# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
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data_123
_database_code_depnum_ccdc_archive 'CCDC 1506214'
loop_
_audit_author_name
_audit_author_address
'Fe complex'
;Nanjing Forestry University
China
;
_audit_update_record
;
2019-04-06 deposited with the CCDC. 2019-05-01 downloaded from the CCDC.
;
_audit_creation_date 2019-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C14 H14 Cl2 Fe N3 O4'
_chemical_formula_sum 'C14 H13 Cl2 Fe N3 O4'
_chemical_formula_weight 414.02
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 8.177(3)
_cell_length_b 22.891(7)
_cell_length_c 10.113(2)
_cell_angle_alpha 90
_cell_angle_beta 117.87(2)
_cell_angle_gamma 90
_cell_volume 1673.4(9)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 2562
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 27.48
_cell_measurement_theta_min 2.45
_shelx_estimated_absorpt_T_max 0.789
_shelx_estimated_absorpt_T_min 0.746
_exptl_absorpt_coefficient_mu 1.244
_exptl_absorpt_correction_T_max 0.7890
_exptl_absorpt_correction_T_min 0.7462
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details SADABS
_exptl_absorpt_special_details ?
_exptl_crystal_colour black
_exptl_crystal_colour_primary black
_exptl_crystal_density_diffrn 1.643
_exptl_crystal_density_meas .
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 840
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.2
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0377
_diffrn_reflns_av_unetI/netI 0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 8390
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.050
_diffrn_reflns_theta_max 25.050
_diffrn_reflns_theta_min 1.779
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2338
_reflns_number_total 2964
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max 0.486
_refine_diff_density_min -0.536
_refine_diff_density_rms 0.089
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.092
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 226
_refine_ls_number_reflns 2964
_refine_ls_number_restraints 3
_refine_ls_R_factor_all 0.0587
_refine_ls_R_factor_gt 0.0416
_refine_ls_restrained_S_all 1.092
_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^)+(0.0597P)^2^+1.2363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1034
_refine_ls_wR_factor_ref 0.1219
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
O4-H4A = O4-H4B
0.85 with sigma of 0.01
H4A-H4B
1.35 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
N2(H2), C2(H2A), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14)
3.b Idealised Me refined as rotating group:
C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary iterative
_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 0.15522(7) 0.91323(2) 0.67065(5) 0.02375(18) Uani 1 1 d . . . . .
Cl1 Cl 0.36861(15) 0.83580(4) 0.70241(10) 0.0390(3) Uani 1 1 d . . . . .
Cl2 Cl 0.35307(14) 0.98445(4) 0.66626(11) 0.0396(3) Uani 1 1 d . . . . .
O1 O 0.2266(3) 0.91103(10) 0.8885(3) 0.0281(6) Uani 1 1 d . . . . .
O2 O 0.0094(3) 0.90457(10) 0.4595(3) 0.0270(6) Uani 1 1 d . . . . .
O3 O -0.1303(4) 0.92153(11) 0.1707(3) 0.0335(6) Uani 1 1 d . . . . .
O4 O -0.0374(4) 0.97812(11) 0.6592(3) 0.0335(6) Uani 1 1 d D . . . .
N1 N 0.2988(5) 0.85062(15) 1.3807(4) 0.0397(9) Uani 1 1 d . . . . .
N2 N 0.0239(4) 0.83384(13) 0.8325(3) 0.0325(8) Uani 1 1 d . . . . .
H2 H -0.026260 0.805922 0.857731 0.039 Uiso 1 1 calc R . . . .
N3 N -0.0152(4) 0.84790(13) 0.6869(3) 0.0280(7) Uani 1 1 d . . . . .
C1 C 0.1488(5) 0.86974(16) 0.9246(4) 0.0268(8) Uani 1 1 d . . . . .
C2 C -0.1405(5) 0.81659(16) 0.5825(4) 0.0298(9) Uani 1 1 d . . . . .
H2A H -0.196503 0.787073 0.610206 0.036 Uiso 1 1 calc R . . . .
C3 C -0.1984(5) 0.82467(15) 0.4260(4) 0.0261(8) Uani 1 1 d . . . . .
C4 C -0.1270(5) 0.86905(15) 0.3714(4) 0.0241(8) Uani 1 1 d . . . . .
C5 C -0.2045(5) 0.87645(15) 0.2144(4) 0.0259(8) Uani 1 1 d . . . . .
C6 C -0.2253(7) 0.9386(2) 0.0170(4) 0.0505(12) Uani 1 1 d . . . . .
H6A H -0.216192 0.907908 -0.044003 0.076 Uiso 1 1 calc GR . . . .
H6B H -0.170318 0.973540 0.003080 0.076 Uiso 1 1 calc GR . . . .
H6C H -0.353110 0.945712 -0.011319 0.076 Uiso 1 1 calc GR . . . .
C7 C -0.3409(5) 0.83960(17) 0.1181(4) 0.0313(9) Uani 1 1 d . . . . .
H7 H -0.390880 0.844892 0.015295 0.038 Uiso 1 1 calc R . . . .
C8 C -0.4046(5) 0.79427(17) 0.1742(4) 0.0343(9) Uani 1 1 d . . . . .
H8 H -0.494889 0.768874 0.108625 0.041 Uiso 1 1 calc R . . . .
C9 C -0.3354(5) 0.78700(17) 0.3244(4) 0.0324(9) Uani 1 1 d . . . . .
H9 H -0.379363 0.756699 0.360428 0.039 Uiso 1 1 calc R . . . .
C10 C 0.2004(5) 0.86225(15) 1.0857(4) 0.0263(8) Uani 1 1 d . . . . .
C11 C 0.1388(5) 0.81498(18) 1.1358(4) 0.0344(9) Uani 1 1 d . . . . .
H11 H 0.063278 0.786846 1.068714 0.041 Uiso 1 1 calc R . . . .
C12 C 0.1905(6) 0.81015(19) 1.2852(4) 0.0396(10) Uani 1 1 d . . . . .
H12 H 0.149929 0.778585 1.319961 0.048 Uiso 1 1 calc R . . . .
C13 C 0.3592(6) 0.8964(2) 1.3357(4) 0.0419(11) Uani 1 1 d . . . . .
H13 H 0.432667 0.924172 1.405371 0.050 Uiso 1 1 calc R . . . .
C14 C 0.3152(6) 0.90343(17) 1.1884(4) 0.0343(9) Uani 1 1 d . . . . .
H14 H 0.360804 0.934949 1.157678 0.041 Uiso 1 1 calc R . . . .
H4A H -0.002(6) 1.0126(8) 0.687(5) 0.054(15) Uiso 1 1 d D . . . .
H4B H -0.140(5) 0.980(2) 0.582(5) 0.15(3) Uiso 1 1 d D . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0289(3) 0.0246(3) 0.0145(3) 0.00061(19) 0.0075(2) -0.0033(2)
Cl1 0.0505(6) 0.0432(6) 0.0208(5) 0.0067(4) 0.0145(4) 0.0181(5)
Cl2 0.0338(6) 0.0420(6) 0.0356(6) 0.0055(4) 0.0101(4) -0.0117(4)
O1 0.0359(15) 0.0293(14) 0.0176(13) -0.0008(10) 0.0111(11) -0.0067(12)
O2 0.0302(14) 0.0280(13) 0.0153(12) 0.0012(10) 0.0044(11) -0.0062(11)
O3 0.0413(16) 0.0350(15) 0.0168(13) 0.0021(11) 0.0075(12) -0.0022(12)
O4 0.0373(17) 0.0284(15) 0.0302(15) 0.0002(12) 0.0120(13) -0.0001(12)
N1 0.049(2) 0.050(2) 0.0258(18) 0.0054(16) 0.0223(17) 0.0075(18)
N2 0.043(2) 0.0323(17) 0.0208(16) 0.0031(13) 0.0141(15) -0.0110(15)
N3 0.0349(18) 0.0289(16) 0.0154(15) 0.0001(12) 0.0078(13) -0.0036(14)
C1 0.033(2) 0.0279(19) 0.0207(18) 0.0022(15) 0.0137(16) 0.0008(17)
C2 0.036(2) 0.0263(19) 0.026(2) 0.0013(15) 0.0132(17) -0.0055(17)
C3 0.027(2) 0.0250(18) 0.0217(19) -0.0021(14) 0.0072(15) -0.0013(15)
C4 0.0244(19) 0.0242(18) 0.0179(17) -0.0031(14) 0.0050(15) 0.0013(15)
C5 0.027(2) 0.0252(19) 0.0220(19) -0.0002(15) 0.0090(16) 0.0034(16)
C6 0.064(3) 0.054(3) 0.021(2) 0.0097(19) 0.010(2) -0.006(2)
C7 0.030(2) 0.038(2) 0.0189(18) -0.0071(16) 0.0056(16) 0.0045(17)
C8 0.031(2) 0.034(2) 0.031(2) -0.0123(17) 0.0084(18) -0.0053(18)
C9 0.034(2) 0.030(2) 0.030(2) -0.0051(16) 0.0128(18) -0.0075(17)
C10 0.028(2) 0.0303(19) 0.0201(18) 0.0024(15) 0.0105(16) 0.0036(16)
C11 0.038(2) 0.037(2) 0.028(2) 0.0022(17) 0.0160(18) -0.0042(18)
C12 0.048(3) 0.044(2) 0.034(2) 0.0110(19) 0.026(2) 0.003(2)
C13 0.045(3) 0.052(3) 0.023(2) -0.0070(18) 0.0111(19) -0.001(2)
C14 0.043(2) 0.038(2) 0.023(2) 0.0008(16) 0.0159(18) -0.0012(19)
_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 Cl1 2.4012(12) . ?
Fe1 Cl2 2.3116(12) . ?
Fe1 O1 1.999(2) . ?
Fe1 O2 1.908(2) . ?
Fe1 O4 2.128(3) . ?
Fe1 N3 2.102(3) . ?
O1 C1 1.284(4) . ?
O2 C4 1.330(4) . ?
O3 C5 1.371(4) . ?
O3 C6 1.429(4) . ?
O4 H4A 0.842(10) . ?
O4 H4B 0.841(10) . ?
N1 C12 1.333(5) . ?
N1 C13 1.327(5) . ?
N2 H2 0.8600 . ?
N2 N3 1.391(4) . ?
N2 C1 1.302(5) . ?
N3 C2 1.291(5) . ?
C1 C10 1.489(5) . ?
C2 H2A 0.9300 . ?
C2 C3 1.436(5) . ?
C3 C4 1.407(5) . ?
C3 C9 1.407(5) . ?
C4 C5 1.418(5) . ?
C5 C7 1.374(5) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7 0.9300 . ?
C7 C8 1.396(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.361(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.385(5) . ?
C10 C14 1.392(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.370(5) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.369(5) . ?
C14 H14 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Fe1 Cl1 92.97(5) . . ?
O1 Fe1 Cl1 90.83(8) . . ?
O1 Fe1 Cl2 101.11(8) . . ?
O1 Fe1 O4 84.53(10) . . ?
O1 Fe1 N3 76.01(10) . . ?
O2 Fe1 Cl1 96.19(8) . . ?
O2 Fe1 Cl2 97.39(8) . . ?
O2 Fe1 O1 159.83(11) . . ?
O2 Fe1 O4 87.27(11) . . ?
O2 Fe1 N3 85.61(11) . . ?
O4 Fe1 Cl1 174.53(8) . . ?
O4 Fe1 Cl2 90.78(9) . . ?
N3 Fe1 Cl1 86.05(9) . . ?
N3 Fe1 Cl2 176.93(8) . . ?
N3 Fe1 O4 90.00(12) . . ?
C1 O1 Fe1 113.8(2) . . ?
C4 O2 Fe1 134.6(2) . . ?
C5 O3 C6 117.3(3) . . ?
Fe1 O4 H4A 120(3) . . ?
Fe1 O4 H4B 119(4) . . ?
H4A O4 H4B 107.0(17) . . ?
C13 N1 C12 121.9(3) . . ?
N3 N2 H2 125.5 . . ?
C1 N2 H2 125.5 . . ?
C1 N2 N3 109.1(3) . . ?
N2 N3 Fe1 114.5(2) . . ?
C2 N3 Fe1 129.2(3) . . ?
C2 N3 N2 116.1(3) . . ?
O1 C1 N2 126.0(3) . . ?
O1 C1 C10 118.1(3) . . ?
N2 C1 C10 115.9(3) . . ?
N3 C2 H2A 118.1 . . ?
N3 C2 C3 123.8(3) . . ?
C3 C2 H2A 118.1 . . ?
C4 C3 C2 122.8(3) . . ?
C9 C3 C2 117.8(3) . . ?
C9 C3 C4 119.4(3) . . ?
O2 C4 C3 123.4(3) . . ?
O2 C4 C5 118.2(3) . . ?
C3 C4 C5 118.4(3) . . ?
O3 C5 C4 114.7(3) . . ?
O3 C5 C7 124.6(3) . . ?
C7 C5 C4 120.7(3) . . ?
O3 C6 H6A 109.5 . . ?
O3 C6 H6B 109.5 . . ?
O3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7 119.9 . . ?
C5 C7 C8 120.1(3) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 119.8 . . ?
C9 C8 C7 120.4(3) . . ?
C9 C8 H8 119.8 . . ?
C3 C9 H9 119.5 . . ?
C8 C9 C3 120.9(4) . . ?
C8 C9 H9 119.5 . . ?
C11 C10 C1 121.6(3) . . ?
C11 C10 C14 119.3(3) . . ?
C14 C10 C1 119.1(3) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 C10 119.3(4) . . ?
C12 C11 H11 120.4 . . ?
N1 C12 C11 120.1(4) . . ?
N1 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
N1 C13 H13 119.5 . . ?
N1 C13 C14 121.0(4) . . ?
C14 C13 H13 119.5 . . ?
C10 C14 H14 120.8 . . ?
C13 C14 C10 118.4(4) . . ?
C13 C14 H14 120.8 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 O1 C1 N2 -4.9(5) . . . . ?
Fe1 O1 C1 C10 176.7(2) . . . . ?
Fe1 O2 C4 C3 -0.4(5) . . . . ?
Fe1 O2 C4 C5 179.4(2) . . . . ?
Fe1 N3 C2 C3 -5.3(6) . . . . ?
O1 C1 C10 C11 -172.7(3) . . . . ?
O1 C1 C10 C14 6.5(5) . . . . ?
O2 C4 C5 O3 -1.4(5) . . . . ?
O2 C4 C5 C7 177.6(3) . . . . ?
O3 C5 C7 C8 178.8(3) . . . . ?
N1 C13 C14 C10 2.0(6) . . . . ?
N2 N3 C2 C3 -179.8(3) . . . . ?
N2 C1 C10 C11 8.8(5) . . . . ?
N2 C1 C10 C14 -172.0(4) . . . . ?
N3 N2 C1 O1 -1.1(5) . . . . ?
N3 N2 C1 C10 177.4(3) . . . . ?
N3 C2 C3 C4 -1.9(6) . . . . ?
N3 C2 C3 C9 179.5(4) . . . . ?
C1 N2 N3 Fe1 6.2(4) . . . . ?
C1 N2 N3 C2 -178.5(3) . . . . ?
C1 C10 C11 C12 180.0(4) . . . . ?
C1 C10 C14 C13 179.1(4) . . . . ?
C2 C3 C4 O2 5.1(6) . . . . ?
C2 C3 C4 C5 -174.7(3) . . . . ?
C2 C3 C9 C8 176.2(4) . . . . ?
C3 C4 C5 O3 178.4(3) . . . . ?
C3 C4 C5 C7 -2.6(5) . . . . ?
C4 C3 C9 C8 -2.5(6) . . . . ?
C4 C5 C7 C8 -0.1(6) . . . . ?
C5 C7 C8 C9 1.5(6) . . . . ?
C6 O3 C5 C4 -168.1(3) . . . . ?
C6 O3 C5 C7 13.0(5) . . . . ?
C7 C8 C9 C3 -0.2(6) . . . . ?
C9 C3 C4 O2 -176.3(3) . . . . ?
C9 C3 C4 C5 3.8(5) . . . . ?
C10 C11 C12 N1 0.0(6) . . . . ?
C11 C10 C14 C13 -1.7(6) . . . . ?
C12 N1 C13 C14 -1.2(6) . . . . ?
C13 N1 C12 C11 0.2(6) . . . . ?
C14 C10 C11 C12 0.8(6) . . . . ?
_iucr_refine_instructions_details
;
TITL 123 in P21/c
123.res
created by SHELXL-2016/6 at 19:10:21 on 05-Apr-2019
CELL 0.71073 8.177 22.891 10.113 90 117.87 90
ZERR 4 0.003 0.007 0.002 0 0.02 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl Fe N O
UNIT 56 52 8 4 12 16
DFIX 0.85 0.01 O4 H4a O4 H4b
DFIX 1.35 0.01 H4a H4b
L.S. 60
PLAN 20
SIZE 0.25 0.22 0.2
BOND $H
CONF
HTAB
fmap 2
acta
OMIT -3 50.1
REM
REM
REM
WGHT 0.059700 1.236300
FVAR 0.10390
FE1 4 0.155223 0.913235 0.670649 11.00000 0.02894 0.02461 =
0.01453 0.00061 0.00751 -0.00331
CL1 3 0.368611 0.835802 0.702406 11.00000 0.05046 0.04324 =
0.02078 0.00668 0.01453 0.01815
CL2 3 0.353067 0.984448 0.666261 11.00000 0.03384 0.04199 =
0.03562 0.00546 0.01007 -0.01167
O1 6 0.226553 0.911027 0.888495 11.00000 0.03591 0.02925 =
0.01755 -0.00076 0.01109 -0.00665
O2 6 0.009428 0.904569 0.459493 11.00000 0.03024 0.02801 =
0.01526 0.00117 0.00436 -0.00622
O3 6 -0.130285 0.921534 0.170677 11.00000 0.04134 0.03502 =
0.01679 0.00211 0.00747 -0.00218
O4 6 -0.037393 0.978124 0.659222 11.00000 0.03730 0.02841 =
0.03023 0.00020 0.01202 -0.00014
N1 5 0.298808 0.850622 1.380683 11.00000 0.04901 0.04991 =
0.02585 0.00537 0.02228 0.00753
N2 5 0.023933 0.833842 0.832540 11.00000 0.04323 0.03226 =
0.02083 0.00313 0.01408 -0.01098
AFIX 43
H2 2 -0.026260 0.805922 0.857731 11.00000 -1.20000
AFIX 0
N3 5 -0.015182 0.847899 0.686943 11.00000 0.03490 0.02889 =
0.01538 0.00008 0.00781 -0.00355
C1 1 0.148760 0.869740 0.924620 11.00000 0.03320 0.02795 =
0.02066 0.00219 0.01372 0.00083
C2 1 -0.140493 0.816585 0.582475 11.00000 0.03565 0.02632 =
0.02613 0.00134 0.01323 -0.00555
AFIX 43
H2A 2 -0.196503 0.787073 0.610206 11.00000 -1.20000
AFIX 0
C3 1 -0.198395 0.824670 0.426026 11.00000 0.02675 0.02498 =
0.02166 -0.00207 0.00718 -0.00134
C4 1 -0.126955 0.869047 0.371418 11.00000 0.02441 0.02425 =
0.01787 -0.00313 0.00501 0.00131
C5 1 -0.204507 0.876448 0.214403 11.00000 0.02746 0.02519 =
0.02196 -0.00016 0.00898 0.00343
C6 1 -0.225271 0.938571 0.016999 11.00000 0.06403 0.05402 =
0.02133 0.00974 0.00979 -0.00575
AFIX 137
H6A 2 -0.216192 0.907908 -0.044003 11.00000 -1.50000
H6B 2 -0.170318 0.973540 0.003080 11.00000 -1.50000
H6C 2 -0.353110 0.945712 -0.011319 11.00000 -1.50000
AFIX 0
C7 1 -0.340933 0.839602 0.118072 11.00000 0.03016 0.03778 =
0.01891 -0.00714 0.00563 0.00454
AFIX 43
H7 2 -0.390880 0.844892 0.015295 11.00000 -1.20000
AFIX 0
C8 1 -0.404633 0.794265 0.174228 11.00000 0.03080 0.03375 =
0.03101 -0.01227 0.00844 -0.00526
AFIX 43
H8 2 -0.494889 0.768874 0.108625 11.00000 -1.20000
AFIX 0
C9 1 -0.335431 0.787000 0.324434 11.00000 0.03414 0.02998 =
0.03046 -0.00514 0.01279 -0.00748
AFIX 43
H9 2 -0.379363 0.756699 0.360428 11.00000 -1.20000
AFIX 0
C10 1 0.200414 0.862251 1.085703 11.00000 0.02767 0.03032 =
0.02009 0.00238 0.01049 0.00356
C11 1 0.138847 0.814985 1.135780 11.00000 0.03842 0.03738 =
0.02794 0.00222 0.01604 -0.00422
AFIX 43
H11 2 0.063278 0.786846 1.068714 11.00000 -1.20000
AFIX 0
C12 1 0.190490 0.810146 1.285164 11.00000 0.04849 0.04402 =
0.03447 0.01096 0.02615 0.00269
AFIX 43
H12 2 0.149929 0.778585 1.319961 11.00000 -1.20000
AFIX 0
C13 1 0.359240 0.896414 1.335732 11.00000 0.04523 0.05228 =
0.02254 -0.00702 0.01107 -0.00131
AFIX 43
H13 2 0.432667 0.924172 1.405371 11.00000 -1.20000
AFIX 0
C14 1 0.315164 0.903427 1.188402 11.00000 0.04299 0.03789 =
0.02268 0.00077 0.01592 -0.00120
AFIX 43
H14 2 0.360804 0.934949 1.157678 11.00000 -1.20000
AFIX 0
H4A 2 -0.002225 1.012606 0.686863 11.00000 0.05369
H4B 2 -0.140446 0.980229 0.581948 11.00000 0.14626
HKLF 4 1 -1 0 0 0 -1 0 1 0 1
REM 123 in P21/c
REM R1 = 0.0416 for 2338 Fo > 4sig(Fo) and 0.0587 for all 2964 data
REM 226 parameters refined using 3 restraints
END
WGHT 0.0597 1.2362
REM Instructions for potential hydrogen bonds
EQIV $1 x-1, y, z-1
HTAB C7 Cl1_$1
EQIV $2 -x+1, -y+2, -z+2
HTAB C14 Cl2_$2
EQIV $3 -x, -y+2, -z+1
HTAB O4 O2_$3
HTAB O4 O3_$3
HTAB O4 Cl2_$3
REM Highest difference peak 0.486, deepest hole -0.536, 1-sigma level 0.089
Q1 1 0.3456 0.8417 1.4844 11.00000 0.05 0.49
Q2 1 0.4207 0.8683 0.6931 11.00000 0.05 0.46
Q3 1 0.1892 0.8631 0.6824 11.00000 0.05 0.45
Q4 1 0.3054 0.8787 0.6989 11.00000 0.05 0.43
Q5 1 0.2464 0.9582 0.6789 11.00000 0.05 0.38
Q6 1 -0.4029 0.8249 0.1599 11.00000 0.05 0.35
Q7 1 -0.5704 0.7360 0.2378 11.00000 0.05 0.33
Q8 1 -0.2918 0.8185 0.3710 11.00000 0.05 0.33
Q9 1 -0.1753 0.9686 0.6919 11.00000 0.05 0.33
Q10 1 0.2698 0.8722 1.1447 11.00000 0.05 0.33
Q11 1 0.0438 0.8785 0.6997 11.00000 0.05 0.32
Q12 1 -0.2485 0.8444 0.1778 11.00000 0.05 0.30
Q13 1 0.3432 0.9444 0.6609 11.00000 0.05 0.29
Q14 1 0.4959 0.8011 0.7039 11.00000 0.05 0.29
Q15 1 0.2296 0.8401 1.3394 11.00000 0.05 0.29
Q16 1 0.0291 0.9463 0.6623 11.00000 0.05 0.29
Q17 1 0.2966 0.8276 0.6421 11.00000 0.05 0.28
Q18 1 0.1783 0.8323 1.1009 11.00000 0.05 0.28
Q19 1 -0.3281 0.8022 0.1565 11.00000 0.05 0.28
Q20 1 -0.3329 0.8734 0.1492 11.00000 0.05 0.28
REM The information below was added by Olex2.
REM
REM R1 = 0.0416 for 2338 Fo > 4sig(Fo) and 0.0587 for all 9472 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.49, deepest hole -0.54
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0587
REM R1_gt = 0.0416
REM wR_ref = 0.1219
REM GOOF = 1.092
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 9472
REM Reflections_gt = 2338
REM Parameters = n/a
REM Hole = -0.54
REM Peak = 0.49
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_20181024njlydx_0m
_database_code_depnum_ccdc_archive 'CCDC 1885799'
loop_
_audit_author_name
_audit_author_address
'Ni complex'
;Nanjing Forestry University
China
;
_audit_update_record
;
2018-12-18 deposited with the CCDC. 2019-05-01 downloaded from the CCDC.
;
_audit_creation_date 2018-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C52 H38 N10 Ni2 O6'
_chemical_formula_sum 'C52 H38 N10 Ni2 O6'
_chemical_formula_weight 1016.34
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 12.2869(8)
_cell_length_b 21.9321(11)
_cell_length_c 24.0672(13)
_cell_angle_alpha 90
_cell_angle_beta 102.135(2)
_cell_angle_gamma 90
_cell_volume 6340.7(6)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9203
_cell_measurement_temperature 296.15
_cell_measurement_theta_max 26.559
_cell_measurement_theta_min 2.259
_shelx_estimated_absorpt_T_max 0.910
_shelx_estimated_absorpt_T_min 0.856
_exptl_absorpt_coefficient_mu 0.640
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.5913
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1456 before and 0.0749 after correction.
The Ratio of minimum to maximum transmission is 0.7931.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'metallic light yellow'
_exptl_crystal_colour_lustre metallic
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.065
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2096
_exptl_crystal_preparation ?
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_min 0.15
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0627
_diffrn_reflns_av_unetI/netI 0.0711
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 38138
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full 25.000
_diffrn_reflns_theta_max 25.000
_diffrn_reflns_theta_min 2.153
_diffrn_ambient_temperature 296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Bruker SMART APEXII DUO CCD'
_diffrn_measurement_method ?
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_special_details ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7948
_reflns_number_total 11108
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 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 0.628
_refine_diff_density_min -0.718
_refine_diff_density_rms 0.104
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.107
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 633
_refine_ls_number_reflns 11108
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0942
_refine_ls_R_factor_gt 0.0656
_refine_ls_restrained_S_all 1.107
_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^)+(0.0944P)^2^+5.8717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1695
_refine_ls_wR_factor_ref 0.1838
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
C16(H16), C18(H18), C0AA(H0AA), C27(H27), C28(H28), C30(H30), C34(H34),
C38(H38), C40(H40), C41(H41), C42(H42), C45(H45), C47(H47), C48(H48), C50(H50),
C53(H53), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C61(H61),
C62(H62), C63(H63), C64(H64), C65(H65), C68(H68), C70(H70), C72(H72), C75(H75),
C77(H77), C2(H2)
2.b Idealised Me refined as rotating group:
C76(H76A,H76B,H76C), C83(H83A,H83B,H83C)
;
_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
Ni1 Ni 0.29852(4) 0.37035(2) 0.03261(2) 0.01364(16) Uani 1 1 d . . . . .
Ni2 Ni 0.71462(5) 0.40930(2) 0.38880(2) 0.01573(16) Uani 1 1 d . . . . .
O1 O 0.4189(2) 0.38606(12) 0.10416(12) 0.0169(7) Uani 1 1 d . . . . .
O4 O 0.6636(2) 0.33102(12) 0.42464(12) 0.0161(6) Uani 1 1 d . . . . .
O5 O 0.7460(3) 0.49342(12) 0.36002(12) 0.0203(7) Uani 1 1 d . . . . .
O2 O 0.1720(2) 0.34596(13) -0.03060(12) 0.0190(7) Uani 1 1 d . . . . .
N20 N 0.8339(3) 0.42373(15) 0.46458(15) 0.0176(8) Uani 1 1 d . . . . .
O3 O 0.0203(3) 0.33221(14) -0.12098(13) 0.0263(8) Uani 1 1 d . . . . .
N21 N 0.3410(3) 0.44255(15) -0.01434(15) 0.0158(8) Uani 1 1 d . . . . .
N8 N 0.3143(3) 0.31530(15) 0.14239(13) 0.0128(7) Uani 1 1 d . . . . .
N9 N 0.8559(3) 0.37318(16) 0.36660(16) 0.0216(8) Uani 1 1 d . . . . .
N10 N 0.5905(3) 0.44212(15) 0.42130(15) 0.0170(8) Uani 1 1 d . . . . .
O6 O 0.8101(3) 0.59019(14) 0.31440(14) 0.0311(8) Uani 1 1 d . . . . .
N22 N 0.1957(3) 0.44094(15) 0.05522(14) 0.0162(8) Uani 1 1 d . . . . .
N14 N 0.6102(3) 0.38736(15) 0.30887(15) 0.0173(8) Uani 1 1 d . . . . .
N15 N 0.2496(3) 0.31338(15) 0.08718(15) 0.0158(8) Uani 1 1 d . . . . .
C16 C 0.8201(4) 0.4459(2) 0.51430(19) 0.0251(11) Uani 1 1 d . . . . .
H16 H 0.748664 0.456699 0.517830 0.030 Uiso 1 1 calc R . . . .
C17 C 0.3965(3) 0.35408(17) 0.14558(17) 0.0133(9) Uani 1 1 d . . . . .
C18 C 0.5379(4) 0.41545(18) 0.21237(18) 0.0178(9) Uani 1 1 d . . . . .
H18 H 0.537507 0.443294 0.183188 0.021 Uiso 1 1 calc R . . . .
N50 N 0.5336(3) 0.39885(15) 0.44738(16) 0.0212(9) Uani 1 1 d . . . . .
C21 C 0.0768(3) 0.27962(17) 0.02610(18) 0.0158(9) Uani 1 1 d . . . . .
C22 C 0.9370(4) 0.40725(19) 0.46046(19) 0.0215(10) Uani 1 1 d . . . . .
C0AA C 0.1235(4) 0.4389(2) 0.0889(2) 0.0227(10) Uani 1 1 d . . . . .
H0AA H 0.118884 0.403289 0.109280 0.027 Uiso 1 1 calc R . . . .
C24 C 0.0007(4) 0.30244(18) -0.07414(19) 0.0212(10) Uani 1 1 d . . . . .
C25 C 0.2804(4) 0.49383(18) -0.01120(18) 0.0174(9) Uani 1 1 d . . . . .
C26 C 0.1349(4) 0.54465(18) 0.02871(19) 0.0199(10) Uani 1 1 d . . . . .
C27 C 0.2212(4) 0.59851(18) -0.03853(19) 0.0203(10) Uani 1 1 d . . . . .
H27 H 0.227568 0.633428 -0.059539 0.024 Uiso 1 1 calc R . . . .
C28 C 0.1580(3) 0.28272(17) 0.07851(18) 0.0145(9) Uani 1 1 d . . . . .
H28 H 0.143209 0.260553 0.109026 0.017 Uiso 1 1 calc R . . . .
C29 C 0.4715(4) 0.36380(18) 0.20243(19) 0.0182(9) Uani 1 1 d . . . . .
C30 C 0.0583(4) 0.5404(2) 0.06438(19) 0.0220(10) Uani 1 1 d . . . . .
H30 H 0.011063 0.572880 0.066983 0.026 Uiso 1 1 calc R . . . .
C31 C 0.9489(4) 0.38074(19) 0.4075(2) 0.0252(11) Uani 1 1 d . . . . .
C32 C 0.2914(4) 0.54707(18) -0.04292(18) 0.0197(10) Uani 1 1 d . . . . .
C23 C 0.2016(4) 0.49327(17) 0.02492(18) 0.0168(9) Uani 1 1 d . . . . .
C34 C 0.0530(4) 0.4880(2) 0.0957(2) 0.0247(11) Uani 1 1 d . . . . .
H34 H 0.004420 0.485160 0.120419 0.030 Uiso 1 1 calc R . . . .
C35 C 0.5795(4) 0.34491(19) 0.44541(19) 0.0203(10) Uani 1 1 d . . . . .
C36 C 1.0307(4) 0.4139(2) 0.5056(2) 0.0279(11) Uani 1 1 d . . . . .
C37 C 0.5205(4) 0.29408(19) 0.46900(19) 0.0193(10) Uani 1 1 d . . . . .
C38 C -0.0197(4) 0.24502(19) 0.02602(19) 0.0191(10) Uani 1 1 d . . . . .
H38 H -0.026674 0.224868 0.059095 0.023 Uiso 1 1 calc R . . . .
C39 C 0.0882(4) 0.31063(18) -0.02541(18) 0.0176(9) Uani 1 1 d . . . . .
C40 C 0.4780(4) 0.32376(19) 0.24770(18) 0.0196(10) Uani 1 1 d . . . . .
H40 H 0.435442 0.288353 0.243332 0.024 Uiso 1 1 calc R . . . .
C41 C 0.6035(4) 0.4257(2) 0.26453(19) 0.0231(10) Uani 1 1 d . . . . .
H41 H 0.646158 0.461061 0.269869 0.028 Uiso 1 1 calc R . . . .
C42 C 0.3714(4) 0.54616(19) -0.0768(2) 0.0228(10) Uani 1 1 d . . . . .
H42 H 0.381326 0.580234 -0.098174 0.027 Uiso 1 1 calc R . . . .
C43 C 0.6936(4) 0.54399(19) 0.36841(17) 0.0175(10) Uani 1 1 d . . . . .
C44 C 0.6080(4) 0.54918(18) 0.39800(19) 0.0225(11) Uani 1 1 d . . . . .
C45 C -0.1026(4) 0.2401(2) -0.0205(2) 0.0248(11) Uani 1 1 d . . . . .
H45 H -0.166104 0.217693 -0.018903 0.030 Uiso 1 1 calc R . . . .
C46 C 0.7286(4) 0.59863(19) 0.34488(19) 0.0253(11) Uani 1 1 d . . . . .
C47 C 0.4347(4) 0.4953(2) -0.0783(2) 0.0267(11) Uani 1 1 d . . . . .
H47 H 0.489554 0.494657 -0.099706 0.032 Uiso 1 1 calc R . . . .
C48 C 0.1470(4) 0.59751(19) -0.0050(2) 0.0240(11) Uani 1 1 d . . . . .
H48 H 0.102580 0.631527 -0.003468 0.029 Uiso 1 1 calc R . . . .
C50 C 0.5473(4) 0.33650(18) 0.29878(19) 0.0199(10) Uani 1 1 d . . . . .
H50 H 0.551278 0.308535 0.328180 0.024 Uiso 1 1 calc R . . . .
C51 C 1.0564(4) 0.3624(2) 0.4004(2) 0.0331(13) Uani 1 1 d . . . . .
C53 C 0.5597(4) 0.49786(19) 0.42336(19) 0.0205(10) Uani 1 1 d . . . . .
H53 H 0.502728 0.506227 0.442281 0.025 Uiso 1 1 calc R . . . .
C55 C 0.6008(5) 0.6585(2) 0.3845(2) 0.0366(14) Uani 1 1 d . . . . .
H55 H 0.570686 0.696278 0.390451 0.044 Uiso 1 1 calc R . . . .
C56 C 0.5626(4) 0.6070(2) 0.4070(2) 0.0295(12) Uani 1 1 d . . . . .
H56 H 0.507379 0.610093 0.428053 0.035 Uiso 1 1 calc R . . . .
C57 C 1.1486(4) 0.3716(2) 0.4467(3) 0.0436(15) Uani 1 1 d . . . . .
H57 H 1.219271 0.360695 0.441971 0.052 Uiso 1 1 calc R . . . .
C58 C 0.5119(4) 0.1987(2) 0.5132(2) 0.0331(13) Uani 1 1 d . . . . .
H58 H 0.550274 0.165720 0.532302 0.040 Uiso 1 1 calc R . . . .
C59 C 0.9067(4) 0.4535(2) 0.5609(2) 0.0319(12) Uani 1 1 d . . . . .
H59 H 0.893160 0.469311 0.594623 0.038 Uiso 1 1 calc R . . . .
C61 C 0.8672(5) 0.3479(2) 0.3182(2) 0.0298(12) Uani 1 1 d . . . . .
H61 H 0.803705 0.342740 0.289774 0.036 Uiso 1 1 calc R . . . .
C62 C -0.0930(4) 0.26898(19) -0.0716(2) 0.0236(11) Uani 1 1 d . . . . .
H62 H -0.149989 0.265420 -0.103691 0.028 Uiso 1 1 calc R . . . .
C63 C 0.4150(4) 0.4433(2) -0.04662(19) 0.0216(10) Uani 1 1 d . . . . .
H63 H 0.456326 0.408207 -0.048811 0.026 Uiso 1 1 calc R . . . .
C64 C 1.0123(5) 0.4377(2) 0.5569(2) 0.0331(13) Uani 1 1 d . . . . .
H64 H 1.071270 0.442612 0.587795 0.040 Uiso 1 1 calc R . . . .
C65 C 0.6833(5) 0.6552(2) 0.3533(2) 0.0322(13) Uani 1 1 d . . . . .
H65 H 0.708038 0.690264 0.338130 0.039 Uiso 1 1 calc R . . . .
C68 C 1.1379(4) 0.3957(2) 0.4975(3) 0.0407(14) Uani 1 1 d . . . . .
H68 H 1.200198 0.400316 0.526753 0.049 Uiso 1 1 calc R . . . .
C70 C 0.9687(5) 0.3285(2) 0.3075(3) 0.0434(15) Uani 1 1 d . . . . .
H70 H 0.972417 0.310825 0.272853 0.052 Uiso 1 1 calc R . . . .
C72 C 0.5729(4) 0.2439(2) 0.4959(3) 0.0401(15) Uani 1 1 d . . . . .
H72 H 0.650007 0.240784 0.502476 0.048 Uiso 1 1 calc R . . . .
C75 C 1.0626(5) 0.3359(2) 0.3486(3) 0.0417(15) Uani 1 1 d . . . . .
H75 H 1.130975 0.323331 0.341965 0.050 Uiso 1 1 calc R . . . .
C76 C -0.0665(5) 0.3343(3) -0.1705(2) 0.0405(14) Uani 1 1 d . . . . .
H76A H -0.044132 0.359850 -0.198501 0.061 Uiso 1 1 calc GR . . . .
H76B H -0.132559 0.350721 -0.160813 0.061 Uiso 1 1 calc GR . . . .
H76C H -0.081238 0.293924 -0.185435 0.061 Uiso 1 1 calc GR . . . .
C77 C 0.4086(5) 0.2943(3) 0.4608(4) 0.078(3) Uani 1 1 d . . . . .
H77 H 0.368664 0.327736 0.443610 0.093 Uiso 1 1 calc R . . . .
C83 C 0.8645(6) 0.6428(2) 0.2986(3) 0.0529(18) Uani 1 1 d . . . . .
H83A H 0.811114 0.668178 0.274297 0.079 Uiso 1 1 calc GR . . . .
H83B H 0.921048 0.630488 0.278846 0.079 Uiso 1 1 calc GR . . . .
H83C H 0.898020 0.665204 0.332142 0.079 Uiso 1 1 calc GR . . . .
N1 N 0.4023(3) 0.19808(15) 0.50464(14) 0.0165(8) Uani 1 1 d . . . . .
C2 C 0.3523(5) 0.2452(3) 0.4777(3) 0.068(2) Uani 1 1 d . . . . .
H2 H 0.274900 0.245972 0.469332 0.082 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0141(3) 0.0112(3) 0.0156(3) 0.0009(2) 0.0031(2) 0.0005(2)
Ni2 0.0159(3) 0.0136(3) 0.0165(3) 0.0013(2) 0.0006(2) -0.0029(2)
O1 0.0178(16) 0.0160(15) 0.0165(16) -0.0003(12) 0.0030(13) -0.0036(12)
O4 0.0136(16) 0.0164(15) 0.0185(16) 0.0052(12) 0.0040(13) -0.0013(12)
O5 0.0242(18) 0.0148(15) 0.0206(17) 0.0015(12) 0.0016(14) -0.0039(13)
O2 0.0176(17) 0.0219(16) 0.0180(16) 0.0002(12) 0.0049(13) -0.0031(13)
N20 0.018(2) 0.0150(18) 0.020(2) 0.0027(15) 0.0030(16) -0.0054(15)
O3 0.0253(19) 0.0325(18) 0.0162(17) 0.0030(14) -0.0069(14) 0.0017(14)
N21 0.0108(19) 0.0181(18) 0.0174(19) 0.0032(15) 0.0003(16) 0.0016(14)
N8 0.0159(19) 0.0160(17) 0.0076(17) -0.0005(13) 0.0047(15) -0.0020(14)
N9 0.024(2) 0.024(2) 0.020(2) 0.0030(16) 0.0107(18) 0.0011(16)
N10 0.019(2) 0.0138(18) 0.0169(19) -0.0014(14) 0.0013(16) -0.0017(15)
O6 0.045(2) 0.0224(17) 0.0238(18) 0.0049(14) 0.0035(17) -0.0143(15)
N22 0.016(2) 0.0183(18) 0.0122(18) -0.0003(14) -0.0027(15) 0.0002(15)
N14 0.020(2) 0.0151(18) 0.0159(19) 0.0022(14) 0.0015(16) -0.0044(15)
N15 0.016(2) 0.0134(17) 0.0183(19) -0.0011(14) 0.0041(16) 0.0050(14)
C16 0.022(3) 0.032(3) 0.019(2) 0.003(2) 0.002(2) -0.003(2)
C17 0.015(2) 0.0099(19) 0.016(2) 0.0049(16) 0.0051(18) -0.0015(16)
C18 0.025(3) 0.015(2) 0.013(2) 0.0040(17) 0.0030(19) -0.0033(18)
N50 0.018(2) 0.0144(19) 0.033(2) 0.0062(16) 0.0108(18) 0.0005(15)
C21 0.015(2) 0.0081(19) 0.024(2) -0.0040(17) 0.0037(19) 0.0048(16)
C22 0.018(2) 0.020(2) 0.025(3) 0.0062(19) 0.001(2) -0.0012(18)
C0AA 0.018(3) 0.021(2) 0.030(3) -0.001(2) 0.006(2) -0.0018(18)
C24 0.019(3) 0.014(2) 0.027(3) -0.0050(19) -0.002(2) 0.0067(18)
C25 0.018(2) 0.015(2) 0.018(2) -0.0046(17) 0.0014(19) 0.0009(17)
C26 0.024(3) 0.009(2) 0.024(2) -0.0008(17) 0.000(2) 0.0011(17)
C27 0.026(3) 0.008(2) 0.025(3) 0.0018(18) 0.003(2) -0.0030(17)
C28 0.015(2) 0.0077(19) 0.023(2) 0.0044(17) 0.0084(19) 0.0013(16)
C29 0.016(2) 0.014(2) 0.024(2) 0.0005(18) 0.0047(19) 0.0018(17)
C30 0.021(3) 0.018(2) 0.026(3) -0.0053(19) 0.002(2) 0.0034(18)
C31 0.022(3) 0.018(2) 0.036(3) 0.011(2) 0.006(2) -0.0002(19)
C32 0.021(2) 0.014(2) 0.018(2) 0.0017(17) -0.007(2) -0.0065(18)
C23 0.019(2) 0.009(2) 0.022(2) 0.0000(17) 0.0026(19) -0.0055(17)
C34 0.024(3) 0.024(2) 0.028(3) -0.005(2) 0.010(2) -0.0013(19)
C35 0.017(2) 0.017(2) 0.023(2) 0.0007(18) -0.005(2) -0.0033(18)
C36 0.016(3) 0.025(2) 0.040(3) 0.005(2) -0.002(2) -0.0009(19)
C37 0.018(2) 0.017(2) 0.023(2) -0.0016(18) 0.004(2) -0.0011(17)
C38 0.018(2) 0.017(2) 0.023(2) -0.0051(18) 0.006(2) -0.0034(17)
C39 0.019(2) 0.014(2) 0.020(2) -0.0081(17) 0.0038(19) 0.0056(17)
C40 0.018(2) 0.015(2) 0.023(2) -0.0011(18) 0.000(2) -0.0044(17)
C41 0.028(3) 0.019(2) 0.021(2) 0.0008(18) 0.002(2) -0.0087(19)
C42 0.023(3) 0.017(2) 0.028(3) 0.0085(19) 0.003(2) -0.0035(18)
C43 0.022(2) 0.019(2) 0.007(2) 0.0023(17) -0.0067(18) -0.0093(18)
C44 0.027(3) 0.011(2) 0.026(3) 0.0020(18) -0.004(2) -0.0020(18)
C45 0.018(3) 0.021(2) 0.036(3) -0.010(2) 0.007(2) -0.0007(19)
C46 0.035(3) 0.015(2) 0.021(2) 0.0033(18) -0.006(2) -0.008(2)
C47 0.025(3) 0.028(3) 0.029(3) 0.003(2) 0.009(2) 0.002(2)
C48 0.029(3) 0.013(2) 0.029(3) -0.0021(19) 0.003(2) 0.0046(19)
C50 0.027(3) 0.011(2) 0.021(2) 0.0059(17) 0.002(2) -0.0013(18)
C51 0.029(3) 0.021(2) 0.056(4) 0.006(2) 0.024(3) 0.004(2)
C53 0.016(2) 0.021(2) 0.024(2) -0.0005(19) 0.002(2) 0.0047(18)
C55 0.037(3) 0.011(2) 0.055(4) -0.003(2) -0.005(3) -0.003(2)
C56 0.032(3) 0.019(2) 0.037(3) -0.003(2) 0.006(2) -0.001(2)
C57 0.016(3) 0.039(3) 0.076(5) 0.014(3) 0.011(3) 0.007(2)
C58 0.014(3) 0.029(3) 0.050(3) 0.023(2) -0.009(2) -0.003(2)
C59 0.040(3) 0.029(3) 0.024(3) -0.003(2) 0.001(2) 0.002(2)
C61 0.046(3) 0.019(2) 0.029(3) 0.004(2) 0.019(3) 0.000(2)
C62 0.019(3) 0.017(2) 0.029(3) -0.0155(19) -0.007(2) 0.0019(18)
C63 0.017(2) 0.023(2) 0.024(3) 0.0004(19) 0.002(2) 0.0033(18)
C64 0.035(3) 0.025(3) 0.032(3) 0.003(2) -0.010(2) -0.011(2)
C65 0.045(3) 0.019(2) 0.030(3) 0.008(2) 0.000(3) -0.013(2)
C68 0.020(3) 0.036(3) 0.059(4) 0.013(3) -0.008(3) 0.001(2)
C70 0.069(5) 0.027(3) 0.047(4) 0.000(2) 0.042(4) 0.008(3)
C72 0.015(3) 0.029(3) 0.071(4) 0.029(3) -0.005(3) -0.002(2)
C75 0.046(4) 0.033(3) 0.059(4) 0.011(3) 0.040(3) 0.015(3)
C76 0.041(3) 0.043(3) 0.028(3) 0.001(2) -0.014(3) 0.003(3)
C77 0.025(3) 0.046(4) 0.167(8) 0.068(5) 0.032(4) 0.017(3)
C83 0.079(5) 0.031(3) 0.059(4) 0.001(3) 0.037(4) -0.024(3)
N1 0.022(2) 0.0143(18) 0.0144(19) -0.0002(14) 0.0067(16) 0.0001(15)
C2 0.016(3) 0.044(4) 0.150(7) 0.060(4) 0.030(4) 0.012(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
Ni1 O1 2.050(3) . ?
Ni1 O2 2.006(3) . ?
Ni1 N21 2.075(3) . ?
Ni1 N22 2.140(3) . ?
Ni1 N15 1.995(3) . ?
Ni1 N1 2.166(3) 4_565 ?
Ni2 O4 2.076(3) . ?
Ni2 O5 2.036(3) . ?
Ni2 N20 2.110(4) . ?
Ni2 N9 2.077(4) . ?
Ni2 N10 1.989(4) . ?
Ni2 N14 2.131(3) . ?
O1 C17 1.295(5) . ?
O4 C35 1.276(5) . ?
O5 C43 1.319(5) . ?
O2 C39 1.315(5) . ?
N20 C16 1.335(6) . ?
N20 C22 1.341(6) . ?
O3 C24 1.367(6) . ?
O3 C76 1.422(5) . ?
N21 C25 1.360(5) . ?
N21 C63 1.314(5) . ?
N8 N15 1.398(5) . ?
N8 C17 1.311(5) . ?
N9 C31 1.353(6) . ?
N9 C61 1.323(6) . ?
N10 N50 1.402(5) . ?
N10 C53 1.284(5) . ?
O6 C46 1.372(6) . ?
O6 C83 1.424(6) . ?
N22 C0AA 1.323(6) . ?
N22 C23 1.370(5) . ?
N14 C41 1.347(5) . ?
N14 C50 1.350(5) . ?
N15 C28 1.289(5) . ?
C16 C59 1.384(7) . ?
C17 C29 1.495(6) . ?
C18 C29 1.387(6) . ?
C18 C41 1.361(6) . ?
N50 C35 1.315(5) . ?
C21 C28 1.436(6) . ?
C21 C38 1.408(6) . ?
C21 C39 1.447(6) . ?
C22 C31 1.437(7) . ?
C22 C36 1.414(6) . ?
C0AA C34 1.412(6) . ?
C24 C39 1.426(6) . ?
C24 C62 1.377(6) . ?
C25 C32 1.417(6) . ?
C25 C23 1.430(6) . ?
C26 C30 1.403(6) . ?
C26 C23 1.408(6) . ?
C26 C48 1.441(6) . ?
C27 C32 1.437(6) . ?
C27 C48 1.338(6) . ?
C29 C40 1.389(6) . ?
C30 C34 1.383(6) . ?
C31 C51 1.425(7) . ?
C32 C42 1.402(6) . ?
C35 C37 1.505(6) . ?
C36 C64 1.401(7) . ?
C36 C68 1.428(7) . ?
C37 C72 1.367(6) . ?
C37 C77 1.347(7) . ?
C38 C45 1.351(6) . ?
C40 C50 1.369(6) . ?
C42 C47 1.365(6) . ?
C43 C44 1.393(6) . ?
C43 C46 1.430(6) . ?
C44 C53 1.464(6) . ?
C44 C56 1.421(6) . ?
C45 C62 1.410(7) . ?
C46 C65 1.392(7) . ?
C47 C63 1.421(6) . ?
C51 C57 1.426(8) . ?
C51 C75 1.392(8) . ?
C55 C56 1.377(7) . ?
C55 C65 1.385(7) . ?
C57 C68 1.364(8) . ?
C58 C72 1.360(7) . ?
C58 N1 1.320(6) . ?
C59 C64 1.366(7) . ?
C61 C70 1.393(8) . ?
C70 C75 1.361(8) . ?
C77 C2 1.385(8) . ?
N1 C2 1.304(6) . ?
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
O1 Ni1 N21 96.28(12) . . ?
O1 Ni1 N22 91.44(12) . . ?
O1 Ni1 N1 90.55(12) . 4_565 ?
O2 Ni1 O1 171.67(11) . . ?
O2 Ni1 N21 91.97(13) . . ?
O2 Ni1 N22 88.91(12) . . ?
O2 Ni1 N1 89.56(13) . 4_565 ?
N21 Ni1 N22 79.40(13) . . ?
N21 Ni1 N1 97.34(13) . 4_565 ?
N22 Ni1 N1 176.34(13) . 4_565 ?
N15 Ni1 O1 79.42(13) . . ?
N15 Ni1 O2 92.26(13) . . ?
N15 Ni1 N21 169.03(14) . . ?
N15 Ni1 N22 90.57(13) . . ?
N15 Ni1 N1 92.81(13) . 4_565 ?
O4 Ni2 N20 88.88(12) . . ?
O4 Ni2 N9 97.64(13) . . ?
O4 Ni2 N14 90.66(12) . . ?
O5 Ni2 O4 170.37(12) . . ?
O5 Ni2 N20 90.65(12) . . ?
O5 Ni2 N9 91.72(13) . . ?
O5 Ni2 N14 91.05(12) . . ?
N20 Ni2 N14 172.45(14) . . ?
N9 Ni2 N20 79.24(15) . . ?
N9 Ni2 N14 93.36(15) . . ?
N10 Ni2 O4 79.21(13) . . ?
N10 Ni2 O5 91.23(13) . . ?
N10 Ni2 N20 93.25(14) . . ?
N10 Ni2 N9 171.96(14) . . ?
N10 Ni2 N14 94.07(14) . . ?
C17 O1 Ni1 108.8(2) . . ?
C35 O4 Ni2 107.8(2) . . ?
C43 O5 Ni2 125.2(3) . . ?
C39 O2 Ni1 125.6(3) . . ?
C16 N20 Ni2 129.3(3) . . ?
C16 N20 C22 117.7(4) . . ?
C22 N20 Ni2 113.0(3) . . ?
C24 O3 C76 118.4(4) . . ?
C25 N21 Ni1 113.4(3) . . ?
C63 N21 Ni1 128.0(3) . . ?
C63 N21 C25 118.5(4) . . ?
C17 N8 N15 110.6(3) . . ?
C31 N9 Ni2 113.0(3) . . ?
C61 N9 Ni2 129.3(4) . . ?
C61 N9 C31 117.5(4) . . ?
N50 N10 Ni2 115.2(2) . . ?
C53 N10 Ni2 128.1(3) . . ?
C53 N10 N50 116.6(4) . . ?
C46 O6 C83 118.0(4) . . ?
C0AA N22 Ni1 129.8(3) . . ?
C0AA N22 C23 118.2(4) . . ?
C23 N22 Ni1 111.7(3) . . ?
C41 N14 Ni2 120.0(3) . . ?
C41 N14 C50 115.8(4) . . ?
C50 N14 Ni2 124.2(3) . . ?
N8 N15 Ni1 114.6(2) . . ?
C28 N15 Ni1 126.4(3) . . ?
C28 N15 N8 118.2(3) . . ?
N20 C16 C59 123.3(5) . . ?
O1 C17 N8 126.3(4) . . ?
O1 C17 C29 115.9(3) . . ?
N8 C17 C29 117.7(4) . . ?
C41 C18 C29 120.5(4) . . ?
C35 N50 N10 109.6(4) . . ?
C28 C21 C39 123.8(4) . . ?
C38 C21 C28 117.2(4) . . ?
C38 C21 C39 119.1(4) . . ?
N20 C22 C31 116.7(4) . . ?
N20 C22 C36 123.0(4) . . ?
C36 C22 C31 120.3(4) . . ?
N22 C0AA C34 123.4(4) . . ?
O3 C24 C39 112.6(4) . . ?
O3 C24 C62 125.8(4) . . ?
C62 C24 C39 121.6(4) . . ?
N21 C25 C32 122.4(4) . . ?
N21 C25 C23 118.4(4) . . ?
C32 C25 C23 119.2(4) . . ?
C30 C26 C23 117.4(4) . . ?
C30 C26 C48 124.1(4) . . ?
C23 C26 C48 118.5(4) . . ?
C48 C27 C32 121.8(4) . . ?
N15 C28 C21 126.0(4) . . ?
C18 C29 C17 120.1(4) . . ?
C18 C29 C40 116.5(4) . . ?
C40 C29 C17 123.4(4) . . ?
C34 C30 C26 120.2(4) . . ?
N9 C31 C22 117.8(4) . . ?
N9 C31 C51 122.8(5) . . ?
C51 C31 C22 119.4(5) . . ?
C25 C32 C27 118.7(4) . . ?
C42 C32 C25 117.3(4) . . ?
C42 C32 C27 124.0(4) . . ?
N22 C23 C25 116.7(4) . . ?
N22 C23 C26 122.6(4) . . ?
C26 C23 C25 120.7(4) . . ?
C30 C34 C0AA 118.1(4) . . ?
O4 C35 N50 128.1(4) . . ?
O4 C35 C37 117.7(4) . . ?
N50 C35 C37 114.1(4) . . ?
C22 C36 C68 119.5(5) . . ?
C64 C36 C22 117.3(4) . . ?
C64 C36 C68 123.2(5) . . ?
C72 C37 C35 124.0(4) . . ?
C77 C37 C35 120.0(4) . . ?
C77 C37 C72 115.9(4) . . ?
C45 C38 C21 122.2(4) . . ?
O2 C39 C21 125.3(4) . . ?
O2 C39 C24 117.8(4) . . ?
C24 C39 C21 117.0(4) . . ?
C50 C40 C29 119.9(4) . . ?
N14 C41 C18 123.6(4) . . ?
C47 C42 C32 120.0(4) . . ?
O5 C43 C44 126.3(4) . . ?
O5 C43 C46 116.6(4) . . ?
C44 C43 C46 117.2(4) . . ?
C43 C44 C53 124.5(4) . . ?
C43 C44 C56 120.9(4) . . ?
C56 C44 C53 114.6(4) . . ?
C38 C45 C62 120.1(4) . . ?
O6 C46 C43 114.4(4) . . ?
O6 C46 C65 123.9(4) . . ?
C65 C46 C43 121.7(5) . . ?
C42 C47 C63 118.6(4) . . ?
C27 C48 C26 121.1(4) . . ?
N14 C50 C40 123.7(4) . . ?
C31 C51 C57 118.1(5) . . ?
C75 C51 C31 116.8(5) . . ?
C75 C51 C57 125.1(5) . . ?
N10 C53 C44 124.6(4) . . ?
C56 C55 C65 121.3(5) . . ?
C55 C56 C44 119.7(5) . . ?
C68 C57 C51 123.0(5) . . ?
N1 C58 C72 124.7(4) . . ?
C64 C59 C16 119.5(5) . . ?
N9 C61 C70 123.7(5) . . ?
C24 C62 C45 120.1(4) . . ?
N21 C63 C47 123.0(4) . . ?
C59 C64 C36 119.3(5) . . ?
C55 C65 C46 119.2(4) . . ?
C57 C68 C36 119.7(5) . . ?
C75 C70 C61 119.0(5) . . ?
C58 C72 C37 119.8(5) . . ?
C70 C75 C51 120.2(5) . . ?
C37 C77 C2 120.8(5) . . ?
C58 N1 Ni1 127.3(3) . 4_566 ?
C2 N1 Ni1 117.3(3) . 4_566 ?
C2 N1 C58 115.4(4) . . ?
N1 C2 C77 123.4(5) . . ?
_iucr_refine_instructions_details
;
TITL 20181024njlydx_0m in P21/c #14
20181024njlydx_0m.res
created by SHELXL-2016/6 at 09:28:41 on 21-Nov-2018
CELL 0.71073 12.2869 21.9321 24.0672 90 102.1346 90
ZERR 4 0.0008 0.0011 0.0013 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N Ni O
UNIT 208 152 40 8 24
L.S. 4
PLAN 20
SIZE 0.25 0.21 0.15
TEMP 23
BOND
fmap 2
acta
OMIT 0 50
REM
REM
REM
WGHT 0.094400 5.871700
FVAR 6.55705
NI1 4 0.298523 0.370353 0.032606 11.00000 0.01405 0.01123 =
0.01564 0.00088 0.00312 0.00049
NI2 4 0.714620 0.409298 0.388803 11.00000 0.01591 0.01359 =
0.01647 0.00128 0.00063 -0.00287
O1 5 0.418929 0.386063 0.104159 11.00000 0.01781 0.01605 =
0.01646 -0.00031 0.00301 -0.00363
O4 5 0.663646 0.331025 0.424644 11.00000 0.01361 0.01637 =
0.01847 0.00518 0.00395 -0.00128
O5 5 0.745967 0.493416 0.360017 11.00000 0.02420 0.01482 =
0.02059 0.00153 0.00162 -0.00392
O2 5 0.171989 0.345956 -0.030601 11.00000 0.01760 0.02194 =
0.01800 0.00021 0.00490 -0.00307
N20 3 0.833919 0.423735 0.464578 11.00000 0.01785 0.01502 =
0.01959 0.00274 0.00304 -0.00543
O3 5 0.020297 0.332209 -0.120977 11.00000 0.02526 0.03249 =
0.01618 0.00303 -0.00690 0.00173
N21 3 0.341033 0.442554 -0.014343 11.00000 0.01079 0.01809 =
0.01743 0.00316 0.00032 0.00158
N8 3 0.314293 0.315301 0.142394 11.00000 0.01586 0.01597 =
0.00756 -0.00055 0.00471 -0.00200
N9 3 0.855872 0.373182 0.366604 11.00000 0.02367 0.02413 =
0.01966 0.00299 0.01067 0.00114
N10 3 0.590488 0.442120 0.421297 11.00000 0.01925 0.01381 =
0.01687 -0.00145 0.00129 -0.00171
O6 5 0.810096 0.590195 0.314397 11.00000 0.04544 0.02239 =
0.02378 0.00488 0.00346 -0.01432
N22 3 0.195708 0.440941 0.055217 11.00000 0.01552 0.01827 =
0.01222 -0.00028 -0.00266 0.00019
N14 3 0.610243 0.387364 0.308873 11.00000 0.01994 0.01513 =
0.01589 0.00220 0.00149 -0.00442
N15 3 0.249575 0.313376 0.087183 11.00000 0.01585 0.01339 =
0.01834 -0.00112 0.00415 0.00495
C16 1 0.820080 0.445871 0.514303 11.00000 0.02234 0.03243 =
0.01936 0.00332 0.00168 -0.00304
AFIX 43
H16 2 0.748664 0.456699 0.517830 11.00000 -1.20000
AFIX 0
C17 1 0.396535 0.354076 0.145576 11.00000 0.01456 0.00986 =
0.01627 0.00487 0.00514 -0.00153
C18 1 0.537881 0.415453 0.212373 11.00000 0.02535 0.01475 =
0.01290 0.00399 0.00296 -0.00331
AFIX 43
H18 2 0.537507 0.443294 0.183188 11.00000 -1.20000
AFIX 0
N50 3 0.533645 0.398848 0.447379 11.00000 0.01823 0.01440 =
0.03330 0.00620 0.01080 0.00047
C21 1 0.076777 0.279620 0.026104 11.00000 0.01520 0.00807 =
0.02397 -0.00396 0.00367 0.00485
C22 1 0.936985 0.407245 0.460463 11.00000 0.01803 0.01965 =
0.02510 0.00618 0.00050 -0.00118
C0AA 1 0.123472 0.438914 0.088941 11.00000 0.01828 0.02089 =
0.02953 -0.00125 0.00648 -0.00185
AFIX 43
H0AA 2 0.118884 0.403289 0.109280 11.00000 -1.20000
AFIX 0
C24 1 0.000706 0.302437 -0.074143 11.00000 0.01878 0.01438 =
0.02743 -0.00496 -0.00223 0.00671
C25 1 0.280380 0.493828 -0.011203 11.00000 0.01797 0.01525 =
0.01792 -0.00457 0.00137 0.00088
C26 1 0.134870 0.544645 0.028711 11.00000 0.02409 0.00934 =
0.02378 -0.00077 -0.00043 0.00112
C27 1 0.221247 0.598506 -0.038526 11.00000 0.02613 0.00822 =
0.02548 0.00178 0.00281 -0.00303
AFIX 43
H27 2 0.227568 0.633428 -0.059539 11.00000 -1.20000
AFIX 0
C28 1 0.158014 0.282717 0.078512 11.00000 0.01524 0.00768 =
0.02259 0.00439 0.00837 0.00128
AFIX 43
H28 2 0.143209 0.260553 0.109026 11.00000 -1.20000
AFIX 0
C29 1 0.471503 0.363803 0.202428 11.00000 0.01630 0.01400 =
0.02448 0.00047 0.00472 0.00183
C30 1 0.058343 0.540377 0.064377 11.00000 0.02062 0.01760 =
0.02623 -0.00533 0.00171 0.00343
AFIX 43
H30 2 0.011063 0.572880 0.066983 11.00000 -1.20000
AFIX 0
C31 1 0.948927 0.380736 0.407483 11.00000 0.02178 0.01820 =
0.03565 0.01146 0.00644 -0.00016
C32 1 0.291424 0.547071 -0.042923 11.00000 0.02142 0.01409 =
0.01834 0.00175 -0.00741 -0.00648
C23 1 0.201636 0.493274 0.024919 11.00000 0.01880 0.00937 =
0.02154 -0.00004 0.00256 -0.00553
C34 1 0.053017 0.487985 0.095664 11.00000 0.02398 0.02391 =
0.02812 -0.00458 0.00988 -0.00130
AFIX 43
H34 2 0.004420 0.485160 0.120419 11.00000 -1.20000
AFIX 0
C35 1 0.579510 0.344913 0.445411 11.00000 0.01740 0.01660 =
0.02291 0.00072 -0.00484 -0.00329
C36 1 1.030705 0.413858 0.505578 11.00000 0.01602 0.02467 =
0.03962 0.00508 -0.00159 -0.00090
C37 1 0.520464 0.294082 0.469004 11.00000 0.01769 0.01670 =
0.02306 -0.00157 0.00352 -0.00112
C38 1 -0.019741 0.245018 0.026015 11.00000 0.01821 0.01688 =
0.02287 -0.00513 0.00595 -0.00343
AFIX 43
H38 2 -0.026674 0.224868 0.059095 11.00000 -1.20000
AFIX 0
C39 1 0.088219 0.310631 -0.025415 11.00000 0.01889 0.01386 =
0.01995 -0.00809 0.00385 0.00560
C40 1 0.478045 0.323758 0.247701 11.00000 0.01834 0.01539 =
0.02312 -0.00112 -0.00021 -0.00437
AFIX 43
H40 2 0.435442 0.288353 0.243332 11.00000 -1.20000
AFIX 0
C41 1 0.603542 0.425669 0.264534 11.00000 0.02813 0.01887 =
0.02068 0.00082 0.00172 -0.00873
AFIX 43
H41 2 0.646158 0.461061 0.269869 11.00000 -1.20000
AFIX 0
C42 1 0.371399 0.546162 -0.076776 11.00000 0.02302 0.01656 =
0.02775 0.00848 0.00271 -0.00348
AFIX 43
H42 2 0.381326 0.580234 -0.098174 11.00000 -1.20000
AFIX 0
C43 1 0.693612 0.543994 0.368409 11.00000 0.02161 0.01913 =
0.00740 0.00228 -0.00668 -0.00927
C44 1 0.608030 0.549180 0.398002 11.00000 0.02673 0.01101 =
0.02578 0.00201 -0.00369 -0.00198
C45 1 -0.102622 0.240122 -0.020546 11.00000 0.01825 0.02051 =
0.03638 -0.01035 0.00725 -0.00068
AFIX 43
H45 2 -0.166104 0.217693 -0.018903 11.00000 -1.20000
AFIX 0
C46 1 0.728631 0.598628 0.344880 11.00000 0.03479 0.01536 =
0.02053 0.00335 -0.00589 -0.00775
C47 1 0.434692 0.495283 -0.078335 11.00000 0.02528 0.02754 =
0.02884 0.00270 0.00936 0.00227
AFIX 43
H47 2 0.489554 0.494657 -0.099706 11.00000 -1.20000
AFIX 0
C48 1 0.147046 0.597514 -0.005015 11.00000 0.02884 0.01313 =
0.02858 -0.00207 0.00272 0.00465
AFIX 43
H48 2 0.102580 0.631527 -0.003468 11.00000 -1.20000
AFIX 0
C50 1 0.547330 0.336501 0.298776 11.00000 0.02690 0.01074 =
0.02102 0.00594 0.00250 -0.00131
AFIX 43
H50 2 0.551278 0.308535 0.328180 11.00000 -1.20000
AFIX 0
C51 1 1.056420 0.362351 0.400410 11.00000 0.02905 0.02052 =
0.05642 0.00618 0.02401 0.00448
C53 1 0.559695 0.497857 0.423363 11.00000 0.01570 0.02104 =
0.02380 -0.00050 0.00215 0.00470
AFIX 43
H53 2 0.502728 0.506227 0.442281 11.00000 -1.20000
AFIX 0
C55 1 0.600825 0.658528 0.384549 11.00000 0.03739 0.01102 =
0.05516 -0.00324 -0.00475 -0.00319
AFIX 43
H55 2 0.570686 0.696278 0.390451 11.00000 -1.20000
AFIX 0
C56 1 0.562615 0.607031 0.407048 11.00000 0.03173 0.01901 =
0.03727 -0.00273 0.00612 -0.00121
AFIX 43
H56 2 0.507379 0.610093 0.428053 11.00000 -1.20000
AFIX 0
C57 1 1.148619 0.371602 0.446671 11.00000 0.01558 0.03920 =
0.07646 0.01427 0.01071 0.00674
AFIX 43
H57 2 1.219271 0.360695 0.441971 11.00000 -1.20000
AFIX 0
C58 1 0.511925 0.198655 0.513152 11.00000 0.01390 0.02874 =
0.04992 0.02255 -0.00874 -0.00328
AFIX 43
H58 2 0.550274 0.165720 0.532302 11.00000 -1.20000
AFIX 0
C59 1 0.906721 0.453509 0.560864 11.00000 0.04046 0.02889 =
0.02384 -0.00321 0.00126 0.00175
AFIX 43
H59 2 0.893160 0.469311 0.594623 11.00000 -1.20000
AFIX 0
C61 1 0.867156 0.347886 0.318222 11.00000 0.04593 0.01873 =
0.02942 0.00390 0.01884 -0.00012
AFIX 43
H61 2 0.803705 0.342740 0.289774 11.00000 -1.20000
AFIX 0
C62 1 -0.092978 0.268982 -0.071631 11.00000 0.01917 0.01726 =
0.02902 -0.01554 -0.00680 0.00189
AFIX 43
H62 2 -0.149989 0.265420 -0.103691 11.00000 -1.20000
AFIX 0
C63 1 0.414979 0.443312 -0.046622 11.00000 0.01696 0.02275 =
0.02421 0.00039 0.00210 0.00331
AFIX 43
H63 2 0.456326 0.408207 -0.048811 11.00000 -1.20000
AFIX 0
C64 1 1.012275 0.437663 0.556850 11.00000 0.03487 0.02484 =
0.03234 0.00257 -0.00973 -0.01052
AFIX 43
H64 2 1.071270 0.442612 0.587795 11.00000 -1.20000
AFIX 0
C65 1 0.683279 0.655172 0.353300 11.00000 0.04451 0.01850 =
0.03025 0.00772 -0.00002 -0.01336
AFIX 43
H65 2 0.708038 0.690264 0.338130 11.00000 -1.20000
AFIX 0
C68 1 1.137932 0.395712 0.497493 11.00000 0.02008 0.03617 =
0.05884 0.01332 -0.00778 0.00105
AFIX 43
H68 2 1.200198 0.400316 0.526753 11.00000 -1.20000
AFIX 0
C70 1 0.968738 0.328538 0.307520 11.00000 0.06939 0.02654 =
0.04733 -0.00041 0.04165 0.00784
AFIX 43
H70 2 0.972417 0.310825 0.272853 11.00000 -1.20000
AFIX 0
C72 1 0.572879 0.243925 0.495943 11.00000 0.01456 0.02866 =
0.07096 0.02870 -0.00484 -0.00156
AFIX 43
H72 2 0.650007 0.240784 0.502476 11.00000 -1.20000
AFIX 0
C75 1 1.062553 0.335950 0.348574 11.00000 0.04570 0.03271 =
0.05937 0.01061 0.03981 0.01516
AFIX 43
H75 2 1.130975 0.323331 0.341965 11.00000 -1.20000
AFIX 0
C76 1 -0.066456 0.334350 -0.170451 11.00000 0.04150 0.04285 =
0.02772 0.00133 -0.01439 0.00269
AFIX 137
H76A 2 -0.044132 0.359850 -0.198501 11.00000 -1.50000
H76B 2 -0.132559 0.350721 -0.160813 11.00000 -1.50000
H76C 2 -0.081238 0.293924 -0.185435 11.00000 -1.50000
AFIX 0
C77 1 0.408580 0.294277 0.460801 11.00000 0.02466 0.04615 =
0.16684 0.06821 0.03163 0.01667
AFIX 43
H77 2 0.368664 0.327736 0.443610 11.00000 -1.20000
AFIX 0
C83 1 0.864504 0.642804 0.298636 11.00000 0.07857 0.03148 =
0.05871 0.00148 0.03733 -0.02400
AFIX 137
H83A 2 0.811114 0.668178 0.274297 11.00000 -1.50000
H83B 2 0.921048 0.630488 0.278846 11.00000 -1.50000
H83C 2 0.898020 0.665204 0.332142 11.00000 -1.50000
AFIX 0
N1 3 0.402254 0.198085 0.504638 11.00000 0.02212 0.01425 =
0.01436 -0.00017 0.00669 0.00007
C2 1 0.352308 0.245235 0.477670 11.00000 0.01648 0.04394 =
0.15031 0.05995 0.03039 0.01157
AFIX 43
H2 2 0.274900 0.245972 0.469332 11.00000 -1.20000
AFIX 0
HKLF 4
REM 20181024njlydx_0m in P21/c #14
REM R1 = 0.0656 for 7948 Fo > 4sig(Fo) and 0.0942 for all 11108 data
REM 633 parameters refined using 0 restraints
END
WGHT 0.0944 5.8562
REM Highest difference peak 0.628, deepest hole -0.718, 1-sigma level 0.104
Q1 1 0.7776 0.4334 0.4200 11.00000 0.05 0.63
Q2 1 0.2355 0.3451 0.0086 11.00000 0.05 0.58
Q3 1 0.7635 0.3981 0.4296 11.00000 0.05 0.58
Q4 1 0.3650 0.3649 0.0774 11.00000 0.05 0.57
Q5 1 0.3504 0.3472 0.0634 11.00000 0.05 0.54
Q6 1 0.3695 0.3966 0.0510 11.00000 0.05 0.54
Q7 1 0.3680 0.3124 0.4237 11.00000 0.05 0.53
Q8 1 0.6639 0.3904 0.4082 11.00000 0.05 0.52
Q9 1 0.2412 0.3965 0.0103 11.00000 0.05 0.52
Q10 1 0.6488 0.4310 0.3594 11.00000 0.05 0.49
Q11 1 0.7796 0.3840 0.4022 11.00000 0.05 0.49
Q12 1 0.6927 0.4709 0.3793 11.00000 0.05 0.48
Q13 1 0.7901 0.3936 0.3810 11.00000 0.05 0.48
Q14 1 0.6553 0.3852 0.3644 11.00000 0.05 0.47
Q15 1 0.6132 0.4274 0.3862 11.00000 0.05 0.46
Q16 1 0.5007 0.4087 0.4773 11.00000 0.05 0.45
Q17 1 1.1243 0.3635 0.4765 11.00000 0.05 0.45
Q18 1 0.2205 0.4077 0.0594 11.00000 0.05 0.45
Q19 1 -0.1668 0.2767 -0.1330 11.00000 0.05 0.43
Q20 1 0.8453 0.3135 0.3577 11.00000 0.05 0.43
REM The information below was added by Olex2.
REM
REM R1 = 0.0656 for 7948 Fo > 4sig(Fo) and 0.0942 for all 38138 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.63, deepest hole -0.72
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0942
REM R1_gt = 0.0656
REM wR_ref = 0.1838
REM GOOF = 1.107
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 38138
REM Reflections_gt = 7948
REM Parameters = n/a
REM Hole = -0.72
REM Peak = 0.63
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'