1.20000
H13B 2 0.049310 -0.002536 0.086493 11.00000 -1.20000
AFIX 0
C16 1 0.588455 0.112986 0.330947 11.00000 0.04687 0.05885 =
0.03955 0.00390 -0.00762 0.00160
AFIX 13
H16 2 0.636016 0.077745 0.309517 11.00000 -1.20000
AFIX 0
C19 1 0.576672 0.246046 0.232164 11.00000 0.04301 0.04282 =
0.04927 -0.00934 0.00331 -0.01065
AFIX 13
H19 2 0.534945 0.282385 0.261147 11.00000 -1.20000
AFIX 0
C17 1 0.636849 0.188037 0.363391 11.00000 0.05843 0.08655 =
0.05478 -0.00854 -0.02048 -0.01416
AFIX 23
H17A 2 0.597747 0.216687 0.402647 11.00000 -1.20000
H17B 2 0.691226 0.173282 0.394282 11.00000 -1.20000
AFIX 0
C15 1 0.668980 0.041972 -0.004339 11.00000 0.04581 0.05097 =
0.04830 -0.00337 0.01073 0.00255
AFIX 43
H15 2 0.697867 0.022805 -0.053245 11.00000 -1.20000
AFIX 0
C18 1 0.660737 0.239916 0.288702 11.00000 0.04475 0.06440 =
0.07269 -0.01235 -0.01221 -0.01481
AFIX 23
H18A 2 0.710348 0.216997 0.256420 11.00000 -1.20000
H18B 2 0.678766 0.292047 0.308686 11.00000 -1.20000
AFIX 0
C22 1 0.397493 0.169674 -0.028797 11.00000 0.04232 0.05729 =
0.03365 0.00754 -0.00029 0.00197
AFIX 13
H22 2 0.456593 0.171455 -0.057098 11.00000 -1.20000
AFIX 0
C20 1 0.351526 0.035437 -0.079110 11.00000 0.04779 0.07183 =
0.03744 -0.01842 -0.00089 -0.00236
AFIX 23
H20A 2 0.407023 0.020533 -0.108046 11.00000 -1.20000
H20B 2 0.302249 0.005561 -0.104393 11.00000 -1.20000
AFIX 0
C21 1 0.334891 0.123007 -0.089676 11.00000 0.05362 0.07594 =
0.03340 0.00562 -0.00222 0.00507
AFIX 23
H21A 2 0.272361 0.135019 -0.076460 11.00000 -1.20000
H21B 2 0.346437 0.138464 -0.148796 11.00000 -1.20000
AFIX 0
C23 1 0.203880 0.223880 0.318402 11.00000 0.03819 0.03938 =
0.03722 0.00047 0.00037 0.00086
C24 1 0.157749 0.164078 0.275911 11.00000 0.04144 0.04059 =
0.03227 0.00101 0.00412 -0.00201
C25 1 0.370966 0.372215 0.196386 11.00000 0.06650 0.03685 =
0.06106 0.01164 0.00327 0.00265
AFIX 137
H25A 2 0.428962 0.350117 0.182755 11.00000 -1.50000
H25B 2 0.375127 0.429005 0.197325 11.00000 -1.50000
H25C 2 0.327862 0.356237 0.153622 11.00000 -1.50000
AFIX 0
C26 1 0.369250 0.254377 -0.016293 11.00000 0.06198 0.05157 =
0.05068 0.02058 0.00112 0.00605
AFIX 137
H26A 2 0.312035 0.255974 0.012691 11.00000 -1.50000
H26B 2 0.363974 0.279848 -0.071321 11.00000 -1.50000
H26C 2 0.413683 0.281472 0.017745 11.00000 -1.50000
AFIX 0
C27 1 0.594717 0.280142 0.143078 11.00000 0.06291 0.04883 =
0.06834 0.00639 0.00902 -0.01434
AFIX 137
H27A 2 0.643703 0.251885 0.116692 11.00000 -1.50000
H27B 2 0.610305 0.335190 0.148125 11.00000 -1.50000
H27C 2 0.541522 0.274851 0.108244 11.00000 -1.50000
AFIX 0
C28 1 0.065413 0.154121 0.290992 11.00000 0.04169 0.06149 =
0.04241 -0.00315 0.00487 -0.00776
AFIX 43
H28 2 0.034158 0.113586 0.263448 11.00000 -1.20000
AFIX 0
C31 1 0.156845 0.274106 0.373854 11.00000 0.04899 0.05983 =
0.05677 -0.02282 0.00384 -0.00020
AFIX 43
H31 2 0.187387 0.314750 0.401931 11.00000 -1.20000
AFIX 0
C29 1 0.020491 0.204189 0.346571 11.00000 0.03182 0.08308 =
0.06323 -0.01112 0.01265 -0.00326
AFIX 43
H29 2 -0.040941 0.197173 0.356343 11.00000 -1.20000
AFIX 0
C30 1 0.065674 0.264167 0.387481 11.00000 0.04711 0.08056 =
0.06236 -0.02532 0.01353 0.00914
AFIX 43
H30 2 0.034854 0.298111 0.424384 11.00000 -1.20000
AFIX 0
C32 1 0.142773 0.252607 0.104302 11.00000 0.06100 0.05076 =
0.05948 0.01497 -0.00373 0.01009
AFIX 137
H32A 2 0.094386 0.259760 0.144675 11.00000 -1.50000
H32B 2 0.125893 0.274851 0.049750 11.00000 -1.50000
H32C 2 0.195970 0.278779 0.125252 11.00000 -1.50000
AFIX 0
C34 1 0.200858 -0.060295 0.180508 11.00000 0.06617 0.03689 =
0.04563 -0.00099 0.00140 -0.00570
AFIX 137
H34A 2 0.241989 -0.067467 0.133391 11.00000 -1.50000
H34B 2 0.156516 -0.101801 0.179790 11.00000 -1.50000
H34C 2 0.233599 -0.062030 0.233803 11.00000 -1.50000
AFIX 0
C33 1 0.399792 -0.062176 0.037881 11.00000 0.04774 0.04620 =
0.06718 -0.01484 -0.00546 -0.00296
AFIX 137
H33A 2 0.459659 -0.064852 0.014377 11.00000 -1.50000
H33B 2 0.363446 -0.103584 0.013458 11.00000 -1.50000
H33C 2 0.402523 -0.068641 0.099216 11.00000 -1.50000
AFIX 0
C36 1 0.542210 0.068104 0.404774 11.00000 0.06675 0.07036 =
0.04899 0.01119 -0.00487 0.01107
AFIX 137
H36A 2 0.492675 0.099002 0.426290 11.00000 -1.50000
H36B 2 0.584922 0.059108 0.450214 11.00000 -1.50000
H36C 2 0.520122 0.018144 0.383975 11.00000 -1.50000
AFIX 0
C35 1 0.330332 0.176817 0.473701 11.00000 0.07067 0.06900 =
0.04320 0.00754 -0.00476 -0.01364
AFIX 137
H35A 2 0.273080 0.198576 0.490471 11.00000 -1.50000
H35B 2 0.368196 0.171437 0.523510 11.00000 -1.50000
H35C 2 0.321286 0.125718 0.447894 11.00000 -1.50000
AFIX 0
B1 3 0.883539 0.004469 0.249034 11.00000 0.10047
F1 5 0.965480 -0.035958 0.280064 10.61000 0.09232
PART 1
F2 5 0.882145 0.078936 0.216113 10.59000 0.11062
F3 5 0.818198 -0.049821 0.266228 10.63000 0.12920
PART 0
PART 2
F4 5 0.854026 0.063549 0.301713 10.41000 0.15407
PART 0
PART 1
F5 5 0.885689 -0.039906 0.163841 10.70000 0.15771
PART 0
PART 2
F0AA 5 0.798215 -0.005610 0.286613 10.37000 0.08681
F6 5 0.905514 0.045596 0.180315 10.30000 0.07669
PART 0
F7 5 0.949026 -0.000893 0.301824 10.39000 0.06987
HKLF 4
REM str1816 in P212121 #19
REM wR2 = 0.1142, GooF = S = 1.057, Restrained GooF = 1.057 for all data
REM R1 = 0.0425 for 5728 Fo > 4sig(Fo) and 0.0464 for all 6074 data
REM 423 parameters refined using 0 restraints
END
WGHT 0.0614 3.5927
REM Highest difference peak 0.523, deepest hole -0.418, 1-sigma level 0.060
Q1 1 0.3904 0.0796 0.2514 11.00000 0.05 0.52
Q2 1 0.8466 -0.0909 0.2861 11.00000 0.05 0.52
Q3 1 0.8981 -0.0327 0.2384 11.00000 0.05 0.48
Q4 1 0.3630 0.1918 0.1634 11.00000 0.05 0.45
Q5 1 0.9062 -0.0026 0.1686 11.00000 0.05 0.44
Q6 1 0.8108 -0.0386 0.2170 11.00000 0.05 0.43
Q7 1 0.7994 0.0407 0.3113 11.00000 0.05 0.42
Q8 1 0.9213 0.0440 0.3307 11.00000 0.05 0.42
Q9 1 0.8773 0.0438 0.2710 11.00000 0.05 0.37
Q10 1 0.4746 0.0875 0.0563 11.00000 0.05 0.34
Q11 1 0.9824 -0.0809 0.2611 11.00000 0.05 0.33
Q12 1 0.5846 0.1239 0.2409 11.00000 0.05 0.30
Q13 1 0.2611 0.2404 0.3154 11.00000 0.05 0.29
Q14 1 0.9907 -0.0635 0.2406 11.00000 0.05 0.29
Q15 1 0.3682 0.1891 0.2542 11.00000 0.05 0.28
Q16 1 0.9600 -0.0153 0.2797 11.00000 0.05 0.27
Q17 1 0.3829 0.0578 0.0393 11.00000 0.05 0.26
Q18 1 0.3551 -0.0344 0.2366 11.00000 0.05 0.24
Q19 1 0.3167 0.0953 0.1992 11.00000 0.05 0.23
Q20 1 0.9013 0.0672 0.1985 11.00000 0.05 0.23
;
_shelx_res_checksum 7958
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-19 4 8 0.0730 -19.0000 4.0000 8.0000 -0.9934 0.0313 -0.0349
19 -4 -8 0.0730 19.0000 -4.0000 -8.0000 0.9934 -0.0313 0.0349
-17 12 -7 0.1137 -17.0000 12.0000 -7.0000 -0.7372 0.0091 0.6898
17 -12 7 0.1137 17.0000 -12.0000 7.0000 0.7372 -0.0091 -0.6898
0 24 -2 0.0925 -0.0000 24.0000 -2.0000 -0.1836 -0.7995 0.5954
-1 -24 -2 0.1424 -1.0000 -24.0000 -2.0000 0.2042 0.8945 -0.4335
-5 -3 -21 0.1877 -5.0000 -3.0000 -21.0000 0.1461 0.5991 0.7825
5 5 21 0.1278 5.0000 5.0000 21.0000 -0.1641 -0.6690 -0.7392
4 -12 18 0.1708 4.0000 -12.0000 18.0000 -0.0067 0.0004 -0.9832
3 21 11 0.1161 3.0000 21.0000 11.0000 -0.2345 -0.9991 0.0068
-2 -23 -6 0.1380 -2.0000 -23.0000 -6.0000 0.2158 0.9545 -0.2500
-2 21 -10 0.1155 -2.0000 21.0000 -10.0000 -0.1154 -0.5048 0.8542
-17 -11 6 0.1002 -17.0000 -11.0000 6.0000 -0.7392 0.5598 -0.3025
-20 -6 -2 0.1156 -20.0000 -6.0000 -2.0000 -0.7866 0.5923 0.1390
15 14 -7 0.0816 15.0000 14.0000 -7.0000 0.6410 -0.6108 0.4248
18 1 11 0.0911 18.0000 1.0000 11.0000 0.5997 -0.5582 -0.5704
19 6 6 0.0772 19.0000 6.0000 6.0000 0.6787 -0.6529 -0.2816
11 16 -12 0.1008 11.0000 16.0000 -12.0000 0.5288 -0.5147 0.6969
20 -2 -7 0.0631 20.0000 -2.0000 -7.0000 1.0030 -0.1378 0.0304
17 2 -12 0.0745 17.0000 2.0000 -12.0000 0.9165 -0.1287 0.3362
16 -10 -11 0.0881 16.0000 -10.0000 -11.0000 0.9646 0.2882 0.0481
17 -14 -3 0.1017 17.0000 -14.0000 -3.0000 0.9157 0.2552 -0.3525
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CD2Cl2'
#######################################################################
#
# 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_str1832
_database_code_depnum_ccdc_archive 'CCDC 1952457'
loop_
_audit_author_name
_audit_author_address
'Marta Feliz'
;Instituto de Tecnologia Quimica
Spain
;
_audit_update_record
;
2019-09-09 deposited with the CCDC. 2020-03-20 downloaded from the CCDC.
;
_audit_creation_date 2019-08-21
_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 cappa-[FeI{(R,R)-Me-DuPhos}2]I2\^A.H2O
_chemical_formula_moiety 'C36 H56 Fe I P4, I, H2 O'
_chemical_formula_sum 'C36 H58 Fe I2 O P4'
_chemical_formula_weight 940.35
_chemical_absolute_configuration .
_chemical_melting_point ?
_chemical_oxdiff_formula 'C H I Fe P'
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'
I I -0.4742 1.8119 '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'
P P 0.1023 0.0942 '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 4
_space_group_name_H-M_alt 'P 1 21 1'
_space_group_name_Hall 'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 11.3411(3)
_cell_length_b 20.8867(4)
_cell_length_c 17.3185(3)
_cell_angle_alpha 90
_cell_angle_beta 103.587(2)
_cell_angle_gamma 90
_cell_volume 3987.58(14)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 33222
_cell_measurement_temperature 200.00(10)
_cell_measurement_theta_max 28.9840
_cell_measurement_theta_min 3.5150
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.114
_exptl_absorpt_correction_T_max 0.957
_exptl_absorpt_correction_T_min 0.861
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'dull light red'
_exptl_crystal_colour_lustre dull
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.566
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1896
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -4 23 0.0378
16 -2 -6 0.1358
-16 2 4 0.0782
0 4 -23 0.0226
8 -17 -18 0.0763
-15 0 13 0.0647
0 13 21 0.0257
-13 -10 -7 0.0697
-2 25 -12 0.0282
1 -16 20 0.0504
_exptl_crystal_size_max 0.241
_exptl_crystal_size_mid 0.162
_exptl_crystal_size_min 0.064
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0000 -4.0001 23.0000 -0.9150 0.3157 0.2328
16.0000 -2.0000 -6.0000 -0.2719 0.1124 -0.9588
-16.0000 2.0000 4.0000 0.3509 -0.1277 0.9337
0.0000 4.0001 -23.0000 0.8824 -0.3100 -0.2880
8.0000 -17.0000 -18.0000 0.5583 0.4747 -0.6729
-15.0000 -0.0000 13.0000 -0.0242 0.0138 0.9911
-0.0000 12.9999 21.0000 -0.9119 -0.2724 0.2680
-13.0000 -10.0000 -7.0000 0.7639 0.2053 0.6262
-2.0000 25.0001 -12.0000 0.3793 -0.9375 -0.0330
1.0000 -16.0001 20.0000 -0.7199 0.6930 0.1914
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0362
_diffrn_reflns_av_unetI/netI 0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 70382
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 24.000
_diffrn_reflns_theta_max 24.000
_diffrn_reflns_theta_min 2.850
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 200.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -41.00 62.60 0.70 20.00 -- -11.13 57.00 120.00 148
2 \w -20.00 29.70 0.70 20.00 -- -11.13 -99.00-150.00 71
3 \w -20.00 29.70 0.70 20.00 -- -11.13 -99.00 -90.00 71
4 \w -14.00 87.50 0.70 20.00 -- 12.06 37.00-180.00 145
5 \w -64.00 37.50 0.70 20.00 -- 12.06 -37.00 0.00 145
6 \w -18.00 85.60 0.70 20.00 -- 12.06 57.00 90.00 148
7 \w -67.00 45.00 0.70 20.00 -- 12.06 -77.00 -30.00 160
8 \w -41.00 62.60 0.70 20.00 -- -11.13 57.00-180.00 148
9 \w -20.00 29.70 0.70 20.00 -- -11.13 -99.00-180.00 71
10 \w -70.00 -44.10 0.70 20.00 -- -11.13 127.00-179.45 37
11 \w -100.00 -55.90 0.70 20.00 -- -11.13 178.00 120.00 63
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0325972000
_diffrn_orient_matrix_UB_12 -0.0063827000
_diffrn_orient_matrix_UB_13 -0.0394738000
_diffrn_orient_matrix_UB_21 0.0057324000
_diffrn_orient_matrix_UB_22 -0.0333565000
_diffrn_orient_matrix_UB_23 0.0076763000
_diffrn_orient_matrix_UB_31 -0.0551745000
_diffrn_orient_matrix_UB_32 0.0003030000
_diffrn_orient_matrix_UB_33 0.0125735000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.941
_reflns_Friedel_fraction_full 0.999
_reflns_Friedel_fraction_max 0.999
_reflns_number_gt 11976
_reflns_number_total 12484
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.518
_refine_diff_density_min -0.528
_refine_diff_density_rms 0.054
_refine_ls_abs_structure_details
;
Flack x determined using 5583 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack -0.025(5)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.025
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 823
_refine_ls_number_reflns 12484
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0235
_refine_ls_R_factor_gt 0.0217
_refine_ls_restrained_S_all 1.025
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+2.0210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0531
_refine_ls_wR_factor_ref 0.0542
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H,H) groups
2. Others
Fixed Sof: I3(0.6) I4(0.805) I5(0.195) I6(0.4)
3.a Free rotating group:
O1(H1A,H1B), O0AA(H0AA,H0AB)
3.b Ternary CH refined with riding coordinates:
C1(H1), C3(H3), C5(H5), C8(H8), C9(H9), C12(H12), C13(H13), C15(H15),
C16(H16), C20(H20), C25(H25), C31(H31), C29(H29), C39(H39), C51(H51), C57(H57)
3.c Secondary CH2 refined with riding coordinates:
C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B), C34(H34A,H34B), C37(H37A,
H37B), C43(H43A,H43B), C42(H42A,H42B), C45(H45A,H45B), C55(H55A,H55B),
C64(H64A,H64B), C63(H63A,H63B), C62(H62A,H62B), C60(H60A,H60B), C59(H59A,H59B),
C61(H61A,H61B), C66(H66A,H66B)
3.d Aromatic/amide H refined with riding coordinates:
C14(H14), C19(H19), C21(H21), C24(H24), C36(H36), C41(H41), C46(H46),
C47(H47), C48(H48), C53(H53), C54(H54), C58(H58), C68(H68), C69(H69), C71(H71),
C72(H72)
3.e Idealised Me refined as rotating group:
C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C27(H27A,H27B,
H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C38(H38A,H38B,H38C), C40(H40A,
H40B,H40C), C44(H44A,H44B,H44C), C50(H50A,H50B,H50C), C49(H49A,H49B,H49C),
C52(H52A,H52B,H52C), C56(H56A,H56B,H56C), C67(H67A,H67B,H67C), C65(H65A,H65B,
H65C), C70(H70A,H70B,H70C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe -2.42298(5) -0.30956(3) -0.78484(3) 0.01866(13) Uani 1 1 d . . . . .
I1 I -2.48033(4) -0.31031(2) -0.93785(2) 0.04220(10) Uani 1 1 d . . . . .
P1 P -2.54598(11) -0.36310(6) -0.71982(8) 0.0241(3) Uani 1 1 d . . . . .
P2 P -2.25406(11) -0.25675(6) -0.71549(7) 0.0219(3) Uani 1 1 d . . . . .
P3 P -2.34033(12) -0.40830(6) -0.78444(7) 0.0245(3) Uani 1 1 d . . . . .
P4 P -2.50335(11) -0.21001(6) -0.78691(8) 0.0238(3) Uani 1 1 d . . . . .
Fe2 Fe -2.05016(6) -0.30494(3) -0.17550(4) 0.01981(14) Uani 1 1 d . . . . .
I2 I -1.98677(3) -0.31373(2) -0.02230(2) 0.03203(9) Uani 1 1 d . . . . .
P5 P -1.91712(11) -0.27000(6) -0.24729(8) 0.0232(3) Uani 1 1 d . . . . .
P6 P -2.24319(11) -0.33454(6) -0.23761(7) 0.0226(3) Uani 1 1 d . . . . .
P7 P -1.95224(11) -0.39816(6) -0.18349(8) 0.0254(3) Uani 1 1 d . . . . .
P8 P -2.14490(12) -0.21094(6) -0.16414(7) 0.0240(3) Uani 1 1 d . . . . .
I3 I -2.0954(5) -0.0180(3) -0.3559(4) 0.0492(11) Uani 0.6 1 d . . P A 1
I4 I -2.17691(11) -0.58441(5) -0.33838(6) 0.0482(2) Uani 0.805 1 d . . P B 1
I5 I -2.1713(5) -0.6003(2) -0.3636(2) 0.0509(11) Uani 0.195 1 d . . P C 2
I6 I -2.0847(7) -0.0174(5) -0.3679(6) 0.0421(11) Uani 0.4 1 d . . P D 2
C1 C -2.1469(4) -0.3056(3) -0.6407(3) 0.0281(11) Uani 1 1 d . . . . .
H1 H -2.139400 -0.346606 -0.666527 0.034 Uiso 1 1 calc R . . . .
C2 C -2.3466(5) -0.4429(2) -0.6888(3) 0.0260(11) Uani 1 1 d . . . . .
C3 C -1.9634(5) -0.2002(2) -0.3136(3) 0.0271(11) Uani 1 1 d . . . . .
H3 H -1.999534 -0.169551 -0.283042 0.032 Uiso 1 1 calc R . . . .
C4 C -2.4501(4) -0.4261(2) -0.6629(3) 0.0245(11) Uani 1 1 d . . . . .
C5 C -2.6077(4) -0.3150(3) -0.6479(3) 0.0356(12) Uani 1 1 d . . . . .
H5 H -2.630504 -0.273528 -0.673658 0.043 Uiso 1 1 calc R . . . .
C6 C -1.8979(4) -0.3385(2) -0.3102(3) 0.0276(11) Uani 1 1 d . . . . .
C7 C -2.3413(6) -0.3730(3) -0.1027(3) 0.0420(14) Uani 1 1 d . . . . .
H7A H -2.267879 -0.396513 -0.082407 0.063 Uiso 1 1 calc GR . . . .
H7B H -2.407703 -0.394048 -0.087680 0.063 Uiso 1 1 calc GR . . . .
H7C H -2.332818 -0.330382 -0.081256 0.063 Uiso 1 1 calc GR . . . .
C8 C -2.3658(5) -0.3697(3) -0.1927(3) 0.0335(12) Uani 1 1 d . . . . .
H8 H -2.436887 -0.341996 -0.209859 0.040 Uiso 1 1 calc R . . . .
C9 C -2.6679(5) -0.1890(3) -0.8073(4) 0.0351(13) Uani 1 1 d . . . . .
H9 H -2.692994 -0.184143 -0.757154 0.042 Uiso 1 1 calc R . . . .
C11 C -2.1833(5) -0.3219(3) -0.5643(3) 0.0356(13) Uani 1 1 d . . . . .
H11A H -2.187571 -0.283311 -0.534850 0.053 Uiso 1 1 calc GR . . . .
H11B H -2.124166 -0.350172 -0.533020 0.053 Uiso 1 1 calc GR . . . .
H11C H -2.261178 -0.342416 -0.576466 0.053 Uiso 1 1 calc GR . . . .
C10 C -2.3155(5) -0.2609(3) -0.2855(3) 0.0296(12) Uani 1 1 d . . . . .
C12 C -1.7966(5) -0.4096(3) -0.1163(3) 0.0359(13) Uani 1 1 d . . . . .
H12 H -1.779868 -0.374316 -0.078003 0.043 Uiso 1 1 calc R . . . .
C13 C -2.0064(5) -0.4802(2) -0.1659(4) 0.0352(13) Uani 1 1 d . . . . .
H13 H -2.047523 -0.499475 -0.216636 0.042 Uiso 1 1 calc R . . . .
C14 C -2.2958(6) -0.1169(3) -0.5554(4) 0.0509(17) Uani 1 1 d . . . . .
H14 H -2.249647 -0.096830 -0.510444 0.061 Uiso 1 1 calc R . . . .
C15 C -1.7558(5) -0.2404(3) -0.2097(3) 0.0339(12) Uani 1 1 d . . . . .
H15 H -1.705239 -0.266787 -0.235887 0.041 Uiso 1 1 calc R . . . .
C16 C -2.2599(5) -0.3974(2) -0.3154(3) 0.0279(11) Uani 1 1 d . . . . .
H16 H -2.198865 -0.429849 -0.293452 0.033 Uiso 1 1 calc R . . . .
C17 C -1.9419(6) -0.1371(3) -0.0912(4) 0.0447(15) Uani 1 1 d . . . . .
H17A H -1.943098 -0.160767 -0.043879 0.067 Uiso 1 1 calc GR . . . .
H17B H -1.909324 -0.095199 -0.077135 0.067 Uiso 1 1 calc GR . . . .
H17C H -1.892263 -0.159179 -0.120576 0.067 Uiso 1 1 calc GR . . . .
C18 C -2.4323(5) -0.1745(2) -0.6916(3) 0.0280(11) Uani 1 1 d . . . . .
C22 C -1.9234(4) -0.3990(2) -0.2831(3) 0.0278(11) Uani 1 1 d . . . . .
C19 C -2.2638(5) -0.4868(3) -0.6463(3) 0.0359(13) Uani 1 1 d . . . . .
H19 H -2.195093 -0.498054 -0.663794 0.043 Uiso 1 1 calc R . . . .
C20 C -2.4211(6) -0.4703(3) -0.8580(4) 0.0402(14) Uani 1 1 d . . . . .
H20 H -2.485267 -0.449039 -0.897471 0.048 Uiso 1 1 calc R . . . .
C21 C -2.3887(5) -0.4993(3) -0.5528(3) 0.0397(14) Uani 1 1 d . . . . .
H21 H -2.402658 -0.518346 -0.507210 0.048 Uiso 1 1 calc R . . . .
C23 C -2.2619(5) -0.2026(2) -0.2556(3) 0.0282(11) Uani 1 1 d . . . . .
C25 C -2.1873(5) -0.4269(3) -0.8004(3) 0.0338(13) Uani 1 1 d . . . . .
H25 H -2.128019 -0.428963 -0.749154 0.041 Uiso 1 1 calc R . . . .
C24 C -1.8614(5) -0.3344(3) -0.3819(3) 0.0382(13) Uani 1 1 d . . . . .
H24 H -1.840193 -0.294974 -0.399487 0.046 Uiso 1 1 calc R . . . .
C27 C -2.2348(5) -0.3783(3) -0.3950(3) 0.0354(13) Uani 1 1 d . . . . .
H27A H -2.291488 -0.345842 -0.419303 0.053 Uiso 1 1 calc GR . . . .
H27B H -2.243494 -0.415042 -0.429103 0.053 Uiso 1 1 calc GR . . . .
H27C H -2.153733 -0.361884 -0.386673 0.053 Uiso 1 1 calc GR . . . .
C26 C -2.3117(4) -0.1933(2) -0.6609(3) 0.0248(11) Uani 1 1 d . . . . .
C28 C -2.0909(6) -0.4804(3) -0.1094(4) 0.0445(15) Uani 1 1 d . . . . .
H28A H -2.048702 -0.463995 -0.058623 0.067 Uiso 1 1 calc GR . . . .
H28B H -2.117186 -0.523408 -0.103209 0.067 Uiso 1 1 calc GR . . . .
H28C H -2.160185 -0.453982 -0.130659 0.067 Uiso 1 1 calc GR . . . .
C32 C -1.8459(5) -0.1693(3) -0.3239(3) 0.0354(13) Uani 1 1 d . . . . .
H32A H -1.815166 -0.191974 -0.363968 0.042 Uiso 1 1 calc R . . . .
H32B H -1.860343 -0.125035 -0.340515 0.042 Uiso 1 1 calc R . . . .
C31 C -2.2350(5) -0.2029(3) -0.0854(3) 0.0323(12) Uani 1 1 d . . . . .
H31 H -2.216379 -0.239719 -0.049475 0.039 Uiso 1 1 calc R . . . .
C29 C -2.1283(5) -0.2140(3) -0.7498(4) 0.0362(13) Uani 1 1 d . . . . .
H29 H -2.120912 -0.171580 -0.724888 0.043 Uiso 1 1 calc R . . . .
C33 C -2.3830(5) -0.4296(3) -0.3194(3) 0.0366(13) Uani 1 1 d . . . . .
H33A H -2.447923 -0.404435 -0.351930 0.044 Uiso 1 1 calc R . . . .
H33B H -2.384499 -0.471981 -0.342606 0.044 Uiso 1 1 calc R . . . .
C30 C -2.5236(5) -0.3000(3) -0.5683(3) 0.0446(15) Uani 1 1 d . . . . .
H30A H -2.506551 -0.338568 -0.537540 0.067 Uiso 1 1 calc GR . . . .
H30B H -2.561775 -0.269560 -0.540400 0.067 Uiso 1 1 calc GR . . . .
H30C H -2.449301 -0.282317 -0.576310 0.067 Uiso 1 1 calc GR . . . .
C35 C -2.3993(5) -0.4343(3) -0.2355(4) 0.0408(14) Uani 1 1 d . . . . .
H35A H -2.347672 -0.467853 -0.207115 0.049 Uiso 1 1 calc R . . . .
H35B H -2.482817 -0.444933 -0.236401 0.049 Uiso 1 1 calc R . . . .
C39 C -2.0705(5) -0.1313(3) -0.1422(3) 0.0337(13) Uani 1 1 d . . . . .
H39 H -2.069692 -0.108974 -0.191857 0.040 Uiso 1 1 calc R . . . .
C34 C -2.6758(6) -0.1243(3) -0.8501(4) 0.0527(18) Uani 1 1 d . . . . .
H34A H -2.758732 -0.115763 -0.878556 0.063 Uiso 1 1 calc R . . . .
H34B H -2.649271 -0.090096 -0.812139 0.063 Uiso 1 1 calc R . . . .
C36 C -2.2440(5) -0.1628(3) -0.5939(3) 0.0380(13) Uani 1 1 d . . . . .
H36 H -2.162708 -0.173464 -0.574874 0.046 Uiso 1 1 calc R . . . .
C38 C -2.1460(6) -0.3782(3) -0.8545(4) 0.0450(15) Uani 1 1 d . . . . .
H38A H -2.201677 -0.378347 -0.905648 0.068 Uiso 1 1 calc GR . . . .
H38B H -2.066399 -0.389371 -0.860292 0.068 Uiso 1 1 calc GR . . . .
H38C H -2.143867 -0.336275 -0.831445 0.068 Uiso 1 1 calc GR . . . .
C37 C -2.0228(5) -0.2724(3) -0.6297(4) 0.0415(14) Uani 1 1 d . . . . .
H37A H -2.017552 -0.236098 -0.594153 0.050 Uiso 1 1 calc R . . . .
H37B H -1.957920 -0.302074 -0.607357 0.050 Uiso 1 1 calc R . . . .
C40 C -2.0592(5) -0.2120(3) -0.3903(3) 0.0356(13) Uani 1 1 d . . . . .
H40A H -2.027320 -0.240544 -0.423754 0.053 Uiso 1 1 calc GR . . . .
H40B H -2.080741 -0.172044 -0.417385 0.053 Uiso 1 1 calc GR . . . .
H40C H -2.129892 -0.230721 -0.377965 0.053 Uiso 1 1 calc GR . . . .
C43 C -2.1520(6) -0.0950(3) -0.0970(4) 0.0426(14) Uani 1 1 d . . . . .
H43A H -2.109016 -0.058679 -0.068841 0.051 Uiso 1 1 calc R . . . .
H43B H -2.224689 -0.079614 -0.133738 0.051 Uiso 1 1 calc R . . . .
C41 C -2.4842(5) -0.1281(3) -0.6524(4) 0.0438(15) Uani 1 1 d . . . . .
H41 H -2.564276 -0.115551 -0.672497 0.053 Uiso 1 1 calc R . . . .
C42 C -1.8901(6) -0.5173(3) -0.1304(4) 0.0459(15) Uani 1 1 d . . . . .
H42A H -1.908350 -0.555392 -0.103364 0.055 Uiso 1 1 calc R . . . .
H42B H -1.850457 -0.530104 -0.171828 0.055 Uiso 1 1 calc R . . . .
C44 C -2.3722(5) -0.1990(3) -0.1162(4) 0.0419(14) Uani 1 1 d . . . . .
H44A H -2.393023 -0.159716 -0.144917 0.063 Uiso 1 1 calc GR . . . .
H44B H -2.410361 -0.200348 -0.072280 0.063 Uiso 1 1 calc GR . . . .
H44C H -2.399770 -0.234574 -0.150929 0.063 Uiso 1 1 calc GR . . . .
C45 C -2.1847(6) -0.1424(3) -0.0389(3) 0.0421(14) Uani 1 1 d . . . . .
H45A H -2.245162 -0.124026 -0.014072 0.051 Uiso 1 1 calc R . . . .
H45B H -2.113402 -0.152867 0.002360 0.051 Uiso 1 1 calc R . . . .
C46 C -2.4200(5) -0.2599(3) -0.3477(4) 0.0444(15) Uani 1 1 d . . . . .
H46 H -2.458650 -0.298017 -0.366676 0.053 Uiso 1 1 calc R . . . .
C47 C -1.9167(6) -0.4533(3) -0.3281(4) 0.0409(14) Uani 1 1 d . . . . .
H47 H -1.932510 -0.493415 -0.309664 0.049 Uiso 1 1 calc R . . . .
C48 C -1.8568(6) -0.3882(3) -0.4262(4) 0.0484(16) Uani 1 1 d . . . . .
H48 H -1.833599 -0.384845 -0.474134 0.058 Uiso 1 1 calc R . . . .
C50 C -2.7483(5) -0.2377(3) -0.8598(4) 0.0426(14) Uani 1 1 d . . . . .
H50A H -2.734668 -0.235792 -0.912419 0.064 Uiso 1 1 calc GR . . . .
H50B H -2.831803 -0.228307 -0.861868 0.064 Uiso 1 1 calc GR . . . .
H50C H -2.729118 -0.279837 -0.838355 0.064 Uiso 1 1 calc GR . . . .
C51 C -2.6942(5) -0.4059(3) -0.7612(4) 0.0428(15) Uani 1 1 d . . . . .
H51 H -2.686023 -0.448373 -0.736470 0.051 Uiso 1 1 calc R . . . .
C49 C -2.1443(7) -0.2025(3) -0.8382(4) 0.0543(17) Uani 1 1 d . . . . .
H49A H -2.164235 -0.242131 -0.866332 0.081 Uiso 1 1 calc GR . . . .
H49B H -2.070336 -0.185851 -0.848082 0.081 Uiso 1 1 calc GR . . . .
H49C H -2.208650 -0.172227 -0.856219 0.081 Uiso 1 1 calc GR . . . .
C52 C -2.4767(7) -0.5256(3) -0.8217(4) 0.0554(17) Uani 1 1 d . . . . .
H52A H -2.413768 -0.548912 -0.786026 0.083 Uiso 1 1 calc GR . . . .
H52B H -2.518598 -0.553567 -0.863061 0.083 Uiso 1 1 calc GR . . . .
H52C H -2.532951 -0.509076 -0.792940 0.083 Uiso 1 1 calc GR . . . .
C53 C -2.3078(6) -0.1454(3) -0.2903(3) 0.0401(14) Uani 1 1 d . . . . .
H53 H -2.270211 -0.106988 -0.271431 0.048 Uiso 1 1 calc R . . . .
C54 C -2.4723(5) -0.4563(3) -0.5957(3) 0.0359(13) Uani 1 1 d . . . . .
H54 H -2.543312 -0.447515 -0.579692 0.043 Uiso 1 1 calc R . . . .
C56 C -1.7000(5) -0.2453(3) -0.1208(4) 0.0427(14) Uani 1 1 d . . . . .
H56A H -1.759800 -0.234253 -0.091952 0.064 Uiso 1 1 calc GR . . . .
H56B H -1.632589 -0.216401 -0.106640 0.064 Uiso 1 1 calc GR . . . .
H56C H -1.672567 -0.288314 -0.107855 0.064 Uiso 1 1 calc GR . . . .
C55 C -2.7270(5) -0.3477(4) -0.6435(4) 0.0523(18) Uani 1 1 d . . . . .
H55A H -2.711086 -0.383987 -0.607689 0.063 Uiso 1 1 calc R . . . .
H55B H -2.778942 -0.317836 -0.624097 0.063 Uiso 1 1 calc R . . . .
C57 C -2.4672(5) -0.1502(3) -0.8595(4) 0.0383(14) Uani 1 1 d . . . . .
H57 H -2.424419 -0.171953 -0.894984 0.046 Uiso 1 1 calc R . . . .
C58 C -2.4166(6) -0.1006(3) -0.5835(4) 0.0574(19) Uani 1 1 d . . . . .
H58 H -2.452379 -0.070996 -0.555972 0.069 Uiso 1 1 calc R . . . .
C64 C -1.8082(5) -0.4724(3) -0.0716(4) 0.0451(15) Uani 1 1 d . . . . .
H64A H -1.728966 -0.491701 -0.052090 0.054 Uiso 1 1 calc R . . . .
H64B H -1.843333 -0.463945 -0.026706 0.054 Uiso 1 1 calc R . . . .
C63 C -1.7548(5) -0.1728(3) -0.2438(4) 0.0410(14) Uani 1 1 d . . . . .
H63A H -1.776056 -0.141880 -0.207481 0.049 Uiso 1 1 calc R . . . .
H63B H -1.674240 -0.162639 -0.250239 0.049 Uiso 1 1 calc R . . . .
C62 C -2.0124(5) -0.2506(3) -0.7107(4) 0.0486(16) Uani 1 1 d . . . . .
H62A H -2.002515 -0.287230 -0.742924 0.058 Uiso 1 1 calc R . . . .
H62B H -1.942277 -0.222964 -0.705846 0.058 Uiso 1 1 calc R . . . .
C60 C -2.2021(7) -0.4935(3) -0.8396(4) 0.0558(18) Uani 1 1 d . . . . .
H60A H -2.136413 -0.501651 -0.865483 0.067 Uiso 1 1 calc R . . . .
H60B H -2.201017 -0.526442 -0.800014 0.067 Uiso 1 1 calc R . . . .
C59 C -2.7878(5) -0.3696(4) -0.7264(4) 0.0545(18) Uani 1 1 d . . . . .
H59A H -2.818376 -0.332933 -0.759453 0.065 Uiso 1 1 calc R . . . .
H59B H -2.855651 -0.397421 -0.724720 0.065 Uiso 1 1 calc R . . . .
C61 C -2.3217(7) -0.4935(3) -0.8995(4) 0.0584(19) Uani 1 1 d . . . . .
H61A H -2.340400 -0.536345 -0.920505 0.070 Uiso 1 1 calc R . . . .
H61B H -2.317963 -0.465228 -0.943339 0.070 Uiso 1 1 calc R . . . .
C68 C -2.2852(5) -0.5136(3) -0.5776(3) 0.0413(14) Uani 1 1 d . . . . .
H68 H -2.228712 -0.541719 -0.547849 0.050 Uiso 1 1 calc R . . . .
C67 C -2.7337(6) -0.4171(3) -0.8502(4) 0.0538(18) Uani 1 1 d . . . . .
H67A H -2.735473 -0.377066 -0.877556 0.081 Uiso 1 1 calc GR . . . .
H67B H -2.813244 -0.435893 -0.862876 0.081 Uiso 1 1 calc GR . . . .
H67C H -2.677503 -0.445576 -0.866324 0.081 Uiso 1 1 calc GR . . . .
C65 C -2.3913(6) -0.0924(3) -0.8209(4) 0.0545(17) Uani 1 1 d . . . . .
H65A H -2.434917 -0.069356 -0.788555 0.082 Uiso 1 1 calc GR . . . .
H65B H -2.376009 -0.064629 -0.861684 0.082 Uiso 1 1 calc GR . . . .
H65C H -2.315536 -0.107198 -0.788534 0.082 Uiso 1 1 calc GR . . . .
C66 C -2.5935(7) -0.1284(3) -0.9080(4) 0.0555(18) Uani 1 1 d . . . . .
H66A H -2.587762 -0.087017 -0.932141 0.067 Uiso 1 1 calc R . . . .
H66B H -2.625567 -0.159088 -0.949695 0.067 Uiso 1 1 calc R . . . .
C70 C -1.6927(5) -0.4144(3) -0.1588(4) 0.0480(16) Uani 1 1 d . . . . .
H70A H -1.702844 -0.452239 -0.191132 0.072 Uiso 1 1 calc GR . . . .
H70B H -1.616707 -0.416604 -0.120082 0.072 Uiso 1 1 calc GR . . . .
H70C H -1.693285 -0.377371 -0.191688 0.072 Uiso 1 1 calc GR . . . .
C69 C -1.8862(6) -0.4473(3) -0.4007(4) 0.0502(17) Uani 1 1 d . . . . .
H69 H -1.885685 -0.483224 -0.432324 0.060 Uiso 1 1 calc R . . . .
C71 C -2.4096(7) -0.1449(3) -0.3531(4) 0.0567(18) Uani 1 1 d . . . . .
H71 H -2.439895 -0.106381 -0.376383 0.068 Uiso 1 1 calc R . . . .
C72 C -2.4657(7) -0.2017(4) -0.3808(4) 0.060(2) Uani 1 1 d . . . . .
H72 H -2.534833 -0.201111 -0.422221 0.072 Uiso 1 1 calc R . . . .
O1 O -1.9678(7) -0.1113(4) -0.5094(5) 0.112(2) Uiso 1 1 d . . . . .
H1A H -2.012291 -0.086481 -0.489596 0.168 Uiso 1 1 d G . . . .
H1B H -1.966205 -0.098348 -0.555674 0.168 Uiso 1 1 d G . . . .
O0AA O -1.7616(8) -0.1992(5) -0.5059(6) 0.132(3) Uiso 1 1 d . . . . .
H0AA H -1.738857 -0.171943 -0.535799 0.198 Uiso 1 1 d G . . . .
H0AB H -1.837511 -0.195622 -0.510171 0.198 Uiso 1 1 d G . . . .
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 0.0215(3) 0.0168(3) 0.0171(3) -0.0007(3) 0.0034(2) 0.0022(3)
I1 0.0701(3) 0.03524(19) 0.01839(16) 0.00013(17) 0.00475(16) 0.0136(2)
P1 0.0182(6) 0.0249(7) 0.0281(7) 0.0022(5) 0.0032(5) -0.0001(5)
P2 0.0198(6) 0.0223(6) 0.0243(7) -0.0005(5) 0.0064(5) 0.0010(5)
P3 0.0315(7) 0.0182(6) 0.0237(7) -0.0005(5) 0.0060(5) 0.0055(5)
P4 0.0236(7) 0.0187(6) 0.0262(7) -0.0020(5) -0.0001(5) 0.0045(5)
Fe2 0.0199(3) 0.0195(3) 0.0197(3) 0.0013(3) 0.0040(2) 0.0000(3)
I2 0.03383(18) 0.03880(19) 0.02102(15) 0.00344(16) 0.00156(13) 0.00111(16)
P5 0.0218(6) 0.0227(7) 0.0251(7) 0.0011(5) 0.0053(5) -0.0023(5)
P6 0.0205(6) 0.0235(6) 0.0241(6) -0.0012(5) 0.0055(5) 0.0001(5)
P7 0.0235(7) 0.0221(7) 0.0306(7) 0.0039(5) 0.0064(5) 0.0030(5)
P8 0.0295(7) 0.0212(6) 0.0215(6) -0.0003(5) 0.0062(5) 0.0012(5)
I3 0.0544(15) 0.0384(9) 0.056(2) -0.0053(10) 0.0155(9) -0.0027(8)
I4 0.0476(4) 0.0478(5) 0.0529(6) -0.0055(4) 0.0192(4) -0.0106(4)
I5 0.0610(18) 0.054(3) 0.039(2) 0.0052(16) 0.0127(17) 0.0063(17)
I6 0.0356(12) 0.0478(15) 0.0421(18) -0.0142(14) 0.0074(16) -0.0033(10)
C1 0.020(2) 0.032(3) 0.030(3) -0.002(3) 0.0009(19) 0.005(2)
C2 0.029(3) 0.023(3) 0.025(3) 0.001(2) 0.003(2) 0.001(2)
C3 0.032(3) 0.022(3) 0.027(3) 0.001(2) 0.007(2) 0.001(2)
C4 0.023(3) 0.023(3) 0.025(3) 0.004(2) 0.000(2) -0.002(2)
C5 0.026(3) 0.045(3) 0.040(3) 0.005(3) 0.016(2) 0.009(3)
C6 0.026(3) 0.027(3) 0.032(3) 0.000(2) 0.011(2) 0.003(2)
C7 0.046(4) 0.044(4) 0.044(3) 0.001(3) 0.027(3) -0.007(3)
C8 0.026(3) 0.039(3) 0.039(3) 0.000(3) 0.014(2) -0.004(2)
C9 0.028(3) 0.030(3) 0.042(3) -0.006(3) -0.003(2) 0.011(2)
C11 0.031(3) 0.043(4) 0.029(3) 0.002(3) 0.000(2) 0.002(3)
C10 0.026(3) 0.032(3) 0.028(3) -0.002(2) 0.001(2) 0.009(2)
C12 0.026(3) 0.036(3) 0.042(3) 0.002(3) 0.000(2) 0.007(2)
C13 0.042(3) 0.019(3) 0.043(3) 0.003(2) 0.006(3) -0.001(2)
C14 0.054(4) 0.046(4) 0.042(4) -0.026(3) -0.009(3) 0.007(3)
C15 0.025(3) 0.036(3) 0.041(3) 0.000(3) 0.009(2) -0.007(2)
C16 0.025(3) 0.028(3) 0.030(3) -0.007(2) 0.004(2) -0.002(2)
C17 0.051(4) 0.030(3) 0.052(4) -0.005(3) 0.010(3) -0.017(3)
C18 0.026(3) 0.026(3) 0.029(3) -0.008(2) 0.001(2) 0.002(2)
C22 0.024(3) 0.027(3) 0.032(3) 0.001(2) 0.006(2) 0.003(2)
C19 0.037(3) 0.030(3) 0.039(3) 0.009(3) 0.007(3) 0.007(2)
C20 0.053(4) 0.026(3) 0.036(3) -0.008(2) -0.001(3) 0.001(3)
C21 0.045(4) 0.038(3) 0.034(3) 0.015(3) 0.007(3) -0.005(3)
C23 0.033(3) 0.027(3) 0.024(3) 0.000(2) 0.006(2) 0.011(2)
C25 0.039(3) 0.031(3) 0.036(3) -0.002(2) 0.016(3) 0.014(2)
C24 0.042(3) 0.036(3) 0.041(3) 0.001(3) 0.019(3) 0.003(3)
C27 0.036(3) 0.042(3) 0.027(3) -0.009(2) 0.004(2) -0.006(3)
C26 0.023(3) 0.023(3) 0.027(3) -0.006(2) 0.004(2) 0.002(2)
C28 0.042(3) 0.036(3) 0.059(4) 0.012(3) 0.018(3) -0.006(3)
C32 0.042(3) 0.029(3) 0.037(3) 0.002(2) 0.014(3) -0.009(3)
C31 0.042(3) 0.029(3) 0.029(3) -0.002(2) 0.015(2) 0.005(2)
C29 0.032(3) 0.032(3) 0.050(4) -0.001(3) 0.019(3) -0.008(3)
C33 0.031(3) 0.032(3) 0.046(3) -0.014(3) 0.008(3) -0.009(2)
C30 0.046(3) 0.056(4) 0.037(3) -0.007(3) 0.022(3) 0.005(3)
C35 0.032(3) 0.039(3) 0.055(4) -0.009(3) 0.017(3) -0.011(3)
C39 0.047(3) 0.023(3) 0.032(3) -0.001(2) 0.011(3) -0.003(2)
C34 0.043(4) 0.031(3) 0.070(5) 0.001(3) -0.015(3) 0.016(3)
C36 0.030(3) 0.042(3) 0.035(3) -0.011(3) -0.007(2) 0.006(3)
C38 0.045(4) 0.051(4) 0.047(4) 0.005(3) 0.028(3) 0.013(3)
C37 0.018(3) 0.052(4) 0.051(4) 0.003(3) 0.003(2) 0.003(3)
C40 0.042(3) 0.035(3) 0.028(3) 0.004(2) 0.005(2) -0.002(3)
C43 0.059(4) 0.026(3) 0.043(3) -0.014(3) 0.014(3) 0.001(3)
C41 0.033(3) 0.042(4) 0.051(4) -0.017(3) 0.000(3) 0.016(3)
C42 0.054(4) 0.025(3) 0.062(4) 0.011(3) 0.019(3) 0.010(3)
C44 0.036(3) 0.047(4) 0.048(4) -0.003(3) 0.019(3) 0.010(3)
C45 0.054(4) 0.041(3) 0.035(3) -0.013(3) 0.017(3) -0.002(3)
C46 0.040(3) 0.043(4) 0.040(3) -0.005(3) -0.011(3) 0.013(3)
C47 0.051(4) 0.027(3) 0.049(4) -0.004(3) 0.020(3) 0.003(3)
C48 0.059(4) 0.052(4) 0.043(4) 0.001(3) 0.030(3) 0.007(3)
C50 0.028(3) 0.042(4) 0.051(4) 0.000(3) -0.005(3) 0.007(3)
C51 0.025(3) 0.034(3) 0.062(4) 0.007(3) -0.005(3) -0.008(3)
C49 0.064(4) 0.048(4) 0.059(4) 0.015(3) 0.029(4) 0.001(3)
C52 0.069(4) 0.026(3) 0.061(4) -0.008(3) -0.007(3) -0.006(3)
C53 0.057(4) 0.026(3) 0.035(3) 0.003(2) 0.007(3) 0.011(3)
C54 0.032(3) 0.038(3) 0.038(3) 0.009(3) 0.010(3) -0.006(3)
C56 0.027(3) 0.048(4) 0.046(4) 0.001(3) -0.006(3) -0.012(3)
C55 0.026(3) 0.075(5) 0.063(4) 0.015(4) 0.026(3) 0.008(3)
C57 0.047(4) 0.019(3) 0.045(4) 0.011(2) 0.006(3) -0.001(2)
C58 0.056(4) 0.056(4) 0.055(4) -0.036(4) 0.003(3) 0.017(3)
C64 0.037(3) 0.044(4) 0.051(4) 0.015(3) 0.004(3) 0.017(3)
C63 0.035(3) 0.036(3) 0.052(4) -0.001(3) 0.010(3) -0.015(3)
C62 0.025(3) 0.059(4) 0.066(4) 0.000(3) 0.018(3) -0.004(3)
C60 0.078(5) 0.036(4) 0.056(4) -0.010(3) 0.021(4) 0.023(3)
C59 0.023(3) 0.066(4) 0.072(5) 0.023(4) 0.006(3) -0.004(3)
C61 0.084(5) 0.044(4) 0.048(4) -0.023(3) 0.017(4) 0.001(4)
C68 0.047(4) 0.034(3) 0.036(3) 0.013(3) -0.004(3) 0.007(3)
C67 0.038(4) 0.039(4) 0.069(5) -0.008(3) -0.018(3) -0.006(3)
C65 0.059(4) 0.034(3) 0.069(5) 0.009(3) 0.011(3) -0.006(3)
C66 0.069(5) 0.032(3) 0.053(4) 0.016(3) -0.010(3) 0.003(3)
C70 0.029(3) 0.049(4) 0.064(4) 0.006(3) 0.008(3) 0.010(3)
C69 0.067(4) 0.035(3) 0.056(4) -0.016(3) 0.030(4) 0.000(3)
C71 0.073(5) 0.045(4) 0.042(4) 0.003(3) -0.007(3) 0.023(4)
C72 0.063(5) 0.057(5) 0.045(4) -0.002(3) -0.018(3) 0.026(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 I1 2.5760(6) . ?
Fe1 P1 2.2810(14) . ?
Fe1 P2 2.2909(14) . ?
Fe1 P3 2.2648(14) . ?
Fe1 P4 2.2673(14) . ?
P1 C4 1.839(5) . ?
P1 C5 1.860(5) . ?
P1 C51 1.890(6) . ?
P2 C1 1.859(5) . ?
P2 C26 1.836(5) . ?
P2 C29 1.894(5) . ?
P3 C2 1.824(5) . ?
P3 C20 1.896(6) . ?
P3 C25 1.861(5) . ?
P4 C9 1.869(5) . ?
P4 C18 1.816(5) . ?
P4 C57 1.885(5) . ?
Fe2 I2 2.5872(7) . ?
Fe2 P5 2.2883(13) . ?
Fe2 P6 2.2859(14) . ?
Fe2 P7 2.2619(14) . ?
Fe2 P8 2.2688(14) . ?
P5 C3 1.853(5) . ?
P5 C6 1.842(5) . ?
P5 C15 1.895(5) . ?
P6 C8 1.894(5) . ?
P6 C10 1.846(5) . ?
P6 C16 1.858(5) . ?
P7 C12 1.888(5) . ?
P7 C13 1.869(5) . ?
P7 C22 1.830(5) . ?
P8 C23 1.819(5) . ?
P8 C31 1.894(5) . ?
P8 C39 1.864(5) . ?
C1 C11 1.514(7) . ?
C1 C37 1.540(7) . ?
C2 C4 1.397(7) . ?
C2 C19 1.392(7) . ?
C3 C32 1.529(7) . ?
C3 C40 1.525(7) . ?
C4 C54 1.397(7) . ?
C5 C30 1.514(8) . ?
C5 C55 1.534(8) . ?
C6 C22 1.403(7) . ?
C6 C24 1.400(7) . ?
C7 C8 1.518(8) . ?
C8 C35 1.543(8) . ?
C9 C34 1.534(8) . ?
C9 C50 1.518(8) . ?
C10 C23 1.404(8) . ?
C10 C46 1.402(8) . ?
C12 C64 1.544(8) . ?
C12 C70 1.532(8) . ?
C13 C28 1.522(8) . ?
C13 C42 1.529(8) . ?
C14 C36 1.376(8) . ?
C14 C58 1.384(9) . ?
C15 C56 1.524(8) . ?
C15 C63 1.532(8) . ?
C16 C27 1.525(7) . ?
C16 C33 1.537(7) . ?
C17 C39 1.521(9) . ?
C18 C26 1.401(7) . ?
C18 C41 1.392(7) . ?
C22 C47 1.387(8) . ?
C19 C68 1.388(8) . ?
C20 C52 1.521(9) . ?
C20 C61 1.550(9) . ?
C21 C54 1.388(8) . ?
C21 C68 1.374(8) . ?
C23 C53 1.384(8) . ?
C25 C38 1.529(8) . ?
C25 C60 1.539(8) . ?
C24 C48 1.368(8) . ?
C26 C36 1.386(7) . ?
C32 C63 1.526(8) . ?
C31 C44 1.524(8) . ?
C31 C45 1.535(8) . ?
C29 C49 1.518(9) . ?
C29 C62 1.533(8) . ?
C33 C35 1.511(8) . ?
C39 C43 1.543(7) . ?
C34 C66 1.523(10) . ?
C37 C62 1.505(9) . ?
C43 C45 1.518(8) . ?
C41 C58 1.383(9) . ?
C42 C64 1.527(9) . ?
C46 C72 1.392(9) . ?
C47 C69 1.386(8) . ?
C48 C69 1.377(9) . ?
C51 C59 1.538(9) . ?
C51 C67 1.519(9) . ?
C53 C71 1.388(9) . ?
C55 C59 1.510(10) . ?
C57 C65 1.540(9) . ?
C57 C66 1.549(9) . ?
C60 C61 1.502(10) . ?
C71 C72 1.378(10) . ?
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
P1 Fe1 I1 117.97(4) . . ?
P1 Fe1 P2 120.69(5) . . ?
P2 Fe1 I1 121.34(4) . . ?
P3 Fe1 I1 90.11(4) . . ?
P3 Fe1 P1 81.53(5) . . ?
P3 Fe1 P2 98.19(5) . . ?
P3 Fe1 P4 178.83(5) . . ?
P4 Fe1 I1 89.19(4) . . ?
P4 Fe1 P1 99.63(5) . . ?
P4 Fe1 P2 81.39(5) . . ?
C4 P1 Fe1 105.19(16) . . ?
C4 P1 C5 107.2(2) . . ?
C4 P1 C51 103.1(2) . . ?
C5 P1 Fe1 115.8(2) . . ?
C5 P1 C51 93.9(3) . . ?
C51 P1 Fe1 129.6(2) . . ?
C1 P2 Fe1 115.49(18) . . ?
C1 P2 C29 93.5(2) . . ?
C26 P2 Fe1 105.22(16) . . ?
C26 P2 C1 106.9(2) . . ?
C26 P2 C29 101.9(2) . . ?
C29 P2 Fe1 131.4(2) . . ?
C2 P3 Fe1 105.04(17) . . ?
C2 P3 C20 102.9(3) . . ?
C2 P3 C25 106.8(2) . . ?
C20 P3 Fe1 119.1(2) . . ?
C25 P3 Fe1 126.10(18) . . ?
C25 P3 C20 94.5(3) . . ?
C9 P4 Fe1 126.77(18) . . ?
C9 P4 C57 94.7(3) . . ?
C18 P4 Fe1 105.61(17) . . ?
C18 P4 C9 106.6(2) . . ?
C18 P4 C57 102.4(3) . . ?
C57 P4 Fe1 117.98(19) . . ?
P5 Fe2 I2 121.33(4) . . ?
P6 Fe2 I2 117.91(4) . . ?
P6 Fe2 P5 120.76(5) . . ?
P7 Fe2 I2 88.83(4) . . ?
P7 Fe2 P5 81.11(5) . . ?
P7 Fe2 P6 99.68(5) . . ?
P7 Fe2 P8 178.42(6) . . ?
P8 Fe2 I2 89.75(4) . . ?
P8 Fe2 P5 99.05(5) . . ?
P8 Fe2 P6 81.61(5) . . ?
C3 P5 Fe2 117.42(17) . . ?
C3 P5 C15 93.8(2) . . ?
C6 P5 Fe2 104.98(16) . . ?
C6 P5 C3 107.4(2) . . ?
C6 P5 C15 102.6(2) . . ?
C15 P5 Fe2 128.57(18) . . ?
C8 P6 Fe2 128.74(18) . . ?
C10 P6 Fe2 105.15(17) . . ?
C10 P6 C8 102.5(2) . . ?
C10 P6 C16 107.7(2) . . ?
C16 P6 Fe2 117.10(17) . . ?
C16 P6 C8 93.7(2) . . ?
C12 P7 Fe2 118.23(19) . . ?
C13 P7 Fe2 126.45(18) . . ?
C13 P7 C12 94.5(3) . . ?
C22 P7 Fe2 105.40(17) . . ?
C22 P7 C12 103.4(2) . . ?
C22 P7 C13 106.4(2) . . ?
C23 P8 Fe2 105.69(16) . . ?
C23 P8 C31 102.2(2) . . ?
C23 P8 C39 107.2(3) . . ?
C31 P8 Fe2 119.05(18) . . ?
C39 P8 Fe2 126.10(19) . . ?
C39 P8 C31 94.0(2) . . ?
C11 C1 P2 117.7(3) . . ?
C11 C1 C37 115.0(4) . . ?
C37 C1 P2 105.5(4) . . ?
C4 C2 P3 114.0(4) . . ?
C19 C2 P3 125.2(4) . . ?
C19 C2 C4 120.6(5) . . ?
C32 C3 P5 106.1(4) . . ?
C40 C3 P5 117.0(4) . . ?
C40 C3 C32 115.4(4) . . ?
C2 C4 P1 116.4(4) . . ?
C2 C4 C54 118.9(5) . . ?
C54 C4 P1 124.7(4) . . ?
C30 C5 P1 117.8(4) . . ?
C30 C5 C55 114.9(5) . . ?
C55 C5 P1 105.5(4) . . ?
C22 C6 P5 116.1(4) . . ?
C24 C6 P5 125.3(4) . . ?
C24 C6 C22 118.6(5) . . ?
C7 C8 P6 117.7(4) . . ?
C7 C8 C35 114.7(5) . . ?
C35 C8 P6 105.2(3) . . ?
C34 C9 P4 103.9(4) . . ?
C50 C9 P4 112.8(4) . . ?
C50 C9 C34 110.0(5) . . ?
C23 C10 P6 116.6(4) . . ?
C46 C10 P6 124.3(4) . . ?
C46 C10 C23 119.1(5) . . ?
C64 C12 P7 103.8(4) . . ?
C70 C12 P7 115.2(4) . . ?
C70 C12 C64 110.5(5) . . ?
C28 C13 P7 112.9(4) . . ?
C28 C13 C42 110.7(5) . . ?
C42 C13 P7 104.2(4) . . ?
C36 C14 C58 120.1(6) . . ?
C56 C15 P5 117.6(4) . . ?
C56 C15 C63 114.3(5) . . ?
C63 C15 P5 105.2(4) . . ?
C27 C16 P6 117.5(4) . . ?
C27 C16 C33 115.7(4) . . ?
C33 C16 P6 106.3(3) . . ?
C26 C18 P4 114.6(4) . . ?
C41 C18 P4 125.4(4) . . ?
C41 C18 C26 119.7(5) . . ?
C6 C22 P7 113.8(4) . . ?
C47 C22 P7 125.7(4) . . ?
C47 C22 C6 120.3(5) . . ?
C68 C19 C2 119.2(5) . . ?
C52 C20 P3 115.0(4) . . ?
C52 C20 C61 111.9(5) . . ?
C61 C20 P3 103.6(4) . . ?
C68 C21 C54 120.0(5) . . ?
C10 C23 P8 113.8(4) . . ?
C53 C23 P8 125.7(4) . . ?
C53 C23 C10 120.2(5) . . ?
C38 C25 P3 112.5(4) . . ?
C38 C25 C60 110.3(5) . . ?
C60 C25 P3 104.2(4) . . ?
C48 C24 C6 120.4(5) . . ?
C18 C26 P2 116.1(4) . . ?
C36 C26 P2 124.6(4) . . ?
C36 C26 C18 119.3(5) . . ?
C63 C32 C3 107.2(4) . . ?
C44 C31 P8 115.6(4) . . ?
C44 C31 C45 111.3(5) . . ?
C45 C31 P8 104.7(4) . . ?
C49 C29 P2 118.1(4) . . ?
C49 C29 C62 114.4(5) . . ?
C62 C29 P2 104.8(4) . . ?
C35 C33 C16 107.4(4) . . ?
C33 C35 C8 109.5(5) . . ?
C17 C39 P8 111.9(4) . . ?
C17 C39 C43 110.6(5) . . ?
C43 C39 P8 104.2(4) . . ?
C66 C34 C9 107.0(5) . . ?
C14 C36 C26 120.6(5) . . ?
C62 C37 C1 106.9(5) . . ?
C45 C43 C39 106.6(5) . . ?
C58 C41 C18 119.9(5) . . ?
C64 C42 C13 106.8(5) . . ?
C43 C45 C31 107.9(5) . . ?
C72 C46 C10 119.7(6) . . ?
C69 C47 C22 119.7(5) . . ?
C24 C48 C69 120.7(5) . . ?
C59 C51 P1 104.6(4) . . ?
C67 C51 P1 118.8(4) . . ?
C67 C51 C59 114.0(5) . . ?
C23 C53 C71 120.3(6) . . ?
C21 C54 C4 120.3(5) . . ?
C59 C55 C5 107.4(5) . . ?
C65 C57 P4 114.7(4) . . ?
C65 C57 C66 110.9(5) . . ?
C66 C57 P4 103.7(4) . . ?
C41 C58 C14 120.2(5) . . ?
C42 C64 C12 107.3(5) . . ?
C32 C63 C15 109.3(5) . . ?
C37 C62 C29 108.5(4) . . ?
C61 C60 C25 107.0(5) . . ?
C55 C59 C51 108.6(5) . . ?
C60 C61 C20 108.5(5) . . ?
C21 C68 C19 121.0(5) . . ?
C34 C66 C57 107.0(5) . . ?
C48 C69 C47 120.2(5) . . ?
C72 C71 C53 120.0(6) . . ?
C71 C72 C46 120.8(6) . . ?
_shelx_res_file
;
TITL str1832 in P21 #4
str1832.res
created by SHELXL-2018/3 at 14:04:47 on 21-Aug-2019
REM reset to P21 #4
CELL 0.71073 11.341137 20.886681 17.31852 90 103.5867 90
ZERR 4 0.00025 0.0004 0.000334 0 0.0021 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H Fe I O P
UNIT 144 232 4 8 4 16
L.S. 25
PLAN 20
BOND
fmap 2
acta
OMIT -4 48
REM
REM
REM
WGHT 0.028500 2.021000
FVAR 0.95864
FE1 3 -2.422976 -0.309561 -0.784837 11.00000 0.02146 0.01679 =
0.01713 -0.00068 0.00337 0.00224
I1 4 -2.480326 -0.310309 -0.937849 11.00000 0.07014 0.03524 =
0.01839 0.00013 0.00475 0.01359
P1 6 -2.545981 -0.363103 -0.719815 11.00000 0.01823 0.02493 =
0.02808 0.00218 0.00322 -0.00013
P2 6 -2.254058 -0.256745 -0.715491 11.00000 0.01981 0.02225 =
0.02429 -0.00054 0.00642 0.00097
P3 6 -2.340326 -0.408303 -0.784442 11.00000 0.03146 0.01815 =
0.02366 -0.00050 0.00598 0.00549
P4 6 -2.503350 -0.210008 -0.786906 11.00000 0.02364 0.01869 =
0.02618 -0.00199 -0.00015 0.00451
FE2 3 -2.050158 -0.304940 -0.175499 11.00000 0.01991 0.01949 =
0.01971 0.00134 0.00400 -0.00004
I2 4 -1.986769 -0.313730 -0.022301 11.00000 0.03383 0.03880 =
0.02102 0.00344 0.00156 0.00111
P5 6 -1.917124 -0.269998 -0.247292 11.00000 0.02180 0.02275 =
0.02509 0.00105 0.00532 -0.00231
P6 6 -2.243195 -0.334537 -0.237607 11.00000 0.02047 0.02355 =
0.02409 -0.00125 0.00555 0.00008
P7 6 -1.952238 -0.398164 -0.183491 11.00000 0.02353 0.02212 =
0.03059 0.00389 0.00638 0.00304
P8 6 -2.144903 -0.210937 -0.164142 11.00000 0.02946 0.02117 =
0.02149 -0.00025 0.00623 0.00117
PART 1
I3 4 -2.095415 -0.017967 -0.355883 10.60000 0.05443 0.03845 =
0.05590 -0.00528 0.01555 -0.00265
I4 4 -2.176905 -0.584413 -0.338382 10.80500 0.04757 0.04777 =
0.05293 -0.00546 0.01923 -0.01060
PART 0
PART 2
I5 4 -2.171337 -0.600338 -0.363647 10.19500 0.06095 0.05351 =
0.03876 0.00517 0.01266 0.00628
I6 4 -2.084662 -0.017410 -0.367892 10.40000 0.03558 0.04776 =
0.04209 -0.01419 0.00742 -0.00326
PART 0
C1 1 -2.146945 -0.305577 -0.640659 11.00000 0.01988 0.03184 =
0.03007 -0.00183 0.00090 0.00512
AFIX 13
H1 2 -2.139400 -0.346606 -0.666527 11.00000 -1.20000
AFIX 0
C2 1 -2.346554 -0.442925 -0.688806 11.00000 0.02914 0.02282 =
0.02470 0.00143 0.00338 0.00108
C3 1 -1.963427 -0.200231 -0.313610 11.00000 0.03197 0.02216 =
0.02715 0.00150 0.00718 0.00068
AFIX 13
H3 2 -1.999534 -0.169551 -0.283042 11.00000 -1.20000
AFIX 0
C4 1 -2.450083 -0.426104 -0.662910 11.00000 0.02268 0.02288 =
0.02486 0.00448 -0.00048 -0.00183
C5 1 -2.607693 -0.314972 -0.647944 11.00000 0.02591 0.04524 =
0.03982 0.00453 0.01595 0.00888
AFIX 13
H5 2 -2.630504 -0.273528 -0.673658 11.00000 -1.20000
AFIX 0
C6 1 -1.897908 -0.338494 -0.310216 11.00000 0.02563 0.02714 =
0.03190 0.00022 0.01066 0.00317
C7 1 -2.341295 -0.372956 -0.102739 11.00000 0.04594 0.04367 =
0.04428 0.00058 0.02664 -0.00682
AFIX 137
H7A 2 -2.267879 -0.396513 -0.082407 11.00000 -1.50000
H7B 2 -2.407703 -0.394048 -0.087680 11.00000 -1.50000
H7C 2 -2.332818 -0.330382 -0.081256 11.00000 -1.50000
AFIX 0
C8 1 -2.365781 -0.369674 -0.192661 11.00000 0.02551 0.03912 =
0.03939 -0.00039 0.01445 -0.00365
AFIX 13
H8 2 -2.436887 -0.341996 -0.209859 11.00000 -1.20000
AFIX 0
C9 1 -2.667926 -0.188976 -0.807274 11.00000 0.02771 0.02976 =
0.04243 -0.00640 -0.00274 0.01133
AFIX 13
H9 2 -2.692994 -0.184143 -0.757154 11.00000 -1.20000
AFIX 0
C11 1 -2.183290 -0.321859 -0.564259 11.00000 0.03074 0.04328 =
0.02923 0.00168 -0.00010 0.00215
AFIX 137
H11A 2 -2.187571 -0.283311 -0.534850 11.00000 -1.50000
H11B 2 -2.124166 -0.350172 -0.533020 11.00000 -1.50000
H11C 2 -2.261178 -0.342416 -0.576466 11.00000 -1.50000
AFIX 0
C10 1 -2.315492 -0.260895 -0.285503 11.00000 0.02582 0.03218 =
0.02797 -0.00170 0.00083 0.00932
C12 1 -1.796563 -0.409622 -0.116294 11.00000 0.02601 0.03601 =
0.04176 0.00153 -0.00009 0.00693
AFIX 13
H12 2 -1.779868 -0.374316 -0.078003 11.00000 -1.20000
AFIX 0
C13 1 -2.006384 -0.480167 -0.165877 11.00000 0.04157 0.01896 =
0.04288 0.00341 0.00568 -0.00078
AFIX 13
H13 2 -2.047523 -0.499475 -0.216636 11.00000 -1.20000
AFIX 0
C14 1 -2.295811 -0.116900 -0.555418 11.00000 0.05444 0.04642 =
0.04198 -0.02596 -0.00851 0.00722
AFIX 43
H14 2 -2.249647 -0.096830 -0.510444 11.00000 -1.20000
AFIX 0
C15 1 -1.755844 -0.240449 -0.209679 11.00000 0.02502 0.03611 =
0.04115 0.00002 0.00904 -0.00665
AFIX 13
H15 2 -1.705239 -0.266787 -0.235887 11.00000 -1.20000
AFIX 0
C16 1 -2.259933 -0.397366 -0.315351 11.00000 0.02507 0.02778 =
0.02970 -0.00688 0.00413 -0.00152
AFIX 13
H16 2 -2.198865 -0.429849 -0.293452 11.00000 -1.20000
AFIX 0
C17 1 -1.941934 -0.137145 -0.091245 11.00000 0.05089 0.03027 =
0.05197 -0.00495 0.00985 -0.01736
AFIX 137
H17A 2 -1.943098 -0.160767 -0.043879 11.00000 -1.50000
H17B 2 -1.909324 -0.095199 -0.077135 11.00000 -1.50000
H17C 2 -1.892263 -0.159179 -0.120576 11.00000 -1.50000
AFIX 0
C18 1 -2.432302 -0.174518 -0.691636 11.00000 0.02636 0.02612 =
0.02877 -0.00751 0.00085 0.00212
C22 1 -1.923361 -0.399045 -0.283084 11.00000 0.02431 0.02696 =
0.03208 0.00067 0.00644 0.00300
C19 1 -2.263821 -0.486829 -0.646321 11.00000 0.03727 0.03042 =
0.03923 0.00917 0.00730 0.00712
AFIX 43
H19 2 -2.195093 -0.498054 -0.663794 11.00000 -1.20000
AFIX 0
C20 1 -2.421099 -0.470341 -0.858040 11.00000 0.05323 0.02589 =
0.03601 -0.00798 -0.00082 0.00088
AFIX 13
H20 2 -2.485267 -0.449039 -0.897471 11.00000 -1.20000
AFIX 0
C21 1 -2.388650 -0.499274 -0.552753 11.00000 0.04548 0.03834 =
0.03424 0.01526 0.00737 -0.00528
AFIX 43
H21 2 -2.402658 -0.518346 -0.507210 11.00000 -1.20000
AFIX 0
C23 1 -2.261901 -0.202639 -0.255553 11.00000 0.03275 0.02734 =
0.02422 -0.00019 0.00608 0.01117
C25 1 -2.187284 -0.426896 -0.800376 11.00000 0.03867 0.03069 =
0.03560 -0.00160 0.01590 0.01406
AFIX 13
H25 2 -2.128019 -0.428963 -0.749154 11.00000 -1.20000
AFIX 0
C24 1 -1.861428 -0.334448 -0.381906 11.00000 0.04245 0.03633 =
0.04063 0.00124 0.01950 0.00321
AFIX 43
H24 2 -1.840193 -0.294974 -0.399487 11.00000 -1.20000
AFIX 0
C27 1 -2.234836 -0.378263 -0.394987 11.00000 0.03565 0.04191 =
0.02685 -0.00876 0.00391 -0.00593
AFIX 137
H27A 2 -2.291488 -0.345842 -0.419303 11.00000 -1.50000
H27B 2 -2.243494 -0.415042 -0.429103 11.00000 -1.50000
H27C 2 -2.153733 -0.361884 -0.386673 11.00000 -1.50000
AFIX 0
C26 1 -2.311746 -0.193250 -0.660886 11.00000 0.02342 0.02316 =
0.02709 -0.00577 0.00429 0.00191
C28 1 -2.090921 -0.480410 -0.109374 11.00000 0.04202 0.03584 =
0.05877 0.01232 0.01815 -0.00570
AFIX 137
H28A 2 -2.048702 -0.463995 -0.058623 11.00000 -1.50000
H28B 2 -2.117186 -0.523408 -0.103209 11.00000 -1.50000
H28C 2 -2.160185 -0.453982 -0.130659 11.00000 -1.50000
AFIX 0
C32 1 -1.845927 -0.169273 -0.323933 11.00000 0.04196 0.02899 =
0.03739 0.00240 0.01372 -0.00947
AFIX 23
H32A 2 -1.815166 -0.191974 -0.363968 11.00000 -1.20000
H32B 2 -1.860343 -0.125035 -0.340515 11.00000 -1.20000
AFIX 0
C31 1 -2.235045 -0.202919 -0.085379 11.00000 0.04177 0.02892 =
0.02936 -0.00222 0.01468 0.00525
AFIX 13
H31 2 -2.216379 -0.239719 -0.049475 11.00000 -1.20000
AFIX 0
C29 1 -2.128256 -0.213960 -0.749845 11.00000 0.03241 0.03150 =
0.04957 -0.00061 0.01937 -0.00833
AFIX 13
H29 2 -2.120912 -0.171580 -0.724888 11.00000 -1.20000
AFIX 0
C33 1 -2.383029 -0.429629 -0.319418 11.00000 0.03099 0.03220 =
0.04586 -0.01440 0.00780 -0.00907
AFIX 23
H33A 2 -2.447923 -0.404435 -0.351930 11.00000 -1.20000
H33B 2 -2.384499 -0.471981 -0.342606 11.00000 -1.20000
AFIX 0
C30 1 -2.523638 -0.299983 -0.568256 11.00000 0.04645 0.05637 =
0.03699 -0.00715 0.02209 0.00468
AFIX 137
H30A 2 -2.506551 -0.338568 -0.537540 11.00000 -1.50000
H30B 2 -2.561775 -0.269560 -0.540400 11.00000 -1.50000
H30C 2 -2.449301 -0.282317 -0.576310 11.00000 -1.50000
AFIX 0
C35 1 -2.399257 -0.434255 -0.235471 11.00000 0.03168 0.03873 =
0.05503 -0.00865 0.01651 -0.01069
AFIX 23
H35A 2 -2.347672 -0.467853 -0.207115 11.00000 -1.20000
H35B 2 -2.482817 -0.444933 -0.236401 11.00000 -1.20000
AFIX 0
C39 1 -2.070488 -0.131266 -0.142189 11.00000 0.04708 0.02302 =
0.03198 -0.00113 0.01122 -0.00285
AFIX 13
H39 2 -2.069692 -0.108974 -0.191857 11.00000 -1.20000
AFIX 0
C34 1 -2.675823 -0.124306 -0.850123 11.00000 0.04339 0.03082 =
0.06989 0.00088 -0.01459 0.01576
AFIX 23
H34A 2 -2.758732 -0.115763 -0.878556 11.00000 -1.20000
H34B 2 -2.649271 -0.090096 -0.812139 11.00000 -1.20000
AFIX 0
C36 1 -2.243961 -0.162791 -0.593936 11.00000 0.02973 0.04199 =
0.03537 -0.01100 -0.00653 0.00591
AFIX 43
H36 2 -2.162708 -0.173464 -0.574874 11.00000 -1.20000
AFIX 0
C38 1 -2.145961 -0.378190 -0.854475 11.00000 0.04492 0.05131 =
0.04730 0.00535 0.02769 0.01289
AFIX 137
H38A 2 -2.201677 -0.378347 -0.905648 11.00000 -1.50000
H38B 2 -2.066399 -0.389371 -0.860292 11.00000 -1.50000
H38C 2 -2.143867 -0.336275 -0.831445 11.00000 -1.50000
AFIX 0
C37 1 -2.022783 -0.272416 -0.629706 11.00000 0.01782 0.05246 =
0.05149 0.00346 0.00285 0.00306
AFIX 23
H37A 2 -2.017552 -0.236098 -0.594153 11.00000 -1.20000
H37B 2 -1.957920 -0.302074 -0.607357 11.00000 -1.20000
AFIX 0
C40 1 -2.059218 -0.211972 -0.390280 11.00000 0.04192 0.03514 =
0.02804 0.00429 0.00497 -0.00189
AFIX 137
H40A 2 -2.027320 -0.240544 -0.423754 11.00000 -1.50000
H40B 2 -2.080741 -0.172044 -0.417385 11.00000 -1.50000
H40C 2 -2.129892 -0.230721 -0.377965 11.00000 -1.50000
AFIX 0
C43 1 -2.152024 -0.095033 -0.097028 11.00000 0.05932 0.02598 =
0.04327 -0.01358 0.01357 0.00054
AFIX 23
H43A 2 -2.109016 -0.058679 -0.068841 11.00000 -1.20000
H43B 2 -2.224689 -0.079614 -0.133738 11.00000 -1.20000
AFIX 0
C41 1 -2.484240 -0.128065 -0.652408 11.00000 0.03333 0.04218 =
0.05078 -0.01744 -0.00031 0.01635
AFIX 43
H41 2 -2.564276 -0.115551 -0.672497 11.00000 -1.20000
AFIX 0
C42 1 -1.890059 -0.517277 -0.130357 11.00000 0.05380 0.02475 =
0.06177 0.01100 0.01879 0.00997
AFIX 23
H42A 2 -1.908350 -0.555392 -0.103364 11.00000 -1.20000
H42B 2 -1.850457 -0.530104 -0.171828 11.00000 -1.20000
AFIX 0
C44 1 -2.372243 -0.199029 -0.116231 11.00000 0.03558 0.04673 =
0.04805 -0.00271 0.01907 0.01002
AFIX 137
H44A 2 -2.393023 -0.159716 -0.144917 11.00000 -1.50000
H44B 2 -2.410361 -0.200348 -0.072280 11.00000 -1.50000
H44C 2 -2.399770 -0.234574 -0.150929 11.00000 -1.50000
AFIX 0
C45 1 -2.184713 -0.142411 -0.038903 11.00000 0.05368 0.04140 =
0.03457 -0.01255 0.01706 -0.00180
AFIX 23
H45A 2 -2.245162 -0.124026 -0.014072 11.00000 -1.20000
H45B 2 -2.113402 -0.152867 0.002360 11.00000 -1.20000
AFIX 0
C46 1 -2.420016 -0.259942 -0.347683 11.00000 0.04011 0.04286 =
0.04008 -0.00550 -0.01092 0.01295
AFIX 43
H46 2 -2.458650 -0.298017 -0.366676 11.00000 -1.20000
AFIX 0
C47 1 -1.916665 -0.453257 -0.328114 11.00000 0.05077 0.02744 =
0.04878 -0.00358 0.02041 0.00289
AFIX 43
H47 2 -1.932510 -0.493415 -0.309664 11.00000 -1.20000
AFIX 0
C48 1 -1.856834 -0.388213 -0.426245 11.00000 0.05867 0.05191 =
0.04344 0.00052 0.02950 0.00690
AFIX 43
H48 2 -1.833599 -0.384845 -0.474134 11.00000 -1.20000
AFIX 0
C50 1 -2.748261 -0.237706 -0.859807 11.00000 0.02795 0.04207 =
0.05089 0.00011 -0.00469 0.00750
AFIX 137
H50A 2 -2.734668 -0.235792 -0.912419 11.00000 -1.50000
H50B 2 -2.831803 -0.228307 -0.861868 11.00000 -1.50000
H50C 2 -2.729118 -0.279837 -0.838355 11.00000 -1.50000
AFIX 0
C51 1 -2.694185 -0.405894 -0.761186 11.00000 0.02495 0.03362 =
0.06215 0.00702 -0.00517 -0.00778
AFIX 13
H51 2 -2.686023 -0.448373 -0.736470 11.00000 -1.20000
AFIX 0
C49 1 -2.144347 -0.202489 -0.838239 11.00000 0.06355 0.04816 =
0.05864 0.01517 0.02920 0.00114
AFIX 137
H49A 2 -2.164235 -0.242131 -0.866332 11.00000 -1.50000
H49B 2 -2.070336 -0.185851 -0.848082 11.00000 -1.50000
H49C 2 -2.208650 -0.172227 -0.856219 11.00000 -1.50000
AFIX 0
C52 1 -2.476731 -0.525563 -0.821664 11.00000 0.06895 0.02555 =
0.06074 -0.00816 -0.00653 -0.00649
AFIX 137
H52A 2 -2.413768 -0.548912 -0.786026 11.00000 -1.50000
H52B 2 -2.518598 -0.553567 -0.863061 11.00000 -1.50000
H52C 2 -2.532951 -0.509076 -0.792940 11.00000 -1.50000
AFIX 0
C53 1 -2.307777 -0.145357 -0.290273 11.00000 0.05711 0.02601 =
0.03530 0.00321 0.00694 0.01067
AFIX 43
H53 2 -2.270211 -0.106988 -0.271431 11.00000 -1.20000
AFIX 0
C54 1 -2.472255 -0.456273 -0.595713 11.00000 0.03249 0.03804 =
0.03778 0.00867 0.00966 -0.00602
AFIX 43
H54 2 -2.543312 -0.447515 -0.579692 11.00000 -1.20000
AFIX 0
C56 1 -1.700038 -0.245303 -0.120812 11.00000 0.02684 0.04801 =
0.04631 0.00067 -0.00565 -0.01239
AFIX 137
H56A 2 -1.759800 -0.234253 -0.091952 11.00000 -1.50000
H56B 2 -1.632589 -0.216401 -0.106640 11.00000 -1.50000
H56C 2 -1.672567 -0.288314 -0.107855 11.00000 -1.50000
AFIX 0
C55 1 -2.727045 -0.347663 -0.643532 11.00000 0.02620 0.07485 =
0.06321 0.01481 0.02551 0.00829
AFIX 23
H55A 2 -2.711086 -0.383987 -0.607689 11.00000 -1.20000
H55B 2 -2.778942 -0.317836 -0.624097 11.00000 -1.20000
AFIX 0
C57 1 -2.467175 -0.150150 -0.859491 11.00000 0.04745 0.01939 =
0.04541 0.01061 0.00565 -0.00071
AFIX 13
H57 2 -2.424419 -0.171953 -0.894984 11.00000 -1.20000
AFIX 0
C58 1 -2.416603 -0.100570 -0.583527 11.00000 0.05609 0.05633 =
0.05466 -0.03556 0.00255 0.01656
AFIX 43
H58 2 -2.452379 -0.070996 -0.555972 11.00000 -1.20000
AFIX 0
C64 1 -1.808185 -0.472426 -0.071617 11.00000 0.03669 0.04417 =
0.05147 0.01544 0.00443 0.01688
AFIX 23
H64A 2 -1.728966 -0.491701 -0.052090 11.00000 -1.20000
H64B 2 -1.843333 -0.463945 -0.026706 11.00000 -1.20000
AFIX 0
C63 1 -1.754811 -0.172804 -0.243751 11.00000 0.03466 0.03624 =
0.05196 -0.00065 0.01005 -0.01518
AFIX 23
H63A 2 -1.776056 -0.141880 -0.207481 11.00000 -1.20000
H63B 2 -1.674240 -0.162639 -0.250239 11.00000 -1.20000
AFIX 0
C62 1 -2.012428 -0.250558 -0.710667 11.00000 0.02473 0.05926 =
0.06559 -0.00026 0.01829 -0.00413
AFIX 23
H62A 2 -2.002515 -0.287230 -0.742924 11.00000 -1.20000
H62B 2 -1.942277 -0.222964 -0.705846 11.00000 -1.20000
AFIX 0
C60 1 -2.202059 -0.493471 -0.839613 11.00000 0.07838 0.03555 =
0.05596 -0.00968 0.02094 0.02267
AFIX 23
H60A 2 -2.136413 -0.501651 -0.865483 11.00000 -1.20000
H60B 2 -2.201017 -0.526442 -0.800014 11.00000 -1.20000
AFIX 0
C59 1 -2.787826 -0.369591 -0.726393 11.00000 0.02275 0.06646 =
0.07193 0.02302 0.00632 -0.00398
AFIX 23
H59A 2 -2.818376 -0.332933 -0.759453 11.00000 -1.20000
H59B 2 -2.855651 -0.397421 -0.724720 11.00000 -1.20000
AFIX 0
C61 1 -2.321659 -0.493516 -0.899549 11.00000 0.08374 0.04413 =
0.04820 -0.02312 0.01733 0.00055
AFIX 23
H61A 2 -2.340400 -0.536345 -0.920505 11.00000 -1.20000
H61B 2 -2.317963 -0.465228 -0.943339 11.00000 -1.20000
AFIX 0
C68 1 -2.285222 -0.513628 -0.577567 11.00000 0.04719 0.03394 =
0.03603 0.01262 -0.00357 0.00687
AFIX 43
H68 2 -2.228712 -0.541719 -0.547849 11.00000 -1.20000
AFIX 0
C67 1 -2.733739 -0.417142 -0.850170 11.00000 0.03792 0.03916 =
0.06927 -0.00846 -0.01780 -0.00614
AFIX 137
H67A 2 -2.735473 -0.377066 -0.877556 11.00000 -1.50000
H67B 2 -2.813244 -0.435893 -0.862876 11.00000 -1.50000
H67C 2 -2.677503 -0.445576 -0.866324 11.00000 -1.50000
AFIX 0
C65 1 -2.391260 -0.092394 -0.820935 11.00000 0.05875 0.03411 =
0.06878 0.00933 0.01121 -0.00596
AFIX 137
H65A 2 -2.434917 -0.069356 -0.788555 11.00000 -1.50000
H65B 2 -2.376009 -0.064629 -0.861684 11.00000 -1.50000
H65C 2 -2.315536 -0.107198 -0.788534 11.00000 -1.50000
AFIX 0
C66 1 -2.593544 -0.128434 -0.907961 11.00000 0.06938 0.03234 =
0.05265 0.01591 -0.01014 0.00268
AFIX 23
H66A 2 -2.587762 -0.087017 -0.932141 11.00000 -1.20000
H66B 2 -2.625567 -0.159088 -0.949695 11.00000 -1.20000
AFIX 0
C70 1 -1.692650 -0.414405 -0.158763 11.00000 0.02934 0.04937 =
0.06402 0.00622 0.00849 0.01028
AFIX 137
H70A 2 -1.702844 -0.452239 -0.191132 11.00000 -1.50000
H70B 2 -1.616707 -0.416604 -0.120082 11.00000 -1.50000
H70C 2 -1.693285 -0.377371 -0.191688 11.00000 -1.50000
AFIX 0
C69 1 -1.886245 -0.447273 -0.400731 11.00000 0.06744 0.03464 =
0.05629 -0.01621 0.03040 0.00023
AFIX 43
H69 2 -1.885685 -0.483224 -0.432324 11.00000 -1.20000
AFIX 0
C71 1 -2.409568 -0.144946 -0.353066 11.00000 0.07332 0.04497 =
0.04173 0.00258 -0.00650 0.02294
AFIX 43
H71 2 -2.439895 -0.106381 -0.376383 11.00000 -1.20000
AFIX 0
C72 1 -2.465668 -0.201708 -0.380842 11.00000 0.06254 0.05733 =
0.04523 -0.00206 -0.01846 0.02622
AFIX 43
H72 2 -2.534833 -0.201111 -0.422221 11.00000 -1.20000
AFIX 6
O1 5 -1.967828 -0.111316 -0.509402 11.00000 0.11198
H1A 2 -2.012291 -0.086481 -0.489596 11.00000 -1.50000
H1B 2 -1.966205 -0.098348 -0.555674 11.00000 -1.50000
AFIX 6
O0AA 5 -1.761589 -0.199231 -0.505916 11.00000 0.13229
H0AA 2 -1.738857 -0.171943 -0.535799 11.00000 -1.50000
H0AB 2 -1.837511 -0.195622 -0.510171 11.00000 -1.50000
AFIX 0
HKLF 4
REM str1832 in P21 #4
REM wR2 = 0.0542, GooF = S = 1.025, Restrained GooF = 1.025 for all data
REM R1 = 0.0217 for 11976 Fo > 4sig(Fo) and 0.0235 for all 12484 data
REM 823 parameters refined using 1 restraints
END
WGHT 0.0285 2.0211
REM Highest difference peak 0.518, deepest hole -0.528, 1-sigma level 0.054
Q1 1 -2.3934 -0.3093 -0.7014 11.00000 0.05 0.52
Q2 1 -2.0946 -0.3102 -0.2658 11.00000 0.05 0.49
Q3 1 -2.0096 -0.3546 -0.0500 11.00000 0.05 0.37
Q4 1 -2.1376 -0.6002 -0.2953 11.00000 0.05 0.35
Q5 1 -2.0280 -0.3073 -0.0944 11.00000 0.05 0.31
Q6 1 -2.4907 -0.2630 -0.9672 11.00000 0.05 0.28
Q7 1 -2.0681 0.0249 -0.3381 11.00000 0.05 0.28
Q8 1 -2.2105 -0.5871 -0.4162 11.00000 0.05 0.27
Q9 1 -2.4642 -0.3086 -0.8634 11.00000 0.05 0.27
Q10 1 -2.1488 -0.6282 -0.3325 11.00000 0.05 0.27
Q11 1 -2.0978 0.0304 -0.3760 11.00000 0.05 0.26
Q12 1 -1.9441 -0.3623 0.0017 11.00000 0.05 0.25
Q13 1 -2.0029 -0.2721 -0.0501 11.00000 0.05 0.25
Q14 1 -1.9154 -0.3057 -0.2836 11.00000 0.05 0.24
Q15 1 -2.0755 -0.3432 -0.2068 11.00000 0.05 0.24
Q16 1 -2.4647 -0.3504 -0.9065 11.00000 0.05 0.23
Q17 1 -2.0620 -0.0161 -0.2981 11.00000 0.05 0.23
Q18 1 -2.5208 -0.3616 -0.9607 11.00000 0.05 0.23
Q19 1 -2.0460 -0.3476 -0.1369 11.00000 0.05 0.22
Q20 1 -2.1319 -0.0197 -0.4305 11.00000 0.05 0.22
;
_shelx_res_checksum 74174
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.297
_oxdiff_exptl_absorpt_empirical_full_min 0.832
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF-d8'
#######################################################################
#
# 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_str1619
_database_code_depnum_ccdc_archive 'CCDC 1952455'
loop_
_audit_author_name
_audit_author_address
'Marta Feliz'
;Instituto de Tecnologia Quimica
Spain
;
_audit_update_record
;
2019-09-09 deposited with the CCDC. 2020-03-20 downloaded from the CCDC.
;
_audit_creation_date 2019-08-23
_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 delta-[FeI{(S,S)-Me-DuPhos}2](ClO4)
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H56 Fe I P4, Cl O4'
_chemical_formula_sum 'C36 H56 Cl Fe I O4 P4'
_chemical_formula_weight 894.88
_chemical_absolute_configuration rm
_chemical_melting_point ?
_chemical_oxdiff_formula 'C48 D8 B F4 O P4 Fe'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
_cell_length_a 11.23747(14)
_cell_length_b 20.9195(3)
_cell_length_c 33.7258(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 7928.34(18)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 36898
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 28.6240
_cell_measurement_theta_min 3.1710
_shelx_estimated_absorpt_T_max 0.916
_shelx_estimated_absorpt_T_min 0.683
_exptl_absorpt_coefficient_mu 1.424
_exptl_absorpt_correction_T_max 0.843
_exptl_absorpt_correction_T_min 0.571
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.499
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 3680
_exptl_crystal_size_max 0.2894
_exptl_crystal_size_mid 0.187
_exptl_crystal_size_min 0.0625
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0441
_diffrn_reflns_av_unetI/netI 0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_l_max 44
_diffrn_reflns_limit_l_min -40
_diffrn_reflns_number 93611
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.103
_diffrn_reflns_theta_min 2.922
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -20.00 29.70 0.7000 50.0000
omega____ theta____ kappa____ phi______ frames
- -15.6603 -99.0000 -180.0000 71
#__ type_ start__ end____ width___ exp.time_
2 omega -109.00 -55.10 0.7000 50.0000
omega____ theta____ kappa____ phi______ frames
- -15.6603 178.0000 -120.0000 77
#__ type_ start__ end____ width___ exp.time_
3 omega -112.00 -57.40 0.7000 50.0000
omega____ theta____ kappa____ phi______ frames
- -15.6603 -178.0000 -180.0000 78
#__ type_ start__ end____ width___ exp.time_
4 omega -20.00 100.40 0.7000 50.0000
omega____ theta____ kappa____ phi______ frames
- 16.9103 38.0000 -150.0000 172
#__ type_ start__ end____ width___ exp.time_
5 omega -72.00 99.50 0.7000 50.0000
omega____ theta____ kappa____ phi______ frames
- 16.9103 -19.0000 -150.0000 245
#__ type_ start__ end____ width___ exp.time_
6 omega -70.00 15.40 0.7000 50.0000
omega____ theta____ kappa____ phi______ frames
- 16.9103 -67.0000 48.2429 122
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 0.0493685000
_diffrn_orient_matrix_UB_12 0.0022281000
_diffrn_orient_matrix_UB_13 0.0130209000
_diffrn_orient_matrix_UB_21 0.0213348000
_diffrn_orient_matrix_UB_22 -0.0298371000
_diffrn_orient_matrix_UB_23 -0.0070255000
_diffrn_orient_matrix_UB_31 0.0330383000
_diffrn_orient_matrix_UB_32 0.0159648000
_diffrn_orient_matrix_UB_33 -0.0149414000
_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 0.777
_reflns_Friedel_fraction_full 0.999
_reflns_Friedel_fraction_max 0.882
_reflns_number_gt 17109
_reflns_number_total 19581
_reflns_odcompleteness_completeness 99.71
_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 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.904
_refine_diff_density_min -1.441
_refine_diff_density_rms 0.096
_refine_ls_abs_structure_details
;
Flack x determined using 6797 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack -0.011(6)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.060
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 821
_refine_ls_number_reflns 19581
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0509
_refine_ls_R_factor_gt 0.0397
_refine_ls_restrained_S_all 1.060
_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^)+(0.0498P)^2^+11.1151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1011
_refine_ls_wR_factor_ref 0.1098
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Others
Fixed Sof: O2(0.51) O8(0.54) O9(0.49) O10(0.46)
3.a Ternary CH refined with riding coordinates:
C3(H3), C6(H6), C9(H9), C5(H5), C12(H12), C11(H11), C13(H13), C19(H19),
C21(H21), C26(H26), C24(H24), C29(H29), C30(H30), C38(H38), C34(H34), C40(H40)
3.b Secondary CH2 refined with riding coordinates:
C2(H2A,H2B), C8(H8A,H8B), C7(H7A,H7B), C10(H10A,H10B), C25(H25A,H25B),
C39(H39A,H39B), C45(H45A,H45B), C54(H54A,H54B), C59(H59A,H59B), C58(H58A,H58B),
C55(H55A,H55B), C66(H66A,H66B), C65(H65A,H65B), C74(H74A,H74B), C71(H71A,
H71B), C72(H72A,H72B)
3.c Aromatic/amide H refined with riding coordinates:
C17(H17), C15(H15), C33(H33), C37(H37), C42(H42), C48(H48), C47(H47),
C49(H49), C50(H50), C52(H52), C51(H51), C63(H63), C62(H62), C64(H64), C70(H70),
C73(H73)
3.d Idealised Me refined as rotating group:
C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C31(H31A,H31B,
H31C), C28(H28A,H28B,H28C), C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C43(H43A,
H43B,H43C), C61(H61A,H61B,H61C), C57(H57A,H57B,H57C), C60(H60A,H60B,H60C),
C53(H53A,H53B,H53C), C68(H68A,H68B,H68C), C67(H67A,H67B,H67C), C69(H69A,H69B,
H69C), C75(H75A,H75B,H75C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.69543(6) 0.83013(3) 0.09983(2) 0.01895(14) Uani 1 1 d . . . . .
I1 I 0.70453(3) 0.84188(2) 0.02340(2) 0.03144(9) Uani 1 1 d . . . . .
P1 P 0.52375(12) 0.79920(6) 0.13170(4) 0.0215(3) Uani 1 1 d . . . . .
P2 P 0.86700(12) 0.85133(7) 0.13398(4) 0.0258(3) Uani 1 1 d . . . . .
P3 P 0.60633(12) 0.92733(6) 0.10427(4) 0.0250(3) Uani 1 1 d . . . . .
P4 P 0.78169(12) 0.73235(6) 0.09510(4) 0.0227(3) Uani 1 1 d . . . . .
Fe2 Fe 0.71109(6) 1.16353(3) -0.09779(2) 0.01847(13) Uani 1 1 d . . . . .
I2 I 0.71464(4) 1.15898(2) -0.02098(2) 0.03216(9) Uani 1 1 d . . . . .
P5 P 0.85088(12) 1.21962(6) -0.13323(4) 0.0227(3) Uani 1 1 d . . . . .
P6 P 0.56068(12) 1.10876(7) -0.12800(4) 0.0240(3) Uani 1 1 d . . . . .
P7 P 0.62743(14) 1.26187(7) -0.09470(4) 0.0288(3) Uani 1 1 d . . . . .
P8 P 0.79858(12) 1.06590(6) -0.10106(4) 0.0206(2) Uani 1 1 d . . . . .
C1 C 0.7676(5) 1.2839(3) -0.15881(16) 0.0285(12) Uani 1 1 d . . . . .
C2 C 0.8705(6) 0.9785(3) -0.0459(2) 0.0401(15) Uani 1 1 d . . . . .
H2A H 0.892547 1.005780 -0.023808 0.048 Uiso 1 1 calc R . . . .
H2B H 0.862025 0.935077 -0.036157 0.048 Uiso 1 1 calc R . . . .
C3 C 0.7526(5) 1.0016(3) -0.06441(17) 0.0293(12) Uani 1 1 d . . . . .
H3 H 0.703935 1.021273 -0.043607 0.035 Uiso 1 1 calc R . . . .
C6 C 0.9084(5) 0.7191(3) 0.05918(18) 0.0318(12) Uani 1 1 d . . . . .
H6 H 0.912942 0.755453 0.040937 0.038 Uiso 1 1 calc R . . . .
C9 C 0.7037(5) 0.6568(3) 0.08119(17) 0.0307(11) Uani 1 1 d . . . . .
H9 H 0.671781 0.635886 0.104919 0.037 Uiso 1 1 calc R . . . .
C8 C 0.8008(6) 0.6152(3) 0.06252(19) 0.0381(14) Uani 1 1 d . . . . .
H8A H 0.851231 0.596932 0.082934 0.046 Uiso 1 1 calc R . . . .
H8B H 0.765472 0.580627 0.047395 0.046 Uiso 1 1 calc R . . . .
C7 C 0.8729(6) 0.6584(3) 0.03560(18) 0.0399(14) Uani 1 1 d . . . . .
H7A H 0.826039 0.670164 0.012577 0.048 Uiso 1 1 calc R . . . .
H7B H 0.943641 0.636172 0.026554 0.048 Uiso 1 1 calc R . . . .
C5 C 0.4847(5) 0.9468(3) 0.06782(19) 0.0337(13) Uani 1 1 d . . . . .
H5 H 0.481199 0.912692 0.047962 0.040 Uiso 1 1 calc R . . . .
C12 C 0.4327(5) 1.0629(3) -0.10484(19) 0.0355(13) Uani 1 1 d . . . . .
H12 H 0.434308 1.020220 -0.116869 0.043 Uiso 1 1 calc R . . . .
C10 C 0.9660(6) 0.9813(3) -0.0782(2) 0.0385(14) Uani 1 1 d . . . . .
H10A H 0.950004 0.949799 -0.098673 0.046 Uiso 1 1 calc R . . . .
H10B H 1.044061 0.972878 -0.067100 0.046 Uiso 1 1 calc R . . . .
C11 C 0.9607(5) 1.0491(3) -0.09557(17) 0.0264(11) Uani 1 1 d . . . . .
H11 H 0.999737 1.050222 -0.121543 0.032 Uiso 1 1 calc R . . . .
C13 C 0.9900(6) 1.2625(3) -0.11638(19) 0.0362(14) Uani 1 1 d . . . . .
H13 H 0.985769 1.305663 -0.127624 0.043 Uiso 1 1 calc R . . . .
C17 C 0.8689(6) 0.6605(3) 0.16150(18) 0.0375(13) Uani 1 1 d . . . . .
H17 H 0.834448 0.623873 0.150926 0.045 Uiso 1 1 calc R . . . .
C15 C 0.4091(5) 0.8639(3) 0.19624(19) 0.0353(13) Uani 1 1 d . . . . .
H15 H 0.373703 0.825253 0.202976 0.042 Uiso 1 1 calc R . . . .
C16 C 0.8523(5) 0.7202(3) 0.14306(16) 0.0282(11) Uani 1 1 d . . . . .
C14 C 0.4824(5) 0.8679(3) 0.16302(17) 0.0278(11) Uani 1 1 d . . . . .
C19 C 0.3758(5) 0.7744(3) 0.10942(17) 0.0304(12) Uani 1 1 d . . . . .
H19 H 0.315787 0.800701 0.122829 0.037 Uiso 1 1 calc R . . . .
C22 C 0.5908(6) 0.7355(3) 0.20470(17) 0.0351(13) Uani 1 1 d . . . . .
H22A H 0.666089 0.756582 0.201618 0.053 Uiso 1 1 calc GR . . . .
H22B H 0.602808 0.694411 0.216748 0.053 Uiso 1 1 calc GR . . . .
H22C H 0.539900 0.760901 0.221255 0.053 Uiso 1 1 calc GR . . . .
C20 C 0.3557(5) 0.7851(3) 0.06535(18) 0.0349(13) Uani 1 1 d . . . . .
H20A H 0.341344 0.829670 0.060522 0.052 Uiso 1 1 calc GR . . . .
H20B H 0.288101 0.760665 0.056793 0.052 Uiso 1 1 calc GR . . . .
H20C H 0.424942 0.771717 0.050902 0.052 Uiso 1 1 calc GR . . . .
C21 C 0.5329(5) 0.7268(3) 0.16415(16) 0.0266(11) Uani 1 1 d . . . . .
H21 H 0.582855 0.696096 0.149857 0.032 Uiso 1 1 calc R . . . .
C25 C 0.5883(10) 1.3420(4) -0.0336(2) 0.071(3) Uani 1 1 d . . . . .
H25A H 0.573466 1.311628 -0.012410 0.085 Uiso 1 1 calc R . . . .
H25B H 0.604829 1.383331 -0.021772 0.085 Uiso 1 1 calc R . . . .
C26 C 0.4701(7) 1.2809(3) -0.0819(2) 0.0475(18) Uani 1 1 d . . . . .
H26 H 0.423895 1.286155 -0.106312 0.057 Uiso 1 1 calc R . . . .
C23 C 0.6567(6) 1.2992(3) -0.14269(17) 0.0319(12) Uani 1 1 d . . . . .
C24 C 0.6940(8) 1.3203(3) -0.0582(2) 0.0469(17) Uani 1 1 d . . . . .
H24 H 0.751314 1.298118 -0.041174 0.056 Uiso 1 1 calc R . . . .
C29 C 1.0172(5) 0.8793(3) 0.1152(2) 0.0386(15) Uani 1 1 d . . . . .
H29 H 1.075217 0.847823 0.124653 0.046 Uiso 1 1 calc R . . . .
C32 C 0.9031(5) 0.7755(3) 0.15941(17) 0.0300(12) Uani 1 1 d . . . . .
C27 C 1.0188(5) 1.0974(3) -0.0677(2) 0.0362(14) Uani 1 1 d . . . . .
H27A H 1.010400 1.139640 -0.078476 0.054 Uiso 1 1 calc GR . . . .
H27B H 1.101736 1.087447 -0.064824 0.054 Uiso 1 1 calc GR . . . .
H27C H 0.980761 1.095521 -0.042224 0.054 Uiso 1 1 calc GR . . . .
C30 C 0.8589(5) 0.9140(3) 0.17236(18) 0.0340(13) Uani 1 1 d . . . . .
H30 H 0.813812 0.949255 0.160464 0.041 Uiso 1 1 calc R . . . .
C31 C 0.7924(6) 0.8964(3) 0.21062(18) 0.0409(14) Uani 1 1 d . . . . .
H31A H 0.714714 0.880420 0.204083 0.061 Uiso 1 1 calc GR . . . .
H31B H 0.784717 0.933621 0.227053 0.061 Uiso 1 1 calc GR . . . .
H31C H 0.836103 0.864062 0.224620 0.061 Uiso 1 1 calc GR . . . .
C33 C 0.9764(6) 0.7700(4) 0.1928(2) 0.0448(16) Uani 1 1 d . . . . .
H33 H 1.013591 0.805890 0.203254 0.054 Uiso 1 1 calc R . . . .
C28 C 0.6832(6) 0.9463(3) -0.08246(19) 0.0386(15) Uani 1 1 d . . . . .
H28A H 0.614340 0.962528 -0.095945 0.058 Uiso 1 1 calc GR . . . .
H28B H 0.658714 0.917543 -0.061835 0.058 Uiso 1 1 calc GR . . . .
H28C H 0.732937 0.923916 -0.100994 0.058 Uiso 1 1 calc GR . . . .
C35 C 0.7521(5) 1.0327(2) -0.14874(16) 0.0225(10) Uani 1 1 d . . . . .
C38 C 0.4610(5) 1.1565(3) -0.16086(19) 0.0366(13) Uani 1 1 d . . . . .
H38 H 0.445010 1.196599 -0.146842 0.044 Uiso 1 1 calc R . . . .
C37 C 0.5832(5) 1.0181(3) -0.19169(17) 0.0307(12) Uani 1 1 d . . . . .
H37 H 0.503757 1.025698 -0.197845 0.037 Uiso 1 1 calc R . . . .
C39 C 1.0930(6) 1.2283(4) -0.1379(2) 0.0427(16) Uani 1 1 d . . . . .
H39A H 1.160497 1.256951 -0.140575 0.051 Uiso 1 1 calc R . . . .
H39B H 1.118058 1.191136 -0.122946 0.051 Uiso 1 1 calc R . . . .
C36 C 0.6346(5) 1.0481(2) -0.15928(17) 0.0258(11) Uani 1 1 d . . . . .
C34 C 0.6801(6) 1.0069(3) 0.0996(2) 0.0391(14) Uani 1 1 d . . . . .
H34 H 0.698274 1.023644 0.126017 0.047 Uiso 1 1 calc R . . . .
C41 C 0.8592(5) 1.1586(3) -0.20963(16) 0.0327(12) Uani 1 1 d . . . . .
H41A H 0.788661 1.135296 -0.202610 0.049 Uiso 1 1 calc GR . . . .
H41B H 0.907018 1.133208 -0.227181 0.049 Uiso 1 1 calc GR . . . .
H41C H 0.837265 1.197689 -0.222624 0.049 Uiso 1 1 calc GR . . . .
C44 C 0.7945(6) 1.0035(3) 0.0750(3) 0.0516(19) Uani 1 1 d . . . . .
H44A H 0.844311 0.969887 0.085046 0.077 Uiso 1 1 calc GR . . . .
H44B H 0.836033 1.043512 0.076833 0.077 Uiso 1 1 calc GR . . . .
H44C H 0.775026 0.994985 0.047826 0.077 Uiso 1 1 calc GR . . . .
C40 C 0.9298(5) 1.1738(3) -0.17237(16) 0.0267(11) Uani 1 1 d . . . . .
H40 H 0.949481 1.132402 -0.160442 0.032 Uiso 1 1 calc R . . . .
C45 C 0.3539(6) 0.7059(3) 0.1238(2) 0.0398(15) Uani 1 1 d . . . . .
H45A H 0.269066 0.697481 0.124978 0.048 Uiso 1 1 calc R . . . .
H45B H 0.389694 0.675739 0.105567 0.048 Uiso 1 1 calc R . . . .
C42 C 0.5848(6) 1.3443(3) -0.1610(2) 0.0453(16) Uani 1 1 d . . . . .
H42 H 0.510919 1.354513 -0.150284 0.054 Uiso 1 1 calc R . . . .
C43 C 0.3606(6) 0.9554(3) 0.0856(2) 0.0422(15) Uani 1 1 d . . . . .
H43A H 0.339004 0.917628 0.100082 0.063 Uiso 1 1 calc GR . . . .
H43B H 0.304096 0.962581 0.064756 0.063 Uiso 1 1 calc GR . . . .
H43C H 0.360814 0.991467 0.103259 0.063 Uiso 1 1 calc GR . . . .
C46 C 0.5291(5) 0.9272(3) 0.15199(17) 0.0277(11) Uani 1 1 d . . . . .
C48 C 0.3888(7) 0.9183(3) 0.2194(2) 0.0470(17) Uani 1 1 d . . . . .
H48 H 0.341343 0.915386 0.241935 0.056 Uiso 1 1 calc R . . . .
C47 C 0.5070(6) 0.9812(3) 0.1756(2) 0.0417(15) Uani 1 1 d . . . . .
H47 H 0.538599 1.020659 0.168616 0.050 Uiso 1 1 calc R . . . .
C49 C 0.8184(5) 0.9911(3) -0.17195(18) 0.0328(13) Uani 1 1 d . . . . .
H49 H 0.896190 0.981151 -0.164860 0.039 Uiso 1 1 calc R . . . .
C50 C 0.7685(6) 0.9644(3) -0.20582(19) 0.0392(15) Uani 1 1 d . . . . .
H50 H 0.814004 0.938387 -0.222270 0.047 Uiso 1 1 calc R . . . .
C52 C 0.9367(8) 0.6572(4) 0.1954(2) 0.055(2) Uani 1 1 d . . . . .
H52 H 0.944315 0.618287 0.208539 0.066 Uiso 1 1 calc R . . . .
C51 C 0.6497(6) 0.9768(3) -0.21495(18) 0.0375(14) Uani 1 1 d . . . . .
H51 H 0.614802 0.957217 -0.236808 0.045 Uiso 1 1 calc R . . . .
C61 C 0.5101(6) 1.1749(4) -0.20125(19) 0.0452(17) Uani 1 1 d . . . . .
H61A H 0.587587 1.193568 -0.198103 0.068 Uiso 1 1 calc GR . . . .
H61B H 0.457841 1.205328 -0.213546 0.068 Uiso 1 1 calc GR . . . .
H61C H 0.515907 1.137507 -0.217623 0.068 Uiso 1 1 calc GR . . . .
C57 C 1.0338(6) 0.8829(4) 0.0698(2) 0.0463(17) Uani 1 1 d . . . . .
H57A H 1.021294 0.841395 0.058474 0.069 Uiso 1 1 calc GR . . . .
H57B H 1.113001 0.897179 0.063922 0.069 Uiso 1 1 calc GR . . . .
H57C H 0.977282 0.912503 0.058892 0.069 Uiso 1 1 calc GR . . . .
C54 C 0.4084(6) 0.6981(3) 0.1648(2) 0.0371(14) Uani 1 1 d . . . . .
H54A H 0.412448 0.653180 0.171770 0.044 Uiso 1 1 calc R . . . .
H54B H 0.359834 0.719823 0.184427 0.044 Uiso 1 1 calc R . . . .
C59 C 0.3193(6) 1.0953(4) -0.1203(2) 0.052(2) Uani 1 1 d . . . . .
H59A H 0.254155 1.064881 -0.120753 0.063 Uiso 1 1 calc R . . . .
H59B H 0.297373 1.130450 -0.103010 0.063 Uiso 1 1 calc R . . . .
C60 C 0.4338(6) 1.0522(3) -0.0601(2) 0.0424(15) Uani 1 1 d . . . . .
H60A H 0.496694 1.023125 -0.053380 0.064 Uiso 1 1 calc GR . . . .
H60B H 0.358885 1.034548 -0.051968 0.064 Uiso 1 1 calc GR . . . .
H60C H 0.446543 1.092272 -0.046915 0.064 Uiso 1 1 calc GR . . . .
C58 C 0.3436(5) 1.1200(4) -0.1620(2) 0.0511(19) Uani 1 1 d . . . . .
H58A H 0.279736 1.148014 -0.170474 0.061 Uiso 1 1 calc R . . . .
H58B H 0.348901 1.084581 -0.180459 0.061 Uiso 1 1 calc R . . . .
C55 C 0.9855(6) 0.9394(4) 0.1782(2) 0.0476(17) Uani 1 1 d . . . . .
H55A H 1.029705 0.911559 0.195859 0.057 Uiso 1 1 calc R . . . .
H55B H 0.983427 0.981908 0.189676 0.057 Uiso 1 1 calc R . . . .
C53 C 0.6036(6) 0.6701(3) 0.0516(2) 0.0397(14) Uani 1 1 d . . . . .
H53A H 0.543826 0.696017 0.064034 0.059 Uiso 1 1 calc GR . . . .
H53B H 0.568911 0.630360 0.043243 0.059 Uiso 1 1 calc GR . . . .
H53C H 0.635238 0.692160 0.029002 0.059 Uiso 1 1 calc GR . . . .
C63 C 0.7365(7) 1.3620(3) -0.2104(2) 0.0432(16) Uani 1 1 d . . . . .
H63 H 0.764697 1.384201 -0.232324 0.052 Uiso 1 1 calc R . . . .
C62 C 0.8078(6) 1.3161(3) -0.19225(19) 0.0358(13) Uani 1 1 d . . . . .
H62 H 0.882694 1.307064 -0.202544 0.043 Uiso 1 1 calc R . . . .
C66 C 1.0492(5) 1.2083(3) -0.17841(19) 0.0383(15) Uani 1 1 d . . . . .
H66A H 1.106233 1.179948 -0.190903 0.046 Uiso 1 1 calc R . . . .
H66B H 1.038554 1.245498 -0.195236 0.046 Uiso 1 1 calc R . . . .
C64 C 0.6243(7) 1.3746(3) -0.1959(2) 0.0495(19) Uani 1 1 d . . . . .
H64 H 0.574716 1.403031 -0.209123 0.059 Uiso 1 1 calc R . . . .
C65 C 1.0447(6) 0.9413(4) 0.1373(2) 0.0496(18) Uani 1 1 d . . . . .
H65A H 1.014982 0.977530 0.122328 0.060 Uiso 1 1 calc R . . . .
H65B H 1.130120 0.946140 0.140275 0.060 Uiso 1 1 calc R . . . .
C68 C 0.7543(8) 1.3788(3) -0.0777(2) 0.055(2) Uani 1 1 d . . . . .
H68A H 0.817176 1.364592 -0.094801 0.082 Uiso 1 1 calc GR . . . .
H68B H 0.786531 1.406043 -0.057446 0.082 Uiso 1 1 calc GR . . . .
H68C H 0.696569 1.402127 -0.092890 0.082 Uiso 1 1 calc GR . . . .
C67 C 1.0093(7) 1.2710(4) -0.0717(2) 0.0505(18) Uani 1 1 d . . . . .
H67A H 0.949194 1.298849 -0.061238 0.076 Uiso 1 1 calc GR . . . .
H67B H 1.086424 1.289293 -0.067133 0.076 Uiso 1 1 calc GR . . . .
H67C H 1.004434 1.230141 -0.058878 0.076 Uiso 1 1 calc GR . . . .
C70 C 0.4384(7) 0.9754(3) 0.2092(2) 0.0497(18) Uani 1 1 d . . . . .
H70 H 0.425608 1.011016 0.225140 0.060 Uiso 1 1 calc R . . . .
C74 C 0.4804(9) 1.3466(4) -0.0603(3) 0.073(3) Uani 1 1 d . . . . .
H74A H 0.490224 1.380847 -0.079347 0.087 Uiso 1 1 calc R . . . .
H74B H 0.409353 1.354859 -0.044741 0.087 Uiso 1 1 calc R . . . .
C69 C 1.0305(6) 0.7097(3) 0.0791(2) 0.0423(16) Uani 1 1 d . . . . .
H69A H 1.048832 0.746370 0.095058 0.063 Uiso 1 1 calc GR . . . .
H69B H 1.090511 0.704527 0.059083 0.063 Uiso 1 1 calc GR . . . .
H69C H 1.028309 0.672252 0.095556 0.063 Uiso 1 1 calc GR . . . .
C71 C 0.5272(7) 1.0085(3) 0.0474(2) 0.0462(17) Uani 1 1 d . . . . .
H71A H 0.583671 0.998678 0.026471 0.055 Uiso 1 1 calc R . . . .
H71B H 0.460411 1.031296 0.035869 0.055 Uiso 1 1 calc R . . . .
C73 C 0.9932(8) 0.7101(4) 0.2102(2) 0.056(2) Uani 1 1 d . . . . .
H73 H 1.043167 0.706164 0.232003 0.067 Uiso 1 1 calc R . . . .
C75 C 0.4109(6) 1.2312(3) -0.0558(2) 0.0504(18) Uani 1 1 d . . . . .
H75A H 0.417516 1.189909 -0.067993 0.076 Uiso 1 1 calc GR . . . .
H75B H 0.328362 1.241830 -0.052468 0.076 Uiso 1 1 calc GR . . . .
H75C H 0.449214 1.230441 -0.030349 0.076 Uiso 1 1 calc GR . . . .
C72 C 0.5867(7) 1.0490(3) 0.0799(2) 0.0457(17) Uani 1 1 d . . . . .
H72A H 0.623763 1.086597 0.068365 0.055 Uiso 1 1 calc R . . . .
H72B H 0.528130 1.062861 0.099174 0.055 Uiso 1 1 calc R . . . .
Cl1 Cl 0.6607(2) 0.53584(12) 0.18321(7) 0.0688(6) Uiso 1 1 d . . . . .
Cl2 Cl 0.2628(4) 1.3768(2) -0.18480(12) 0.1172(11) Uiso 1 1 d . . . . .
O1 O 0.6067(4) 0.4656(2) 0.18732(14) 0.0452(11) Uiso 1 1 d . . . . .
O3 O 0.7690(6) 0.5243(3) 0.20550(19) 0.0727(17) Uiso 1 1 d . . . . .
O2 O 0.7065(12) 0.5323(6) 0.1455(3) 0.060(3) Uiso 0.51 1 d . . P A 1
O4 O 0.5871(7) 0.5706(4) 0.2053(2) 0.0809(19) Uiso 1 1 d . . . . .
O5 O 0.2844(8) 1.3555(4) -0.1438(3) 0.104(2) Uiso 1 1 d . . . . .
O6 O 0.1370(7) 1.3742(3) -0.1871(2) 0.084(2) Uiso 1 1 d . . . . .
O7 O 0.3156(7) 1.4294(4) -0.1913(2) 0.095(2) Uiso 1 1 d . . . . .
O8 O 0.3068(13) 1.3128(7) -0.1984(5) 0.083(4) Uiso 0.54 1 d . . P B 1
O9 O 0.6513(10) 0.5481(5) 0.1470(3) 0.044(2) Uiso 0.49 1 d . . P A 2
O10 O 0.2952(16) 1.3365(8) -0.2192(6) 0.090(5) Uiso 0.46 1 d . . P B 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0191(3) 0.0189(3) 0.0188(3) 0.0019(3) 0.0006(3) 0.0001(3)
I1 0.03668(19) 0.03668(19) 0.02095(17) 0.00652(14) 0.00107(15) 0.00168(17)
P1 0.0214(6) 0.0220(6) 0.0211(6) 0.0012(5) 0.0017(5) -0.0022(5)
P2 0.0213(6) 0.0291(7) 0.0269(7) -0.0019(5) -0.0011(5) -0.0005(5)
P3 0.0250(6) 0.0200(6) 0.0301(7) 0.0038(5) 0.0012(6) 0.0002(5)
P4 0.0247(6) 0.0223(6) 0.0212(6) -0.0002(5) 0.0019(5) 0.0031(5)
Fe2 0.0213(3) 0.0176(3) 0.0165(3) 0.0003(2) 0.0019(3) 0.0008(3)
I2 0.0465(2) 0.03170(18) 0.01823(16) -0.00065(13) 0.00030(15) 0.00070(17)
P5 0.0255(6) 0.0218(6) 0.0209(6) 0.0028(5) 0.0008(5) -0.0009(5)
P6 0.0185(6) 0.0305(7) 0.0230(7) -0.0007(5) 0.0012(5) 0.0003(5)
P7 0.0386(8) 0.0231(6) 0.0246(7) 0.0014(5) 0.0094(6) 0.0096(6)
P8 0.0220(6) 0.0179(5) 0.0219(6) 0.0016(5) 0.0004(5) 0.0021(5)
C1 0.039(3) 0.024(3) 0.023(3) 0.002(2) 0.003(2) 0.004(2)
C2 0.038(3) 0.037(3) 0.045(4) 0.022(3) -0.002(3) -0.001(3)
C3 0.034(3) 0.024(3) 0.030(3) 0.006(2) 0.007(2) 0.000(2)
C6 0.031(3) 0.035(3) 0.029(3) -0.001(2) 0.008(2) 0.006(2)
C9 0.038(3) 0.020(2) 0.035(3) -0.002(2) 0.003(2) -0.001(2)
C8 0.047(4) 0.030(3) 0.037(3) -0.012(2) -0.003(3) 0.006(3)
C7 0.039(3) 0.052(4) 0.029(3) -0.013(3) 0.007(3) 0.000(3)
C5 0.029(3) 0.037(3) 0.035(3) 0.008(3) -0.002(3) 0.006(2)
C12 0.024(3) 0.043(3) 0.039(3) -0.004(3) 0.006(3) -0.008(2)
C10 0.036(3) 0.034(3) 0.046(4) 0.015(3) -0.002(3) 0.010(3)
C11 0.023(3) 0.027(3) 0.029(3) 0.008(2) 0.000(2) 0.006(2)
C13 0.040(3) 0.028(3) 0.041(4) 0.008(2) -0.010(3) -0.010(3)
C17 0.047(3) 0.035(3) 0.031(3) 0.000(3) -0.002(3) 0.014(3)
C15 0.037(3) 0.035(3) 0.034(3) 0.001(2) 0.010(3) 0.005(2)
C16 0.030(3) 0.030(3) 0.024(3) 0.001(2) 0.002(2) 0.009(2)
C14 0.024(2) 0.033(3) 0.027(3) -0.002(2) 0.002(2) 0.002(2)
C19 0.025(3) 0.034(3) 0.033(3) 0.003(2) -0.002(2) -0.006(2)
C22 0.048(4) 0.032(3) 0.025(3) 0.004(2) 0.002(3) 0.001(3)
C20 0.030(3) 0.039(3) 0.035(3) 0.002(2) -0.008(3) -0.003(2)
C21 0.032(3) 0.024(3) 0.024(3) 0.003(2) 0.003(2) -0.001(2)
C25 0.134(9) 0.034(4) 0.044(4) -0.009(3) 0.037(5) 0.000(5)
C26 0.050(4) 0.041(4) 0.052(4) 0.009(3) 0.025(3) 0.025(3)
C23 0.041(3) 0.025(3) 0.030(3) 0.002(2) 0.008(3) 0.009(2)
C24 0.081(5) 0.023(3) 0.036(3) -0.005(2) 0.010(4) 0.002(3)
C29 0.022(3) 0.047(4) 0.047(4) -0.007(3) 0.003(3) -0.007(3)
C32 0.031(3) 0.034(3) 0.025(3) -0.001(2) -0.002(2) 0.008(2)
C27 0.025(3) 0.045(4) 0.039(3) 0.006(3) -0.004(3) -0.001(3)
C30 0.026(3) 0.040(3) 0.036(3) -0.010(3) -0.001(2) 0.001(2)
C31 0.045(4) 0.047(4) 0.031(3) -0.009(3) -0.007(3) -0.001(3)
C33 0.045(4) 0.051(4) 0.038(4) -0.006(3) -0.019(3) 0.013(3)
C28 0.050(4) 0.027(3) 0.039(4) 0.007(2) 0.003(3) -0.009(3)
C35 0.024(2) 0.019(2) 0.025(3) -0.0012(19) 0.000(2) -0.0018(19)
C38 0.027(3) 0.047(4) 0.037(3) 0.000(3) -0.004(2) 0.011(3)
C37 0.033(3) 0.033(3) 0.026(3) -0.002(2) -0.002(2) -0.005(2)
C39 0.030(3) 0.055(4) 0.043(4) 0.013(3) -0.003(3) -0.011(3)
C36 0.028(3) 0.020(2) 0.029(3) -0.001(2) 0.004(2) -0.003(2)
C34 0.039(3) 0.021(3) 0.057(4) 0.006(3) 0.004(3) -0.005(2)
C41 0.037(3) 0.037(3) 0.024(3) -0.001(2) 0.008(2) 0.002(3)
C44 0.041(4) 0.036(3) 0.078(5) 0.015(3) 0.014(4) -0.010(3)
C40 0.026(2) 0.028(3) 0.027(3) 0.004(2) 0.008(2) 0.006(2)
C45 0.034(3) 0.040(3) 0.045(4) 0.004(3) -0.001(3) -0.016(3)
C42 0.056(4) 0.042(4) 0.038(3) 0.013(3) 0.011(3) 0.023(3)
C43 0.034(3) 0.040(3) 0.053(4) 0.011(3) -0.003(3) 0.009(3)
C46 0.029(3) 0.023(3) 0.030(3) -0.001(2) 0.001(2) 0.004(2)
C48 0.060(4) 0.049(4) 0.032(3) -0.003(3) 0.017(3) 0.016(3)
C47 0.051(4) 0.027(3) 0.047(4) -0.004(3) 0.002(3) 0.005(3)
C49 0.033(3) 0.028(3) 0.037(3) -0.004(2) 0.006(3) 0.002(2)
C50 0.055(4) 0.024(3) 0.038(3) -0.004(2) 0.014(3) -0.005(3)
C52 0.086(6) 0.044(4) 0.036(4) 0.004(3) -0.011(4) 0.032(4)
C51 0.052(4) 0.033(3) 0.028(3) -0.010(2) -0.002(3) -0.009(3)
C61 0.045(4) 0.063(5) 0.027(3) 0.013(3) -0.005(3) 0.014(3)
C57 0.035(3) 0.052(4) 0.051(4) -0.007(3) 0.011(3) -0.010(3)
C54 0.041(3) 0.030(3) 0.040(3) 0.004(3) 0.005(3) -0.014(3)
C59 0.021(3) 0.087(6) 0.049(4) -0.011(4) 0.004(3) -0.008(3)
C60 0.039(3) 0.045(4) 0.044(4) 0.007(3) 0.015(3) -0.007(3)
C58 0.018(3) 0.094(6) 0.042(4) -0.007(4) -0.006(3) 0.008(3)
C55 0.039(4) 0.048(4) 0.056(4) -0.017(3) -0.008(3) -0.011(3)
C53 0.036(3) 0.033(3) 0.050(4) -0.005(3) -0.004(3) -0.004(3)
C63 0.061(4) 0.035(3) 0.034(3) 0.009(2) 0.007(3) 0.007(3)
C62 0.043(3) 0.028(3) 0.036(3) 0.005(2) 0.008(3) 0.002(3)
C66 0.023(3) 0.054(4) 0.038(3) 0.016(3) 0.005(2) 0.003(3)
C64 0.067(5) 0.040(4) 0.042(4) 0.013(3) 0.007(4) 0.027(3)
C65 0.031(3) 0.052(4) 0.066(5) -0.010(4) -0.002(3) -0.015(3)
C68 0.086(6) 0.025(3) 0.052(4) -0.005(3) 0.011(4) -0.010(3)
C67 0.065(5) 0.040(4) 0.047(4) -0.002(3) -0.018(4) -0.009(3)
C70 0.067(5) 0.039(4) 0.043(4) -0.009(3) 0.012(4) 0.017(3)
C74 0.107(7) 0.036(4) 0.076(6) 0.007(4) 0.063(6) 0.027(4)
C69 0.035(3) 0.047(4) 0.044(4) -0.011(3) 0.004(3) 0.010(3)
C71 0.046(4) 0.044(4) 0.049(4) 0.024(3) 0.006(3) 0.011(3)
C73 0.072(5) 0.057(5) 0.038(4) 0.000(3) -0.025(4) 0.023(4)
C75 0.047(4) 0.046(4) 0.058(5) 0.004(3) 0.022(4) 0.014(3)
C72 0.053(4) 0.025(3) 0.060(5) 0.017(3) 0.006(3) 0.006(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 I1 2.5915(8) . ?
Fe1 P1 2.3013(15) . ?
Fe1 P2 2.2892(15) . ?
Fe1 P3 2.2714(15) . ?
Fe1 P4 2.2692(14) . ?
P1 C14 1.843(6) . ?
P1 C19 1.897(6) . ?
P1 C21 1.871(5) . ?
P2 C29 1.895(6) . ?
P2 C32 1.849(6) . ?
P2 C30 1.845(6) . ?
P3 C5 1.883(6) . ?
P3 C34 1.866(6) . ?
P3 C46 1.829(6) . ?
P4 C6 1.890(6) . ?
P4 C9 1.868(6) . ?
P4 C16 1.819(6) . ?
Fe2 I2 2.5924(7) . ?
Fe2 P5 2.2964(15) . ?
Fe2 P6 2.2821(15) . ?
Fe2 P7 2.2641(15) . ?
Fe2 P8 2.2694(14) . ?
P5 C1 1.851(6) . ?
P5 C13 1.890(6) . ?
P5 C40 1.857(5) . ?
P6 C12 1.897(6) . ?
P6 C38 1.865(6) . ?
P6 C36 1.848(6) . ?
P7 C26 1.862(7) . ?
P7 C23 1.827(6) . ?
P7 C24 1.889(7) . ?
P8 C3 1.899(5) . ?
P8 C11 1.865(5) . ?
P8 C35 1.828(5) . ?
C1 C23 1.397(8) . ?
C1 C62 1.390(8) . ?
C2 C3 1.543(8) . ?
C2 C10 1.532(9) . ?
C3 C28 1.522(8) . ?
C6 C7 1.551(9) . ?
C6 C69 1.540(9) . ?
C9 C8 1.531(8) . ?
C9 C53 1.529(9) . ?
C8 C7 1.515(9) . ?
C5 C43 1.529(9) . ?
C5 C71 1.539(9) . ?
C12 C59 1.535(9) . ?
C12 C60 1.524(9) . ?
C10 C11 1.536(8) . ?
C11 C27 1.526(8) . ?
C13 C39 1.543(10) . ?
C13 C67 1.531(9) . ?
C17 C16 1.407(8) . ?
C17 C52 1.376(9) . ?
C15 C14 1.393(8) . ?
C15 C48 1.398(9) . ?
C16 C32 1.403(8) . ?
C14 C46 1.397(8) . ?
C19 C20 1.520(8) . ?
C19 C45 1.534(8) . ?
C22 C21 1.525(8) . ?
C21 C54 1.523(8) . ?
C25 C24 1.518(11) . ?
C25 C74 1.514(14) . ?
C26 C74 1.560(11) . ?
C26 C75 1.516(10) . ?
C23 C42 1.387(8) . ?
C24 C68 1.546(9) . ?
C29 C57 1.542(10) . ?
C29 C65 1.528(9) . ?
C32 C33 1.398(8) . ?
C30 C31 1.536(9) . ?
C30 C55 1.531(9) . ?
C33 C73 1.395(10) . ?
C35 C36 1.405(8) . ?
C35 C49 1.387(7) . ?
C38 C61 1.519(9) . ?
C38 C58 1.525(9) . ?
C37 C36 1.387(8) . ?
C37 C51 1.385(9) . ?
C39 C66 1.510(9) . ?
C34 C44 1.531(9) . ?
C34 C72 1.523(9) . ?
C41 C40 1.520(8) . ?
C40 C66 1.538(8) . ?
C45 C54 1.521(9) . ?
C42 C64 1.408(9) . ?
C46 C47 1.405(8) . ?
C48 C70 1.363(10) . ?
C47 C70 1.374(10) . ?
C49 C50 1.390(9) . ?
C50 C51 1.395(10) . ?
C52 C73 1.371(12) . ?
C59 C58 1.523(11) . ?
C55 C65 1.532(11) . ?
C63 C62 1.391(9) . ?
C63 C64 1.378(10) . ?
C71 C72 1.539(11) . ?
Cl1 O1 1.595(5) . ?
Cl1 O3 1.451(7) . ?
Cl1 O2 1.375(12) . ?
Cl1 O4 1.329(7) . ?
Cl1 O9 1.251(10) . ?
Cl2 O5 1.472(9) . ?
Cl2 O6 1.417(8) . ?
Cl2 O7 1.270(8) . ?
Cl2 O8 1.499(14) . ?
Cl2 O10 1.480(17) . ?
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
P1 Fe1 I1 121.62(5) . . ?
P2 Fe1 I1 116.67(5) . . ?
P2 Fe1 P1 121.71(6) . . ?
P3 Fe1 I1 89.89(4) . . ?
P3 Fe1 P1 81.46(5) . . ?
P3 Fe1 P2 99.48(6) . . ?
P4 Fe1 I1 89.92(4) . . ?
P4 Fe1 P1 97.90(5) . . ?
P4 Fe1 P2 81.39(5) . . ?
P4 Fe1 P3 179.10(6) . . ?
C14 P1 Fe1 105.06(19) . . ?
C14 P1 C19 102.6(3) . . ?
C14 P1 C21 108.0(3) . . ?
C19 P1 Fe1 128.80(19) . . ?
C21 P1 Fe1 117.04(19) . . ?
C21 P1 C19 93.4(2) . . ?
C29 P2 Fe1 129.9(2) . . ?
C32 P2 Fe1 104.61(19) . . ?
C32 P2 C29 103.0(3) . . ?
C30 P2 Fe1 116.7(2) . . ?
C30 P2 C29 93.4(3) . . ?
C30 P2 C32 107.2(3) . . ?
C5 P3 Fe1 118.1(2) . . ?
C34 P3 Fe1 126.7(2) . . ?
C34 P3 C5 94.2(3) . . ?
C46 P3 Fe1 105.41(18) . . ?
C46 P3 C5 103.3(3) . . ?
C46 P3 C34 106.7(3) . . ?
C6 P4 Fe1 119.96(19) . . ?
C9 P4 Fe1 125.49(19) . . ?
C9 P4 C6 93.9(3) . . ?
C16 P4 Fe1 104.47(18) . . ?
C16 P4 C6 102.7(3) . . ?
C16 P4 C9 108.0(3) . . ?
P5 Fe2 I2 121.90(5) . . ?
P6 Fe2 I2 116.04(5) . . ?
P6 Fe2 P5 122.06(6) . . ?
P7 Fe2 I2 89.65(4) . . ?
P7 Fe2 P5 81.01(5) . . ?
P7 Fe2 P6 99.74(6) . . ?
P7 Fe2 P8 178.85(6) . . ?
P8 Fe2 I2 90.51(4) . . ?
P8 Fe2 P5 97.94(5) . . ?
P8 Fe2 P6 81.21(5) . . ?
C1 P5 Fe2 105.52(19) . . ?
C1 P5 C13 102.3(3) . . ?
C1 P5 C40 106.6(2) . . ?
C13 P5 Fe2 130.7(2) . . ?
C40 P5 Fe2 115.65(18) . . ?
C40 P5 C13 93.7(3) . . ?
C12 P6 Fe2 129.2(2) . . ?
C38 P6 Fe2 116.2(2) . . ?
C38 P6 C12 93.5(3) . . ?
C36 P6 Fe2 105.48(18) . . ?
C36 P6 C12 103.2(3) . . ?
C36 P6 C38 107.4(3) . . ?
C26 P7 Fe2 126.8(2) . . ?
C26 P7 C24 94.9(4) . . ?
C23 P7 Fe2 105.84(18) . . ?
C23 P7 C26 106.6(3) . . ?
C23 P7 C24 103.3(3) . . ?
C24 P7 Fe2 117.0(2) . . ?
C3 P8 Fe2 119.21(18) . . ?
C11 P8 Fe2 126.00(18) . . ?
C11 P8 C3 93.9(2) . . ?
C35 P8 Fe2 105.14(17) . . ?
C35 P8 C3 103.0(2) . . ?
C35 P8 C11 107.2(3) . . ?
C23 C1 P5 115.9(4) . . ?
C62 C1 P5 124.5(5) . . ?
C62 C1 C23 119.6(5) . . ?
C10 C2 C3 107.5(5) . . ?
C2 C3 P8 104.6(4) . . ?
C28 C3 P8 114.7(4) . . ?
C28 C3 C2 111.3(5) . . ?
C7 C6 P4 104.8(4) . . ?
C69 C6 P4 114.2(4) . . ?
C69 C6 C7 110.4(5) . . ?
C8 C9 P4 104.5(4) . . ?
C53 C9 P4 110.8(4) . . ?
C53 C9 C8 111.1(5) . . ?
C7 C8 C9 106.8(5) . . ?
C8 C7 C6 108.6(5) . . ?
C43 C5 P3 115.5(5) . . ?
C43 C5 C71 111.1(5) . . ?
C71 C5 P3 104.4(4) . . ?
C59 C12 P6 105.4(5) . . ?
C60 C12 P6 118.4(4) . . ?
C60 C12 C59 114.0(5) . . ?
C2 C10 C11 106.2(5) . . ?
C10 C11 P8 104.5(4) . . ?
C27 C11 P8 110.8(4) . . ?
C27 C11 C10 111.1(5) . . ?
C39 C13 P5 105.0(4) . . ?
C67 C13 P5 117.9(5) . . ?
C67 C13 C39 114.2(6) . . ?
C52 C17 C16 119.1(6) . . ?
C14 C15 C48 119.9(6) . . ?
C17 C16 P4 125.1(5) . . ?
C32 C16 P4 114.3(4) . . ?
C32 C16 C17 120.2(5) . . ?
C15 C14 P1 124.3(5) . . ?
C15 C14 C46 119.3(5) . . ?
C46 C14 P1 116.4(4) . . ?
C20 C19 P1 118.5(4) . . ?
C20 C19 C45 115.1(5) . . ?
C45 C19 P1 105.7(4) . . ?
C22 C21 P1 116.9(4) . . ?
C54 C21 P1 106.1(4) . . ?
C54 C21 C22 115.2(5) . . ?
C74 C25 C24 108.7(6) . . ?
C74 C26 P7 103.1(6) . . ?
C75 C26 P7 113.9(5) . . ?
C75 C26 C74 111.4(6) . . ?
C1 C23 P7 114.0(4) . . ?
C42 C23 P7 125.5(5) . . ?
C42 C23 C1 120.2(5) . . ?
C25 C24 P7 103.9(6) . . ?
C25 C24 C68 109.8(6) . . ?
C68 C24 P7 114.1(5) . . ?
C57 C29 P2 117.0(4) . . ?
C65 C29 P2 106.2(4) . . ?
C65 C29 C57 114.7(6) . . ?
C16 C32 P2 115.8(4) . . ?
C33 C32 P2 125.0(5) . . ?
C33 C32 C16 119.2(6) . . ?
C31 C30 P2 116.2(4) . . ?
C55 C30 P2 106.9(4) . . ?
C55 C30 C31 115.3(5) . . ?
C73 C33 C32 119.5(7) . . ?
C36 C35 P8 113.8(4) . . ?
C49 C35 P8 125.5(4) . . ?
C49 C35 C36 120.4(5) . . ?
C61 C38 P6 116.8(4) . . ?
C61 C38 C58 114.8(6) . . ?
C58 C38 P6 105.4(5) . . ?
C51 C37 C36 120.2(6) . . ?
C66 C39 C13 108.0(5) . . ?
C35 C36 P6 115.8(4) . . ?
C37 C36 P6 125.0(4) . . ?
C37 C36 C35 119.2(5) . . ?
C44 C34 P3 112.2(4) . . ?
C72 C34 P3 104.3(4) . . ?
C72 C34 C44 111.7(6) . . ?
C41 C40 P5 116.5(4) . . ?
C41 C40 C66 116.4(5) . . ?
C66 C40 P5 105.6(4) . . ?
C54 C45 C19 108.9(5) . . ?
C23 C42 C64 119.6(6) . . ?
C14 C46 P3 114.5(4) . . ?
C14 C46 C47 119.7(5) . . ?
C47 C46 P3 125.6(5) . . ?
C70 C48 C15 120.3(6) . . ?
C70 C47 C46 119.7(6) . . ?
C35 C49 C50 120.0(6) . . ?
C49 C50 C51 119.5(6) . . ?
C73 C52 C17 121.1(7) . . ?
C37 C51 C50 120.5(6) . . ?
C45 C54 C21 108.3(5) . . ?
C58 C59 C12 108.3(5) . . ?
C59 C58 C38 107.6(5) . . ?
C30 C55 C65 107.3(5) . . ?
C64 C63 C62 120.2(6) . . ?
C1 C62 C63 120.3(6) . . ?
C39 C66 C40 107.2(5) . . ?
C63 C64 C42 120.0(6) . . ?
C29 C65 C55 109.2(6) . . ?
C48 C70 C47 121.0(6) . . ?
C25 C74 C26 106.3(6) . . ?
C72 C71 C5 106.1(5) . . ?
C52 C73 C33 120.7(6) . . ?
C34 C72 C71 106.9(5) . . ?
O3 Cl1 O1 97.0(3) . . ?
O2 Cl1 O1 100.0(5) . . ?
O2 Cl1 O3 99.0(6) . . ?
O4 Cl1 O1 102.6(4) . . ?
O4 Cl1 O3 108.7(4) . . ?
O4 Cl1 O2 141.4(7) . . ?
O9 Cl1 O1 104.0(5) . . ?
O9 Cl1 O3 127.6(6) . . ?
O9 Cl1 O4 112.5(6) . . ?
O5 Cl2 O8 87.8(7) . . ?
O5 Cl2 O10 121.6(9) . . ?
O6 Cl2 O5 101.8(6) . . ?
O6 Cl2 O8 106.1(7) . . ?
O6 Cl2 O10 100.4(8) . . ?
O7 Cl2 O5 110.4(6) . . ?
O7 Cl2 O6 119.3(6) . . ?
O7 Cl2 O8 124.6(7) . . ?
O7 Cl2 O10 104.1(8) . . ?
_shelx_res_file
;
TITL str1619 in P212121 #19
str1619.res
created by SHELXL-2018/3 at 12:50:33 on 23-Aug-2019
REM reset to P212121 #19
CELL 0.71073 11.237469 20.919523 33.725773 90 90 90
ZERR 8 0.000145 0.000268 0.000442 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl Fe I O P
UNIT 288 448 8 8 8 32 32
L.S. 10
PLAN 20
SIZE 0.0625 0.187 0.2894
fmap 2
acta
REM
REM
REM
WGHT 0.049800 11.115101
FVAR 0.55118
FE1 4 0.695432 0.830134 0.099833 11.00000 0.01910 0.01894 =
0.01881 0.00190 0.00056 0.00010
I1 5 0.704528 0.841877 0.023398 11.00000 0.03668 0.03668 =
0.02095 0.00652 0.00107 0.00168
P1 7 0.523753 0.799197 0.131704 11.00000 0.02143 0.02196 =
0.02105 0.00117 0.00169 -0.00215
P2 7 0.867005 0.851332 0.133982 11.00000 0.02127 0.02907 =
0.02692 -0.00185 -0.00113 -0.00052
P3 7 0.606331 0.927330 0.104270 11.00000 0.02501 0.01998 =
0.03007 0.00377 0.00118 0.00020
P4 7 0.781689 0.732351 0.095104 11.00000 0.02474 0.02233 =
0.02116 -0.00023 0.00189 0.00306
FE2 4 0.711090 1.163534 -0.097787 11.00000 0.02125 0.01762 =
0.01654 0.00026 0.00191 0.00082
I2 5 0.714643 1.158976 -0.020981 11.00000 0.04655 0.03170 =
0.01823 -0.00065 0.00030 0.00070
P5 7 0.850883 1.219621 -0.133232 11.00000 0.02549 0.02180 =
0.02085 0.00281 0.00077 -0.00089
P6 7 0.560679 1.108759 -0.127998 11.00000 0.01854 0.03050 =
0.02295 -0.00073 0.00118 0.00026
P7 7 0.627426 1.261866 -0.094703 11.00000 0.03863 0.02315 =
0.02458 0.00141 0.00939 0.00962
P8 7 0.798579 1.065904 -0.101064 11.00000 0.02198 0.01792 =
0.02190 0.00163 0.00040 0.00214
C1 1 0.767572 1.283864 -0.158807 11.00000 0.03861 0.02405 =
0.02297 0.00188 0.00305 0.00368
C2 1 0.870530 0.978482 -0.045869 11.00000 0.03844 0.03664 =
0.04524 0.02170 -0.00216 -0.00118
AFIX 23
H2A 2 0.892547 1.005780 -0.023808 11.00000 -1.20000
H2B 2 0.862025 0.935077 -0.036157 11.00000 -1.20000
AFIX 0
C3 1 0.752559 1.001595 -0.064412 11.00000 0.03382 0.02409 =
0.02992 0.00613 0.00720 -0.00021
AFIX 13
H3 2 0.703935 1.021273 -0.043607 11.00000 -1.20000
AFIX 0
C6 1 0.908450 0.719076 0.059185 11.00000 0.03140 0.03504 =
0.02892 -0.00080 0.00834 0.00597
AFIX 13
H6 2 0.912942 0.755453 0.040937 11.00000 -1.20000
AFIX 0
C9 1 0.703749 0.656764 0.081187 11.00000 0.03771 0.01999 =
0.03455 -0.00151 0.00331 -0.00105
AFIX 13
H9 2 0.671781 0.635886 0.104919 11.00000 -1.20000
AFIX 0
C8 1 0.800822 0.615194 0.062519 11.00000 0.04729 0.03043 =
0.03655 -0.01175 -0.00264 0.00610
AFIX 23
H8A 2 0.851231 0.596932 0.082934 11.00000 -1.20000
H8B 2 0.765472 0.580627 0.047395 11.00000 -1.20000
AFIX 0
C7 1 0.872867 0.658351 0.035600 11.00000 0.03912 0.05150 =
0.02918 -0.01290 0.00700 -0.00004
AFIX 23
H7A 2 0.826039 0.670164 0.012577 11.00000 -1.20000
H7B 2 0.943641 0.636172 0.026554 11.00000 -1.20000
AFIX 0
C5 1 0.484717 0.946844 0.067818 11.00000 0.02882 0.03695 =
0.03526 0.00765 -0.00214 0.00642
AFIX 13
H5 2 0.481199 0.912692 0.047962 11.00000 -1.20000
AFIX 0
C12 1 0.432749 1.062852 -0.104836 11.00000 0.02403 0.04317 =
0.03924 -0.00435 0.00618 -0.00797
AFIX 13
H12 2 0.434308 1.020220 -0.116869 11.00000 -1.20000
AFIX 0
C10 1 0.966040 0.981282 -0.078245 11.00000 0.03577 0.03385 =
0.04580 0.01483 -0.00166 0.01016
AFIX 23
H10A 2 0.950004 0.949799 -0.098673 11.00000 -1.20000
H10B 2 1.044061 0.972878 -0.067100 11.00000 -1.20000
AFIX 0
C11 1 0.960712 1.049134 -0.095566 11.00000 0.02305 0.02711 =
0.02893 0.00751 0.00013 0.00587
AFIX 13
H11 2 0.999737 1.050222 -0.121543 11.00000 -1.20000
AFIX 0
C13 1 0.990001 1.262526 -0.116381 11.00000 0.03954 0.02798 =
0.04120 0.00768 -0.00951 -0.01023
AFIX 13
H13 2 0.985769 1.305663 -0.127624 11.00000 -1.20000
AFIX 0
C17 1 0.868861 0.660531 0.161503 11.00000 0.04685 0.03463 =
0.03103 -0.00001 -0.00223 0.01433
AFIX 43
H17 2 0.834448 0.623873 0.150926 11.00000 -1.20000
AFIX 0
C15 1 0.409088 0.863944 0.196237 11.00000 0.03714 0.03451 =
0.03433 0.00146 0.01045 0.00450
AFIX 43
H15 2 0.373703 0.825253 0.202976 11.00000 -1.20000
AFIX 0
C16 1 0.852304 0.720193 0.143058 11.00000 0.03046 0.03039 =
0.02377 0.00102 0.00201 0.00880
C14 1 0.482382 0.867899 0.163016 11.00000 0.02409 0.03262 =
0.02654 -0.00225 0.00198 0.00182
C19 1 0.375760 0.774448 0.109418 11.00000 0.02497 0.03356 =
0.03275 0.00300 -0.00152 -0.00608
AFIX 13
H19 2 0.315787 0.800701 0.122829 11.00000 -1.20000
AFIX 0
C22 1 0.590791 0.735482 0.204699 11.00000 0.04793 0.03174 =
0.02550 0.00438 0.00213 0.00139
AFIX 137
H22A 2 0.666089 0.756582 0.201618 11.00000 -1.50000
H22B 2 0.602808 0.694411 0.216748 11.00000 -1.50000
H22C 2 0.539900 0.760901 0.221255 11.00000 -1.50000
AFIX 0
C20 1 0.355689 0.785106 0.065352 11.00000 0.03046 0.03885 =
0.03542 0.00213 -0.00842 -0.00346
AFIX 137
H20A 2 0.341344 0.829670 0.060522 11.00000 -1.50000
H20B 2 0.288101 0.760665 0.056793 11.00000 -1.50000
H20C 2 0.424942 0.771717 0.050902 11.00000 -1.50000
AFIX 0
C21 1 0.532927 0.726828 0.164148 11.00000 0.03169 0.02381 =
0.02428 0.00279 0.00252 -0.00086
AFIX 13
H21 2 0.582855 0.696096 0.149857 11.00000 -1.20000
AFIX 0
C25 1 0.588305 1.341991 -0.033578 11.00000 0.13357 0.03414 =
0.04403 -0.00932 0.03694 -0.00027
AFIX 23
H25A 2 0.573466 1.311628 -0.012410 11.00000 -1.20000
H25B 2 0.604829 1.383331 -0.021772 11.00000 -1.20000
AFIX 0
C26 1 0.470142 1.280868 -0.081896 11.00000 0.04965 0.04096 =
0.05184 0.00902 0.02507 0.02494
AFIX 13
H26 2 0.423895 1.286155 -0.106312 11.00000 -1.20000
AFIX 0
C23 1 0.656679 1.299196 -0.142685 11.00000 0.04074 0.02453 =
0.03031 0.00234 0.00781 0.00938
C24 1 0.693954 1.320303 -0.058195 11.00000 0.08135 0.02311 =
0.03625 -0.00492 0.00980 0.00163
AFIX 13
H24 2 0.751314 1.298118 -0.041174 11.00000 -1.20000
AFIX 0
C29 1 1.017192 0.879283 0.115179 11.00000 0.02155 0.04696 =
0.04734 -0.00740 0.00276 -0.00651
AFIX 13
H29 2 1.075217 0.847823 0.124653 11.00000 -1.20000
AFIX 0
C32 1 0.903148 0.775502 0.159413 11.00000 0.03057 0.03429 =
0.02519 -0.00055 -0.00161 0.00840
C27 1 1.018790 1.097415 -0.067686 11.00000 0.02465 0.04497 =
0.03891 0.00580 -0.00392 -0.00081
AFIX 137
H27A 2 1.010400 1.139640 -0.078476 11.00000 -1.50000
H27B 2 1.101736 1.087447 -0.064824 11.00000 -1.50000
H27C 2 0.980761 1.095521 -0.042224 11.00000 -1.50000
AFIX 0
C30 1 0.858921 0.914045 0.172358 11.00000 0.02603 0.03980 =
0.03631 -0.01043 -0.00117 0.00118
AFIX 13
H30 2 0.813812 0.949255 0.160464 11.00000 -1.20000
AFIX 0
C31 1 0.792371 0.896380 0.210617 11.00000 0.04458 0.04677 =
0.03149 -0.00852 -0.00746 -0.00143
AFIX 137
H31A 2 0.714714 0.880420 0.204083 11.00000 -1.50000
H31B 2 0.784717 0.933621 0.227053 11.00000 -1.50000
H31C 2 0.836103 0.864062 0.224620 11.00000 -1.50000
AFIX 0
C33 1 0.976370 0.769969 0.192760 11.00000 0.04497 0.05133 =
0.03807 -0.00638 -0.01888 0.01301
AFIX 43
H33 2 1.013591 0.805890 0.203254 11.00000 -1.20000
AFIX 0
C28 1 0.683240 0.946292 -0.082462 11.00000 0.04954 0.02686 =
0.03929 0.00713 0.00347 -0.00921
AFIX 137
H28A 2 0.614340 0.962528 -0.095945 11.00000 -1.50000
H28B 2 0.658714 0.917543 -0.061835 11.00000 -1.50000
H28C 2 0.732937 0.923916 -0.100994 11.00000 -1.50000
AFIX 0
C35 1 0.752075 1.032672 -0.148736 11.00000 0.02394 0.01885 =
0.02483 -0.00120 0.00025 -0.00185
C38 1 0.461015 1.156479 -0.160863 11.00000 0.02677 0.04651 =
0.03652 -0.00043 -0.00387 0.01086
AFIX 13
H38 2 0.445010 1.196599 -0.146842 11.00000 -1.20000
AFIX 0
C37 1 0.583174 1.018080 -0.191693 11.00000 0.03282 0.03306 =
0.02613 -0.00162 -0.00211 -0.00454
AFIX 43
H37 2 0.503757 1.025698 -0.197845 11.00000 -1.20000
AFIX 0
C39 1 1.093028 1.228341 -0.137949 11.00000 0.02970 0.05505 =
0.04325 0.01255 -0.00309 -0.01136
AFIX 23
H39A 2 1.160497 1.256951 -0.140575 11.00000 -1.20000
H39B 2 1.118058 1.191136 -0.122946 11.00000 -1.20000
AFIX 0
C36 1 0.634595 1.048091 -0.159277 11.00000 0.02839 0.02039 =
0.02867 -0.00079 0.00391 -0.00336
C34 1 0.680108 1.006906 0.099560 11.00000 0.03933 0.02114 =
0.05688 0.00642 0.00391 -0.00495
AFIX 13
H34 2 0.698274 1.023644 0.126017 11.00000 -1.20000
AFIX 0
C41 1 0.859181 1.158597 -0.209626 11.00000 0.03719 0.03739 =
0.02351 -0.00130 0.00848 0.00158
AFIX 137
H41A 2 0.788661 1.135296 -0.202610 11.00000 -1.50000
H41B 2 0.907018 1.133208 -0.227181 11.00000 -1.50000
H41C 2 0.837265 1.197689 -0.222624 11.00000 -1.50000
AFIX 0
C44 1 0.794535 1.003506 0.075030 11.00000 0.04087 0.03630 =
0.07777 0.01493 0.01443 -0.01030
AFIX 137
H44A 2 0.844311 0.969887 0.085046 11.00000 -1.50000
H44B 2 0.836033 1.043512 0.076833 11.00000 -1.50000
H44C 2 0.775026 0.994985 0.047826 11.00000 -1.50000
AFIX 0
C40 1 0.929781 1.173792 -0.172365 11.00000 0.02559 0.02758 =
0.02702 0.00398 0.00774 0.00613
AFIX 13
H40 2 0.949481 1.132402 -0.160442 11.00000 -1.20000
AFIX 0
C45 1 0.353871 0.705931 0.123844 11.00000 0.03443 0.04034 =
0.04454 0.00416 -0.00108 -0.01583
AFIX 23
H45A 2 0.269066 0.697481 0.124978 11.00000 -1.20000
H45B 2 0.389694 0.675739 0.105567 11.00000 -1.20000
AFIX 0
C42 1 0.584783 1.344316 -0.160992 11.00000 0.05554 0.04215 =
0.03828 0.01327 0.01090 0.02317
AFIX 43
H42 2 0.510919 1.354513 -0.150284 11.00000 -1.20000
AFIX 0
C43 1 0.360609 0.955429 0.085637 11.00000 0.03357 0.04039 =
0.05271 0.01083 -0.00322 0.00936
AFIX 137
H43A 2 0.339004 0.917628 0.100082 11.00000 -1.50000
H43B 2 0.304096 0.962581 0.064756 11.00000 -1.50000
H43C 2 0.360814 0.991467 0.103259 11.00000 -1.50000
AFIX 0
C46 1 0.529073 0.927184 0.151992 11.00000 0.02930 0.02341 =
0.03035 -0.00083 0.00112 0.00449
C48 1 0.388838 0.918254 0.219423 11.00000 0.06000 0.04907 =
0.03196 -0.00337 0.01737 0.01622
AFIX 43
H48 2 0.341343 0.915386 0.241935 11.00000 -1.20000
AFIX 0
C47 1 0.506959 0.981171 0.175638 11.00000 0.05125 0.02708 =
0.04664 -0.00391 0.00186 0.00452
AFIX 43
H47 2 0.538599 1.020659 0.168616 11.00000 -1.20000
AFIX 0
C49 1 0.818395 0.991114 -0.171951 11.00000 0.03314 0.02838 =
0.03700 -0.00421 0.00559 0.00207
AFIX 43
H49 2 0.896190 0.981151 -0.164860 11.00000 -1.20000
AFIX 0
C50 1 0.768495 0.964372 -0.205818 11.00000 0.05499 0.02448 =
0.03825 -0.00449 0.01390 -0.00532
AFIX 43
H50 2 0.814004 0.938387 -0.222270 11.00000 -1.20000
AFIX 0
C52 1 0.936677 0.657167 0.195412 11.00000 0.08557 0.04437 =
0.03574 0.00375 -0.01149 0.03177
AFIX 43
H52 2 0.944315 0.618287 0.208539 11.00000 -1.20000
AFIX 0
C51 1 0.649663 0.976796 -0.214946 11.00000 0.05235 0.03265 =
0.02759 -0.00981 -0.00151 -0.00931
AFIX 43
H51 2 0.614802 0.957217 -0.236808 11.00000 -1.20000
AFIX 0
C61 1 0.510106 1.174918 -0.201251 11.00000 0.04537 0.06293 =
0.02740 0.01333 -0.00522 0.01428
AFIX 137
H61A 2 0.587587 1.193568 -0.198103 11.00000 -1.50000
H61B 2 0.457841 1.205328 -0.213546 11.00000 -1.50000
H61C 2 0.515907 1.137507 -0.217623 11.00000 -1.50000
AFIX 0
C57 1 1.033756 0.882934 0.069836 11.00000 0.03540 0.05235 =
0.05124 -0.00718 0.01098 -0.00967
AFIX 137
H57A 2 1.021294 0.841395 0.058474 11.00000 -1.50000
H57B 2 1.113001 0.897179 0.063922 11.00000 -1.50000
H57C 2 0.977282 0.912503 0.058892 11.00000 -1.50000
AFIX 0
C54 1 0.408390 0.698123 0.164824 11.00000 0.04117 0.03024 =
0.03976 0.00410 0.00492 -0.01370
AFIX 23
H54A 2 0.412448 0.653180 0.171770 11.00000 -1.20000
H54B 2 0.359834 0.719823 0.184427 11.00000 -1.20000
AFIX 0
C59 1 0.319307 1.095288 -0.120276 11.00000 0.02087 0.08727 =
0.04909 -0.01069 0.00407 -0.00846
AFIX 23
H59A 2 0.254155 1.064881 -0.120753 11.00000 -1.20000
H59B 2 0.297373 1.130450 -0.103010 11.00000 -1.20000
AFIX 0
C60 1 0.433816 1.052215 -0.060141 11.00000 0.03876 0.04470 =
0.04383 0.00672 0.01466 -0.00697
AFIX 137
H60A 2 0.496694 1.023125 -0.053380 11.00000 -1.50000
H60B 2 0.358885 1.034548 -0.051968 11.00000 -1.50000
H60C 2 0.446543 1.092272 -0.046915 11.00000 -1.50000
AFIX 0
C58 1 0.343612 1.119996 -0.161978 11.00000 0.01777 0.09390 =
0.04168 -0.00682 -0.00593 0.00775
AFIX 23
H58A 2 0.279736 1.148014 -0.170474 11.00000 -1.20000
H58B 2 0.348901 1.084581 -0.180459 11.00000 -1.20000
AFIX 0
C55 1 0.985529 0.939412 0.178193 11.00000 0.03875 0.04789 =
0.05627 -0.01690 -0.00814 -0.01141
AFIX 23
H55A 2 1.029705 0.911559 0.195859 11.00000 -1.20000
H55B 2 0.983427 0.981908 0.189676 11.00000 -1.20000
AFIX 0
C53 1 0.603613 0.670063 0.051615 11.00000 0.03629 0.03294 =
0.04975 -0.00522 -0.00390 -0.00432
AFIX 137
H53A 2 0.543826 0.696017 0.064034 11.00000 -1.50000
H53B 2 0.568911 0.630360 0.043243 11.00000 -1.50000
H53C 2 0.635238 0.692160 0.029002 11.00000 -1.50000
AFIX 0
C63 1 0.736532 1.361981 -0.210361 11.00000 0.06100 0.03483 =
0.03390 0.00888 0.00728 0.00678
AFIX 43
H63 2 0.764697 1.384201 -0.232324 11.00000 -1.20000
AFIX 0
C62 1 0.807809 1.316150 -0.192246 11.00000 0.04297 0.02844 =
0.03605 0.00492 0.00826 0.00193
AFIX 43
H62 2 0.882694 1.307064 -0.202544 11.00000 -1.20000
AFIX 0
C66 1 1.049193 1.208330 -0.178410 11.00000 0.02306 0.05392 =
0.03805 0.01616 0.00482 0.00254
AFIX 23
H66A 2 1.106233 1.179948 -0.190903 11.00000 -1.20000
H66B 2 1.038554 1.245498 -0.195236 11.00000 -1.20000
AFIX 0
C64 1 0.624311 1.374569 -0.195870 11.00000 0.06697 0.04006 =
0.04156 0.01322 0.00696 0.02711
AFIX 43
H64 2 0.574716 1.403031 -0.209123 11.00000 -1.20000
AFIX 0
C65 1 1.044736 0.941310 0.137300 11.00000 0.03094 0.05215 =
0.06575 -0.00995 -0.00174 -0.01529
AFIX 23
H65A 2 1.014982 0.977530 0.122328 11.00000 -1.20000
H65B 2 1.130120 0.946140 0.140275 11.00000 -1.20000
AFIX 0
C68 1 0.754271 1.378808 -0.077679 11.00000 0.08650 0.02473 =
0.05245 -0.00487 0.01133 -0.01010
AFIX 137
H68A 2 0.817176 1.364592 -0.094801 11.00000 -1.50000
H68B 2 0.786531 1.406043 -0.057446 11.00000 -1.50000
H68C 2 0.696569 1.402127 -0.092890 11.00000 -1.50000
AFIX 0
C67 1 1.009315 1.270992 -0.071744 11.00000 0.06500 0.03974 =
0.04662 -0.00207 -0.01849 -0.00901
AFIX 137
H67A 2 0.949194 1.298849 -0.061238 11.00000 -1.50000
H67B 2 1.086424 1.289293 -0.067133 11.00000 -1.50000
H67C 2 1.004434 1.230141 -0.058878 11.00000 -1.50000
AFIX 0
C70 1 0.438394 0.975412 0.209187 11.00000 0.06702 0.03911 =
0.04287 -0.00864 0.01158 0.01742
AFIX 43
H70 2 0.425608 1.011016 0.225140 11.00000 -1.20000
AFIX 0
C74 1 0.480354 1.346560 -0.060266 11.00000 0.10742 0.03566 =
0.07563 0.00705 0.06258 0.02674
AFIX 23
H74A 2 0.490224 1.380847 -0.079347 11.00000 -1.20000
H74B 2 0.409353 1.354859 -0.044741 11.00000 -1.20000
AFIX 0
C69 1 1.030517 0.709671 0.079095 11.00000 0.03537 0.04746 =
0.04405 -0.01111 0.00378 0.01012
AFIX 137
H69A 2 1.048832 0.746370 0.095058 11.00000 -1.50000
H69B 2 1.090511 0.704527 0.059083 11.00000 -1.50000
H69C 2 1.028309 0.672252 0.095556 11.00000 -1.50000
AFIX 0
C71 1 0.527233 1.008526 0.047358 11.00000 0.04590 0.04390 =
0.04876 0.02352 0.00582 0.01082
AFIX 23
H71A 2 0.583671 0.998678 0.026471 11.00000 -1.20000
H71B 2 0.460411 1.031296 0.035869 11.00000 -1.20000
AFIX 0
C73 1 0.993159 0.710138 0.210170 11.00000 0.07157 0.05736 =
0.03783 -0.00006 -0.02548 0.02320
AFIX 43
H73 2 1.043167 0.706164 0.232003 11.00000 -1.20000
AFIX 0
C75 1 0.410874 1.231208 -0.055782 11.00000 0.04690 0.04610 =
0.05809 0.00383 0.02151 0.01421
AFIX 137
H75A 2 0.417516 1.189909 -0.067993 11.00000 -1.50000
H75B 2 0.328362 1.241830 -0.052468 11.00000 -1.50000
H75C 2 0.449214 1.230441 -0.030349 11.00000 -1.50000
AFIX 0
C72 1 0.586722 1.049047 0.079870 11.00000 0.05254 0.02460 =
0.05984 0.01654 0.00636 0.00638
AFIX 23
H72A 2 0.623763 1.086597 0.068365 11.00000 -1.20000
H72B 2 0.528130 1.062861 0.099174 11.00000 -1.20000
AFIX 0
CL1 3 0.660661 0.535836 0.183206 11.00000 0.06882
CL2 3 0.262815 1.376764 -0.184800 11.00000 0.11718
O1 6 0.606713 0.465628 0.187323 11.00000 0.04522
O3 6 0.768994 0.524340 0.205502 11.00000 0.07271
PART 1
O2 6 0.706469 0.532272 0.145456 10.51000 0.06012
PART 0
O4 6 0.587106 0.570552 0.205329 11.00000 0.08088
O5 6 0.284440 1.355471 -0.143834 11.00000 0.10404
O6 6 0.137026 1.374205 -0.187126 11.00000 0.08352
O7 6 0.315592 1.429420 -0.191316 11.00000 0.09515
PART 1
O8 6 0.306771 1.312753 -0.198367 10.54000 0.08319
PART 0
PART 2
O9 6 0.651343 0.548103 0.147038 10.49000 0.04403
O10 6 0.295237 1.336508 -0.219216 10.46000 0.08980
HKLF 4
REM str1619 in P212121 #19
REM wR2 = 0.1098, GooF = S = 1.060, Restrained GooF = 1.060 for all data
REM R1 = 0.0397 for 17109 Fo > 4sig(Fo) and 0.0509 for all 19581 data
REM 821 parameters refined using 0 restraints
END
WGHT 0.0497 11.1569
REM Highest difference peak 0.904, deepest hole -1.441, 1-sigma level 0.096
Q1 1 0.3110 1.3205 -0.1653 11.00000 0.05 0.90
Q2 1 0.7048 0.8446 -0.0528 11.00000 0.05 0.61
Q3 1 0.5862 0.5806 0.1827 11.00000 0.05 0.54
Q4 1 0.6967 1.1616 -0.1382 11.00000 0.05 0.52
Q5 1 0.2608 1.4427 -0.1927 11.00000 0.05 0.50
Q6 1 0.6935 0.8264 0.1411 11.00000 0.05 0.48
Q7 1 0.7680 0.5269 0.1473 11.00000 0.05 0.47
Q8 1 0.1357 1.3797 -0.1660 11.00000 0.05 0.46
Q9 1 0.3465 1.3341 -0.2112 11.00000 0.05 0.46
Q10 1 0.6806 0.8754 0.0265 11.00000 0.05 0.45
Q11 1 0.6176 0.5758 0.1547 11.00000 0.05 0.45
Q12 1 0.7536 0.5208 0.2183 11.00000 0.05 0.44
Q13 1 0.6791 0.5418 0.1484 11.00000 0.05 0.44
Q14 1 0.6783 1.1622 -0.0286 11.00000 0.05 0.39
Q15 1 0.1456 1.3618 -0.2180 11.00000 0.05 0.39
Q16 1 0.7376 0.7811 0.0910 11.00000 0.05 0.39
Q17 1 0.3338 1.3998 -0.2085 11.00000 0.05 0.38
Q18 1 0.5985 0.8410 0.0242 11.00000 0.05 0.38
Q19 1 0.2427 1.3427 -0.2296 11.00000 0.05 0.38
Q20 1 0.6339 1.2605 -0.0189 11.00000 0.05 0.36
;
_shelx_res_checksum 86982
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
12 17 -15 0.0638 12.0000 16.9999 -14.9996 0.4350 -0.1458 0.8920
-13 -16 -11 0.0498 -13.0000 -15.9999 -11.0004 -0.8207 0.2773 -0.5206
3 0 47 0.0757 3.0000 -0.0000 47.0000 0.7601 -0.2662 -0.6031
15 -9 -2 0.0268 15.0000 -9.0002 -2.0002 0.6944 0.6026 0.3818
13 -14 10 0.0283 13.0000 -14.0002 9.9998 0.7408 0.6248 0.0566
-15 6 8 0.0506 -15.0000 6.0002 8.0001 -0.6230 -0.5553 -0.5193
-15 9 2 0.0357 -15.0000 9.0002 2.0002 -0.6944 -0.6026 -0.3818
2 -28 -16 0.0638 2.0001 -28.0001 -16.0006 -0.1720 0.9905 -0.1419
-8 11 38 0.0684 -8.0000 11.0001 38.0002 0.1244 -0.7659 -0.6565
5 27 -14 0.0830 4.9999 27.0000 -13.9995 0.1247 -0.6006 0.8054
-16 0 -8 0.0327 -16.0000 0.0002 -8.0000 -0.8941 -0.2852 -0.4091
-12 17 13 0.0493 -12.0001 17.0002 13.0003 -0.3853 -0.8546 -0.3193
_olex2_date_sample_data_collection 2014-02-27
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF-d8'