# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_FJU-67
_database_code_depnum_ccdc_archive 'CCDC 1851265'
_audit_update_record
;
2018-06-24 deposited with the CCDC.
2018-10-30 downloaded from the CCDC.
;
_audit_creation_date 2016-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number 2013-2
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C32 H22 Cd N6 O8'
_chemical_formula_sum 'C32 H22 Cd N6 O8'
_chemical_formula_weight 730.95
_chemical_melting_point ?
_chemical_oxdiff_formula 'c1 h1 o1 n1 cd1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.9477(5)
_cell_length_b 12.6996(5)
_cell_length_c 12.7984(4)
_cell_angle_alpha 110.328(3)
_cell_angle_beta 100.145(3)
_cell_angle_gamma 108.530(4)
_cell_volume 1497.63(10)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 10212
_cell_measurement_temperature 296.62(10)
_cell_measurement_theta_max 74.0850
_cell_measurement_theta_min 3.8620
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 6.392
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.72347
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.621
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description bright
_exptl_crystal_F_000 736
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0228
_diffrn_reflns_av_unetI/netI 0.0242
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 17211
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 74.116
_diffrn_reflns_theta_min 3.891
_diffrn_ambient_environment air
_diffrn_ambient_temperature 296.62(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.5148
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -115.00 -17.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 -38.0000 60.0000 98
#__ type_ start__ end____ width___ exp.time_
2 omega -96.00 -2.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 125.0000 -90.0000 94
#__ type_ start__ end____ width___ exp.time_
3 omega -50.00 33.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 38.0000 60.0000 83
#__ type_ start__ end____ width___ exp.time_
4 omega -50.00 33.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 38.0000 -150.0000 83
#__ type_ start__ end____ width___ exp.time_
5 omega 23.00 97.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 41.0749 -125.0000 -180.0000 74
#__ type_ start__ end____ width___ exp.time_
6 omega 23.00 97.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 41.0749 -125.0000 -30.0000 74
#__ type_ start__ end____ width___ exp.time_
7 omega 23.00 97.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 41.0749 -125.0000 -120.0000 74
#__ type_ start__ end____ width___ exp.time_
8 omega 30.00 91.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -30.0000 -180.0000 61
#__ type_ start__ end____ width___ exp.time_
9 omega 30.00 91.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -30.0000 0.0000 61
#__ type_ start__ end____ width___ exp.time_
10 omega 30.00 91.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -30.0000 -60.0000 61
#__ type_ start__ end____ width___ exp.time_
11 omega 24.00 109.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -94.0000 -60.0000 85
#__ type_ start__ end____ width___ exp.time_
12 omega 24.00 109.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -94.0000 120.0000 85
#__ type_ start__ end____ width___ exp.time_
13 omega 33.00 98.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -45.0000 120.0000 65
#__ type_ start__ end____ width___ exp.time_
14 omega 30.00 139.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -77.0000 -30.0000 109
#__ type_ start__ end____ width___ exp.time_
15 omega 94.00 178.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 125.0000 0.0000 84
#__ type_ start__ end____ width___ exp.time_
16 omega 78.00 178.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 30.0000 0.0000 100
#__ type_ start__ end____ width___ exp.time_
17 omega 33.00 121.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -125.0000 60.0000 88
#__ type_ start__ end____ width___ exp.time_
18 omega 30.00 91.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -30.0000 60.0000 61
#__ type_ start__ end____ width___ exp.time_
19 omega 30.00 91.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -30.0000 90.0000 61
#__ type_ start__ end____ width___ exp.time_
20 omega 81.00 178.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 45.0000 90.0000 97
#__ type_ start__ end____ width___ exp.time_
21 omega 33.00 121.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -125.0000 -90.0000 88
#__ type_ start__ end____ width___ exp.time_
22 omega -114.00 -13.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 -57.0000 -180.0000 101
#__ type_ start__ end____ width___ exp.time_
23 omega -114.00 -13.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 -57.0000 -90.0000 101
;
_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 -0.0749532000
_diffrn_orient_matrix_UB_12 -0.1147045000
_diffrn_orient_matrix_UB_13 -0.1189967000
_diffrn_orient_matrix_UB_21 -0.1113215000
_diffrn_orient_matrix_UB_22 0.0459501000
_diffrn_orient_matrix_UB_23 -0.0250981000
_diffrn_orient_matrix_UB_31 0.0810531000
_diffrn_orient_matrix_UB_32 0.0697148000
_diffrn_orient_matrix_UB_33 -0.0599806000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5495
_reflns_number_total 5940
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max 0.562
_refine_diff_density_min -0.618
_refine_diff_density_rms 0.061
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.056
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 439
_refine_ls_number_reflns 5940
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0277
_refine_ls_R_factor_gt 0.0242
_refine_ls_restrained_S_all 1.056
_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^)+(0.0379P)^2^+0.3483P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0624
_refine_ls_wR_factor_ref 0.0647
_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.a Aromatic/amide H refined with riding coordinates:
N4(H4), N1(H1), C8(H8), C3(H3), C7(H7), C2AA(H2AA), C3AA(H3AA), C35(H35),
C4(H4A), C34(H34)
2.b Idealised Me refined as rotating group:
C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C)
;
_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
Cd1 Cd 0.32678(2) 0.78415(2) 0.31171(2) 0.02659(6) Uani 1 1 d . . . . .
O3 O 0.13314(19) 0.77321(17) 0.36613(16) 0.0464(4) Uani 1 1 d . . . . .
O2 O 0.44635(19) 0.76298(16) 0.47573(15) 0.0437(4) Uani 1 1 d . . . . .
O4 O 0.2769(2) 0.95274(19) 0.3930(2) 0.0581(5) Uani 1 1 d . . . . .
O1 O 0.3438(2) 0.60441(17) 0.30345(15) 0.0476(4) Uani 1 1 d . . . . .
O7 O -0.04256(18) 0.63021(17) -0.16607(14) 0.0410(4) Uani 1 1 d . . . . .
N2 N 0.2367(2) 0.66202(17) 0.11069(15) 0.0320(4) Uani 1 1 d . . . . .
O6 O 0.58904(18) 0.8845(2) -0.02175(17) 0.0604(6) Uani 1 1 d . . . . .
N3 N 0.51270(19) 0.90822(17) 0.29291(17) 0.0334(4) Uani 1 1 d . . . . .
O8 O 0.25193(19) 0.45244(19) -0.24864(15) 0.0483(4) Uani 1 1 d . . . . .
N4 N 0.5451(2) 1.02987(18) 0.32588(17) 0.0366(4) Uani 1 1 d . . . . .
H4 H 0.5096 1.0708 0.3697 0.044 Uiso 1 1 calc R . . . .
N1 N 0.19459(19) 0.53894(17) 0.07364(15) 0.0310(4) Uani 1 1 d . . . . .
H1 H 0.2007 0.5049 0.1207 0.037 Uiso 1 1 calc R . . . .
O5 O 0.93585(19) 1.1087(2) 0.32586(16) 0.0567(5) Uani 1 1 d . . . . .
N6 N 0.10608(19) 0.54264(17) -0.20573(15) 0.0309(4) Uani 1 1 d . . . . .
N5 N 0.7614(2) 0.98919(19) 0.15255(18) 0.0384(5) Uani 1 1 d . . . . .
C12 C 0.5866(2) 0.8785(2) 0.2249(2) 0.0352(5) Uani 1 1 d . . . . .
C6 C 0.4613(2) 0.5745(2) 0.45604(19) 0.0310(4) Uani 1 1 d . . . . .
C11 C 0.2124(2) 0.6786(2) 0.01294(19) 0.0317(5) Uani 1 1 d . . . . .
C1 C 0.4147(2) 0.6533(2) 0.40929(19) 0.0313(4) Uani 1 1 d . . . . .
C8 C 0.4833(2) 0.3844(2) 0.4235(2) 0.0369(5) Uani 1 1 d . . . . .
H8 H 0.4715 0.3065 0.3721 0.044 Uiso 1 1 calc R . . . .
C28 C 0.0200(2) 0.50688(19) -0.44151(16) 0.0262(4) Uani 1 1 d . . . . .
C1AA C 0.1178(2) 0.4641(2) -0.40765(18) 0.0290(4) Uani 1 1 d . . . . .
C17 C 0.2504(4) 0.8039(3) 0.0187(3) 0.0513(7) Uani 1 1 d . . . . .
C19 C -0.0365(2) 0.5652(2) -0.36127(18) 0.0282(4) Uani 1 1 d . . . . .
C2 C 0.1690(2) 0.8865(2) 0.4004(2) 0.0375(5) Uani 1 1 d . . . . .
C36 C 0.8120(2) 0.9430(2) -0.0337(2) 0.0350(5) Uani 1 1 d . . . . .
C9 C 0.1423(2) 0.4754(2) -0.04355(18) 0.0305(4) Uani 1 1 d . . . . .
C3 C 0.1354(3) 1.0710(2) 0.5221(2) 0.0410(5) Uani 1 1 d . . . . .
H3 H 0.2263 1.1190 0.5372 0.049 Uiso 1 1 calc R . . . .
C20 C 0.0053(2) 0.5820(2) -0.23771(18) 0.0306(4) Uani 1 1 d . . . . .
C13 C 0.6660(2) 0.9827(2) 0.2161(2) 0.0371(5) Uani 1 1 d . . . . .
C33 C 0.9994(2) 1.0485(2) 0.1546(2) 0.0354(5) Uani 1 1 d . . . . .
C14 C 0.6393(3) 1.0790(2) 0.2822(2) 0.0397(5) Uani 1 1 d . . . . .
C7 C 0.4453(3) 0.4590(2) 0.3795(2) 0.0370(5) Uani 1 1 d . . . . .
H7 H 0.4093 0.4315 0.2987 0.044 Uiso 1 1 calc R . . . .
C16 C 0.5805(3) 0.7516(3) 0.1720(3) 0.0563(8) Uani 1 1 d . . . . .
H16A H 0.5349 0.7047 0.2092 0.084 Uiso 1 1 calc GR . . . .
H16B H 0.6712 0.7556 0.1836 0.084 Uiso 1 1 calc GR . . . .
H16C H 0.5314 0.7128 0.0893 0.084 Uiso 1 1 calc GR . . . .
C10 C 0.1515(2) 0.5636(2) -0.08510(18) 0.0309(4) Uani 1 1 d . . . . .
C5 C 0.0809(2) 0.9456(2) 0.4511(2) 0.0363(5) Uani 1 1 d . . . . .
C45 C 0.9522(2) 0.9975(2) 0.0309(2) 0.0318(5) Uani 1 1 d . . . . .
C2AA C 0.1704(2) 0.4069(2) -0.4881(2) 0.0359(5) Uani 1 1 d . . . . .
H2AA H 0.2338 0.3779 -0.4656 0.043 Uiso 1 1 calc R . . . .
C18 C 0.0931(3) 0.3396(2) -0.1020(2) 0.0424(6) Uani 1 1 d . . . . .
H18A H 0.1681 0.3182 -0.1125 0.064 Uiso 1 1 calc GR . . . .
H18B H 0.0260 0.3076 -0.1772 0.064 Uiso 1 1 calc GR . . . .
H18C H 0.0533 0.3050 -0.0539 0.064 Uiso 1 1 calc GR . . . .
C0AA C 0.1656(2) 0.4839(2) -0.28355(19) 0.0330(5) Uani 1 1 d . . . . .
C37 C 0.7102(2) 0.9351(2) 0.0293(2) 0.0398(5) Uani 1 1 d . . . . .
C3AA C -0.1290(2) 0.6082(2) -0.39532(19) 0.0344(5) Uani 1 1 d . . . . .
H3AA H -0.1647 0.6476 -0.3410 0.041 Uiso 1 1 calc R . . . .
C35 C 0.7700(2) 0.8993(2) -0.1537(2) 0.0429(6) Uani 1 1 d . . . . .
H35 H 0.6777 0.8665 -0.1950 0.051 Uiso 1 1 calc R . . . .
C4 C -0.0545(3) 0.8748(2) 0.4292(2) 0.0410(5) Uani 1 1 d . . . . .
H4A H -0.0916 0.7905 0.3817 0.049 Uiso 1 1 calc R . . . .
C32 C 0.9011(2) 1.0524(2) 0.2202(2) 0.0392(5) Uani 1 1 d . . . . .
C15 C 0.6973(4) 1.2110(3) 0.3073(3) 0.0701(10) Uani 1 1 d . . . . .
H15A H 0.6276 1.2309 0.2728 0.105 Uiso 1 1 calc GR . . . .
H15B H 0.7697 1.2273 0.2745 0.105 Uiso 1 1 calc GR . . . .
H15C H 0.7321 1.2604 0.3909 0.105 Uiso 1 1 calc GR . . . .
C34 C 1.1360(3) 1.0968(3) 0.2152(2) 0.0430(6) Uani 1 1 d . . . . .
H34 H 1.1658 1.1267 0.2967 0.052 Uiso 1 1 calc R . . . .
H17A H 0.297(4) 0.865(4) 0.092(4) 0.082(12) Uiso 1 1 d . . . . .
H17B H 0.173(5) 0.810(4) -0.023(4) 0.111(16) Uiso 1 1 d . . . . .
H17C H 0.298(6) 0.813(5) -0.035(5) 0.15(2) Uiso 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.03159(8) 0.03081(9) 0.02348(8) 0.01283(6) 0.01271(6) 0.01692(6)
O3 0.0515(10) 0.0470(11) 0.0467(10) 0.0132(8) 0.0236(9) 0.0314(9)
O2 0.0626(11) 0.0382(9) 0.0348(9) 0.0158(7) 0.0117(8) 0.0282(8)
O4 0.0583(12) 0.0523(12) 0.0792(15) 0.0244(11) 0.0455(11) 0.0332(10)
O1 0.0670(12) 0.0450(10) 0.0294(8) 0.0162(8) 0.0001(8) 0.0292(9)
O7 0.0512(10) 0.0582(11) 0.0251(8) 0.0193(8) 0.0195(7) 0.0311(9)
N2 0.0453(10) 0.0320(10) 0.0211(8) 0.0123(7) 0.0096(8) 0.0183(8)
O6 0.0314(9) 0.0865(16) 0.0450(11) 0.0162(10) 0.0174(8) 0.0131(9)
N3 0.0358(10) 0.0330(10) 0.0359(10) 0.0148(8) 0.0196(8) 0.0155(8)
O8 0.0566(11) 0.0762(13) 0.0295(8) 0.0266(9) 0.0151(8) 0.0436(10)
N4 0.0405(10) 0.0335(10) 0.0370(10) 0.0110(8) 0.0236(9) 0.0154(8)
N1 0.0420(10) 0.0325(10) 0.0212(8) 0.0141(7) 0.0097(8) 0.0160(8)
O5 0.0476(10) 0.0854(15) 0.0301(9) 0.0184(9) 0.0194(8) 0.0222(10)
N6 0.0384(10) 0.0383(10) 0.0177(8) 0.0132(7) 0.0086(7) 0.0170(8)
N5 0.0335(10) 0.0454(12) 0.0357(10) 0.0146(9) 0.0214(9) 0.0132(9)
C12 0.0350(11) 0.0377(12) 0.0360(12) 0.0136(10) 0.0191(10) 0.0173(10)
C6 0.0345(11) 0.0350(12) 0.0260(10) 0.0154(9) 0.0064(9) 0.0165(9)
C11 0.0395(11) 0.0361(12) 0.0220(10) 0.0145(9) 0.0091(9) 0.0168(10)
C1 0.0350(11) 0.0355(12) 0.0304(11) 0.0178(9) 0.0118(9) 0.0183(9)
C8 0.0465(13) 0.0330(11) 0.0267(11) 0.0078(9) 0.0049(10) 0.0204(10)
C28 0.0267(9) 0.0294(10) 0.0196(10) 0.0108(8) 0.0070(8) 0.0081(8)
C1AA 0.0314(10) 0.0340(11) 0.0201(10) 0.0119(8) 0.0078(8) 0.0116(9)
C17 0.072(2) 0.0383(15) 0.0357(14) 0.0191(12) 0.0057(14) 0.0164(14)
C19 0.0286(10) 0.0334(11) 0.0213(10) 0.0124(8) 0.0081(8) 0.0106(9)
C2 0.0422(13) 0.0515(15) 0.0251(10) 0.0125(10) 0.0135(10) 0.0300(12)
C36 0.0326(11) 0.0367(12) 0.0334(11) 0.0111(10) 0.0168(9) 0.0127(9)
C9 0.0351(11) 0.0358(12) 0.0209(9) 0.0119(9) 0.0085(8) 0.0156(9)
C3 0.0386(12) 0.0465(14) 0.0374(12) 0.0116(11) 0.0160(10) 0.0223(11)
C20 0.0326(11) 0.0362(12) 0.0215(10) 0.0124(9) 0.0089(8) 0.0122(9)
C13 0.0343(11) 0.0412(13) 0.0373(12) 0.0146(10) 0.0217(10) 0.0146(10)
C33 0.0343(11) 0.0407(13) 0.0315(11) 0.0142(10) 0.0163(10) 0.0144(10)
C14 0.0402(12) 0.0373(13) 0.0428(13) 0.0161(11) 0.0233(11) 0.0132(10)
C7 0.0486(13) 0.0402(13) 0.0219(10) 0.0113(9) 0.0055(9) 0.0235(11)
C16 0.0574(17) 0.0451(16) 0.076(2) 0.0216(15) 0.0420(16) 0.0273(13)
C10 0.0397(11) 0.0368(12) 0.0181(9) 0.0128(9) 0.0097(9) 0.0168(10)
C5 0.0428(12) 0.0438(13) 0.0296(11) 0.0126(10) 0.0170(10) 0.0274(11)
C45 0.0327(11) 0.0341(11) 0.0306(11) 0.0133(9) 0.0160(9) 0.0140(9)
C2AA 0.0374(12) 0.0487(14) 0.0279(11) 0.0173(10) 0.0112(9) 0.0239(11)
C18 0.0552(15) 0.0351(13) 0.0326(12) 0.0119(10) 0.0109(11) 0.0181(11)
C0AA 0.0378(11) 0.0412(12) 0.0226(10) 0.0151(9) 0.0096(9) 0.0177(10)
C37 0.0322(11) 0.0448(14) 0.0387(13) 0.0139(11) 0.0183(10) 0.0124(10)
C3AA 0.0375(11) 0.0461(13) 0.0248(10) 0.0148(10) 0.0137(9) 0.0218(10)
C35 0.0300(11) 0.0533(15) 0.0342(12) 0.0099(11) 0.0106(10) 0.0134(11)
C4 0.0435(13) 0.0406(13) 0.0367(13) 0.0079(10) 0.0156(11) 0.0228(11)
C32 0.0382(12) 0.0495(14) 0.0333(12) 0.0182(11) 0.0189(10) 0.0177(11)
C15 0.082(2) 0.0386(16) 0.096(3) 0.0259(17) 0.061(2) 0.0193(16)
C34 0.0386(12) 0.0565(16) 0.0274(11) 0.0116(11) 0.0136(10) 0.0175(12)
_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
Cd1 O3 2.3235(17) . ?
Cd1 O2 2.4166(17) . ?
Cd1 O4 2.3152(19) . ?
Cd1 O1 2.3165(17) . ?
Cd1 N2 2.3148(18) . ?
Cd1 N3 2.2541(18) . ?
Cd1 C1 2.699(2) . ?
Cd1 C2 2.656(2) . ?
O3 C2 1.248(3) . ?
O2 C1 1.245(3) . ?
O4 C2 1.256(3) . ?
O1 C1 1.250(3) . ?
O7 C20 1.214(3) . ?
N2 N1 1.353(3) . ?
N2 C11 1.335(3) . ?
O6 C37 1.208(3) . ?
N3 N4 1.355(3) . ?
N3 C12 1.330(3) . ?
O8 C0AA 1.211(3) . ?
N4 C14 1.343(3) . ?
N1 C9 1.338(3) . ?
O5 C32 1.208(3) . ?
N6 C20 1.403(3) . ?
N6 C10 1.436(2) . ?
N6 C0AA 1.412(3) . ?
N5 C13 1.432(3) . ?
N5 C37 1.402(3) . ?
N5 C32 1.416(3) . ?
C12 C13 1.388(3) . ?
C12 C16 1.489(4) . ?
C6 C1 1.501(3) . ?
C6 C8 1.388(3) 2_666 ?
C6 C7 1.386(3) . ?
C11 C17 1.483(4) . ?
C11 C10 1.401(3) . ?
C8 C6 1.388(3) 2_666 ?
C8 C7 1.388(3) . ?
C28 C28 1.415(4) 2_564 ?
C28 C1AA 1.414(3) . ?
C28 C19 1.404(3) . ?
C1AA C2AA 1.370(3) . ?
C1AA C0AA 1.485(3) . ?
C19 C20 1.485(3) . ?
C19 C3AA 1.369(3) . ?
C2 C5 1.502(3) . ?
C36 C45 1.414(3) . ?
C36 C37 1.485(3) . ?
C36 C35 1.369(3) . ?
C9 C10 1.382(3) . ?
C9 C18 1.482(3) . ?
C3 C5 1.384(4) . ?
C3 C4 1.389(3) 2_576 ?
C13 C14 1.375(3) . ?
C33 C45 1.407(3) . ?
C33 C32 1.479(3) . ?
C33 C34 1.376(3) . ?
C14 C15 1.481(4) . ?
C5 C4 1.385(4) . ?
C45 C45 1.417(4) 2_775 ?
C2AA C3AA 1.406(3) 2_564 ?
C3AA C2AA 1.406(3) 2_564 ?
C35 C34 1.401(3) 2_775 ?
C4 C3 1.389(3) 2_576 ?
C34 C35 1.401(3) 2_775 ?
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
O3 Cd1 O2 96.23(7) . . ?
O3 Cd1 C1 101.10(7) . . ?
O3 Cd1 C2 28.03(7) . . ?
O2 Cd1 C1 27.47(6) . . ?
O2 Cd1 C2 102.43(6) . . ?
O4 Cd1 O3 56.23(7) . . ?
O4 Cd1 O2 106.05(7) . . ?
O4 Cd1 O1 152.64(7) . . ?
O4 Cd1 C1 131.17(8) . . ?
O4 Cd1 C2 28.20(7) . . ?
O1 Cd1 O3 102.85(7) . . ?
O1 Cd1 O2 54.99(6) . . ?
O1 Cd1 C1 27.53(6) . . ?
O1 Cd1 C2 128.87(8) . . ?
N2 Cd1 O3 102.50(7) . . ?
N2 Cd1 O2 133.70(6) . . ?
N2 Cd1 O4 119.63(8) . . ?
N2 Cd1 O1 79.53(6) . . ?
N2 Cd1 C1 106.65(7) . . ?
N2 Cd1 C2 113.89(7) . . ?
N3 Cd1 O3 144.85(7) . . ?
N3 Cd1 O2 96.48(7) . . ?
N3 Cd1 O4 88.75(7) . . ?
N3 Cd1 O1 111.28(7) . . ?
N3 Cd1 N2 91.92(7) . . ?
N3 Cd1 C1 105.21(7) . . ?
N3 Cd1 C2 116.91(8) . . ?
C2 Cd1 C1 118.65(7) . . ?
C2 O3 Cd1 90.98(15) . . ?
C1 O2 Cd1 88.99(13) . . ?
C2 O4 Cd1 91.17(15) . . ?
C1 O1 Cd1 93.52(14) . . ?
N1 N2 Cd1 117.33(12) . . ?
C11 N2 Cd1 137.16(15) . . ?
C11 N2 N1 105.50(17) . . ?
N4 N3 Cd1 122.48(13) . . ?
C12 N3 Cd1 129.14(16) . . ?
C12 N3 N4 106.13(18) . . ?
C14 N4 N3 112.12(19) . . ?
C9 N1 N2 113.30(17) . . ?
C20 N6 C10 117.39(18) . . ?
C20 N6 C0AA 124.74(17) . . ?
C0AA N6 C10 117.87(18) . . ?
C37 N5 C13 118.06(19) . . ?
C37 N5 C32 125.11(18) . . ?
C32 N5 C13 116.82(19) . . ?
N3 C12 C13 109.0(2) . . ?
N3 C12 C16 122.3(2) . . ?
C13 C12 C16 128.7(2) . . ?
C8 C6 C1 120.0(2) 2_666 . ?
C7 C6 C1 120.2(2) . . ?
C7 C6 C8 119.8(2) . 2_666 ?
N2 C11 C17 121.0(2) . . ?
N2 C11 C10 109.13(19) . . ?
C10 C11 C17 129.8(2) . . ?
O2 C1 Cd1 63.55(12) . . ?
O2 C1 O1 122.5(2) . . ?
O2 C1 C6 119.9(2) . . ?
O1 C1 Cd1 58.95(12) . . ?
O1 C1 C6 117.6(2) . . ?
C6 C1 Cd1 176.47(16) . . ?
C7 C8 C6 120.3(2) . 2_666 ?
C1AA C28 C28 119.3(2) . 2_564 ?
C19 C28 C28 119.0(2) . 2_564 ?
C19 C28 C1AA 121.66(18) . . ?
C28 C1AA C0AA 119.69(19) . . ?
C2AA C1AA C28 120.31(19) . . ?
C2AA C1AA C0AA 120.0(2) . . ?
C28 C19 C20 119.92(19) . . ?
C3AA C19 C28 120.71(19) . . ?
C3AA C19 C20 119.4(2) . . ?
O3 C2 Cd1 61.00(12) . . ?
O3 C2 O4 121.6(2) . . ?
O3 C2 C5 119.5(2) . . ?
O4 C2 Cd1 60.62(13) . . ?
O4 C2 C5 118.8(2) . . ?
C5 C2 Cd1 179.42(19) . . ?
C45 C36 C37 119.7(2) . . ?
C35 C36 C45 120.3(2) . . ?
C35 C36 C37 120.0(2) . . ?
N1 C9 C10 104.85(19) . . ?
N1 C9 C18 121.7(2) . . ?
C10 C9 C18 133.4(2) . . ?
C5 C3 C4 120.2(2) . 2_576 ?
O7 C20 N6 120.91(19) . . ?
O7 C20 C19 122.0(2) . . ?
N6 C20 C19 117.05(19) . . ?
C12 C13 N5 126.0(2) . . ?
C14 C13 N5 126.3(2) . . ?
C14 C13 C12 107.7(2) . . ?
C45 C33 C32 119.6(2) . . ?
C34 C33 C45 120.8(2) . . ?
C34 C33 C32 119.7(2) . . ?
N4 C14 C13 105.1(2) . . ?
N4 C14 C15 123.8(2) . . ?
C13 C14 C15 131.1(2) . . ?
C6 C7 C8 119.9(2) . . ?
C11 C10 N6 125.9(2) . . ?
C9 C10 N6 126.9(2) . . ?
C9 C10 C11 107.19(18) . . ?
C3 C5 C2 120.2(2) . . ?
C3 C5 C4 119.5(2) . . ?
C4 C5 C2 120.3(2) . . ?
C36 C45 C45 118.9(3) . 2_775 ?
C33 C45 C36 121.9(2) . . ?
C33 C45 C45 119.2(3) . 2_775 ?
C1AA C2AA C3AA 120.2(2) . 2_564 ?
O8 C0AA N6 120.48(19) . . ?
O8 C0AA C1AA 122.7(2) . . ?
N6 C0AA C1AA 116.86(19) . . ?
O6 C37 N5 120.9(2) . . ?
O6 C37 C36 122.5(2) . . ?
N5 C37 C36 116.6(2) . . ?
C19 C3AA C2AA 120.4(2) . 2_564 ?
C36 C35 C34 121.0(2) . 2_775 ?
C5 C4 C3 120.3(2) . 2_576 ?
O5 C32 N5 120.5(2) . . ?
O5 C32 C33 122.8(2) . . ?
N5 C32 C33 116.6(2) . . ?
C33 C34 C35 119.7(2) . 2_775 ?
_shelx_res_file
;
TITL CF solution in P-1
CELL 1.54184 10.94766 12.699589 12.798379 110.3282 100.1445 108.5304
ZERR 2 0.000454 0.000472 0.000392 0.0031 0.003 0.0035
LATT 1
SFAC C H Cd N O
UNIT 64 44 2 12 16
L.S. 4
PLAN 25
BOND
fmap 2
acta
REM
REM
REM
WGHT 0.037900 0.348300
FVAR 5.49038
CD1 3 0.326779 0.784146 0.311708 11.00000 0.03159 0.03081 =
0.02348 0.01283 0.01271 0.01692
O3 5 0.133135 0.773211 0.366132 11.00000 0.05153 0.04703 =
0.04675 0.01322 0.02361 0.03137
O2 5 0.446352 0.762982 0.475725 11.00000 0.06260 0.03819 =
0.03482 0.01585 0.01171 0.02821
O4 5 0.276901 0.952744 0.392965 11.00000 0.05826 0.05228 =
0.07918 0.02437 0.04553 0.03321
O1 5 0.343837 0.604411 0.303446 11.00000 0.06696 0.04499 =
0.02938 0.01618 0.00008 0.02925
O7 5 -0.042556 0.630212 -0.166074 11.00000 0.05116 0.05817 =
0.02512 0.01928 0.01945 0.03113
N2 4 0.236747 0.662024 0.110693 11.00000 0.04535 0.03196 =
0.02108 0.01229 0.00960 0.01827
O6 5 0.589044 0.884484 -0.021754 11.00000 0.03142 0.08653 =
0.04496 0.01617 0.01736 0.01313
N3 4 0.512697 0.908218 0.292909 11.00000 0.03582 0.03300 =
0.03594 0.01479 0.01961 0.01548
O8 5 0.251934 0.452440 -0.248639 11.00000 0.05664 0.07616 =
0.02953 0.02656 0.01509 0.04361
N4 4 0.545145 1.029872 0.325878 11.00000 0.04051 0.03348 =
0.03700 0.01101 0.02360 0.01545
AFIX 43
H4 2 0.509560 1.070809 0.369690 11.00000 -1.20000
AFIX 0
N1 4 0.194590 0.538944 0.073644 11.00000 0.04197 0.03248 =
0.02121 0.01413 0.00971 0.01603
AFIX 43
H1 2 0.200748 0.504899 0.120715 11.00000 -1.20000
AFIX 0
O5 5 0.935846 1.108744 0.325859 11.00000 0.04757 0.08540 =
0.03010 0.01845 0.01939 0.02221
N6 4 0.106083 0.542636 -0.205731 11.00000 0.03837 0.03832 =
0.01767 0.01319 0.00857 0.01696
N5 4 0.761415 0.989192 0.152545 11.00000 0.03349 0.04535 =
0.03570 0.01460 0.02135 0.01324
C12 1 0.586633 0.878521 0.224947 11.00000 0.03495 0.03772 =
0.03603 0.01357 0.01914 0.01730
C6 1 0.461289 0.574477 0.456039 11.00000 0.03447 0.03499 =
0.02600 0.01536 0.00644 0.01655
C11 1 0.212431 0.678585 0.012942 11.00000 0.03953 0.03608 =
0.02195 0.01445 0.00914 0.01682
C1 1 0.414718 0.653294 0.409293 11.00000 0.03497 0.03548 =
0.03041 0.01782 0.01180 0.01832
C8 1 0.483263 0.384414 0.423525 11.00000 0.04646 0.03299 =
0.02675 0.00778 0.00486 0.02041
AFIX 43
H8 2 0.471463 0.306513 0.372115 11.00000 -1.20000
AFIX 0
C28 1 0.019983 0.506879 -0.441514 11.00000 0.02666 0.02940 =
0.01958 0.01075 0.00702 0.00807
C1AA 1 0.117750 0.464086 -0.407648 11.00000 0.03138 0.03404 =
0.02011 0.01188 0.00780 0.01164
C17 1 0.250359 0.803897 0.018700 11.00000 0.07235 0.03828 =
0.03574 0.01915 0.00566 0.01641
C19 1 -0.036469 0.565227 -0.361271 11.00000 0.02857 0.03345 =
0.02131 0.01236 0.00810 0.01056
C2 1 0.168959 0.886491 0.400389 11.00000 0.04221 0.05149 =
0.02514 0.01254 0.01353 0.03001
C36 1 0.811972 0.943025 -0.033724 11.00000 0.03264 0.03671 =
0.03339 0.01111 0.01683 0.01272
C9 1 0.142348 0.475441 -0.043545 11.00000 0.03513 0.03579 =
0.02086 0.01187 0.00853 0.01562
C3 1 0.135357 1.070968 0.522070 11.00000 0.03865 0.04654 =
0.03743 0.01164 0.01602 0.02227
AFIX 43
H3 2 0.226298 1.118993 0.537171 11.00000 -1.20000
AFIX 0
C20 1 0.005333 0.582045 -0.237711 11.00000 0.03257 0.03622 =
0.02149 0.01238 0.00885 0.01216
C13 1 0.665985 0.982742 0.216119 11.00000 0.03431 0.04121 =
0.03727 0.01460 0.02169 0.01463
C33 1 0.999377 1.048535 0.154577 11.00000 0.03434 0.04069 =
0.03146 0.01420 0.01625 0.01445
C14 1 0.639340 1.079038 0.282161 11.00000 0.04016 0.03733 =
0.04278 0.01607 0.02333 0.01322
C7 1 0.445350 0.458988 0.379457 11.00000 0.04862 0.04024 =
0.02190 0.01130 0.00553 0.02351
AFIX 43
H7 2 0.409301 0.431504 0.298655 11.00000 -1.20000
AFIX 0
C16 1 0.580485 0.751633 0.172046 11.00000 0.05736 0.04506 =
0.07638 0.02164 0.04197 0.02734
AFIX 137
H16A 2 0.534877 0.704666 0.209150 11.00000 -1.50000
H16B 2 0.671177 0.755589 0.183579 11.00000 -1.50000
H16C 2 0.531438 0.712826 0.089299 11.00000 -1.50000
AFIX 0
C10 1 0.151461 0.563639 -0.085100 11.00000 0.03970 0.03682 =
0.01808 0.01279 0.00970 0.01685
C5 1 0.080911 0.945606 0.451130 11.00000 0.04282 0.04378 =
0.02962 0.01259 0.01702 0.02739
C45 1 0.952215 0.997469 0.030866 11.00000 0.03275 0.03407 =
0.03060 0.01326 0.01598 0.01398
C2AA 1 0.170441 0.406886 -0.488118 11.00000 0.03736 0.04870 =
0.02790 0.01733 0.01124 0.02392
AFIX 43
H2AA 2 0.233796 0.377935 -0.465559 11.00000 -1.20000
AFIX 0
C18 1 0.093103 0.339582 -0.101952 11.00000 0.05518 0.03514 =
0.03259 0.01191 0.01085 0.01809
AFIX 137
H18A 2 0.168104 0.318202 -0.112540 11.00000 -1.50000
H18B 2 0.026041 0.307552 -0.177241 11.00000 -1.50000
H18C 2 0.053269 0.305001 -0.053902 11.00000 -1.50000
AFIX 0
C0AA 1 0.165596 0.483879 -0.283545 11.00000 0.03779 0.04119 =
0.02258 0.01510 0.00965 0.01774
C37 1 0.710171 0.935132 0.029273 11.00000 0.03223 0.04485 =
0.03871 0.01390 0.01834 0.01238
C3AA 1 -0.129032 0.608174 -0.395323 11.00000 0.03750 0.04611 =
0.02475 0.01483 0.01372 0.02185
AFIX 43
H3AA 2 -0.164729 0.647561 -0.340982 11.00000 -1.20000
AFIX 0
C35 1 0.769988 0.899269 -0.153696 11.00000 0.02995 0.05326 =
0.03419 0.00991 0.01057 0.01340
AFIX 43
H35 2 0.677698 0.866456 -0.194961 11.00000 -1.20000
AFIX 0
C4 1 -0.054530 0.874752 0.429222 11.00000 0.04351 0.04056 =
0.03673 0.00792 0.01558 0.02280
AFIX 43
H4A 2 -0.091554 0.790472 0.381704 11.00000 -1.20000
AFIX 0
C32 1 0.901121 1.052398 0.220213 11.00000 0.03822 0.04950 =
0.03330 0.01821 0.01891 0.01768
C15 1 0.697292 1.211014 0.307308 11.00000 0.08244 0.03855 =
0.09600 0.02590 0.06101 0.01930
AFIX 137
H15A 2 0.627610 1.230898 0.272840 11.00000 -1.50000
H15B 2 0.769726 1.227294 0.274480 11.00000 -1.50000
H15C 2 0.732113 1.260413 0.390907 11.00000 -1.50000
AFIX 0
C34 1 1.135986 1.096796 0.215199 11.00000 0.03864 0.05651 =
0.02744 0.01165 0.01355 0.01747
AFIX 43
H34 2 1.165789 1.126694 0.296703 11.00000 -1.20000
AFIX 0
H17A 2 0.297158 0.864653 0.091988 11.00000 0.08224
H17B 2 0.172931 0.810478 -0.022563 11.00000 0.11065
H17C 2 0.298341 0.812722 -0.034960 11.00000 0.14570
HKLF 4
REM CF solution in P-1
REM R1 = 0.0242 for 5495 Fo > 4sig(Fo) and 0.0277 for all 5940 data
REM 439 parameters refined using 0 restraints
END
WGHT 0.0379 0.3483
REM Highest difference peak 0.562, deepest hole -0.618, 1-sigma level 0.061
Q1 1 0.5498 0.5608 -0.0993 11.00000 0.05 0.56
Q2 1 -0.0242 0.3469 -0.0697 11.00000 0.05 0.47
Q3 1 0.6527 1.2688 0.3571 11.00000 0.05 0.29
Q4 1 0.0000 0.5000 -0.5000 10.50000 0.05 0.28
Q5 1 0.7756 0.9412 0.0040 11.00000 0.05 0.26
Q6 1 0.9730 1.0282 0.0924 11.00000 0.05 0.24
Q7 1 0.3652 0.8515 0.0244 11.00000 0.05 0.24
Q8 1 0.9150 1.0335 0.2996 11.00000 0.05 0.24
Q9 1 0.1880 0.6146 -0.0449 11.00000 0.05 0.24
Q10 1 0.2922 0.5253 -0.2317 11.00000 0.05 0.23
Q11 1 0.4625 0.6167 0.4285 11.00000 0.05 0.23
Q12 1 0.9588 1.0575 0.1852 11.00000 0.05 0.23
Q13 1 0.8789 0.9763 0.0002 11.00000 0.05 0.23
Q14 1 0.6200 0.7454 0.1124 11.00000 0.05 0.23
Q15 1 -0.0164 0.5608 -0.3109 11.00000 0.05 0.23
Q16 1 0.1417 0.4784 -0.3469 11.00000 0.05 0.21
Q17 1 0.2358 0.7981 -0.0592 11.00000 0.05 0.20
Q18 1 0.2585 0.8777 0.1180 11.00000 0.05 0.20
Q19 1 0.0235 0.9024 0.4582 11.00000 0.05 0.20
Q20 1 0.1185 0.9175 0.4317 11.00000 0.05 0.20
Q21 1 0.0980 1.0051 0.4703 11.00000 0.05 0.19
Q22 1 0.0690 0.4963 -0.4279 11.00000 0.05 0.19
Q23 1 -0.0205 0.5227 -0.4017 11.00000 0.05 0.19
Q24 1 0.4882 0.3999 0.4844 11.00000 0.05 0.19
Q25 1 -0.0913 0.8962 0.4630 11.00000 0.05 0.18
;
_shelx_res_checksum 22376
_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_FJU-68
_database_code_depnum_ccdc_archive 'CCDC 1851266'
_audit_update_record
;
2018-06-24 deposited with the CCDC.
2018-10-30 downloaded from the CCDC.
;
_audit_creation_date 2018-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelxl_version_number 2013-2
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C32 H20 Cd N7 O8'
_chemical_formula_sum 'C32 H20 Cd N7 O8'
_chemical_formula_weight 742.95
_chemical_melting_point ?
_chemical_oxdiff_formula 'C1 H1 O1 N1 Cd1'
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'
Cd Cd -0.8075 1.2024 '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 triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.2419(4)
_cell_length_b 12.4720(4)
_cell_length_c 12.7658(4)
_cell_angle_alpha 112.810(3)
_cell_angle_beta 98.524(3)
_cell_angle_gamma 107.333(3)
_cell_volume 1502.58(9)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 10324
_cell_measurement_temperature 292.14(10)
_cell_measurement_theta_max 73.9250
_cell_measurement_theta_min 4.1520
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.793
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.38381
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.642
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description Reddish
_exptl_crystal_F_000 746
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0248
_diffrn_reflns_av_unetI/netI 0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 16069
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full 25.214
_diffrn_reflns_theta_max 26.263
_diffrn_reflns_theta_min 1.812
_diffrn_ambient_environment air
_diffrn_ambient_temperature 292.14(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.5148
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -50.00 33.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 38.0000 120.0000 83
#__ type_ start__ end____ width___ exp.time_
2 omega -114.00 -13.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 -57.0000 -180.0000 101
#__ type_ start__ end____ width___ exp.time_
3 omega -69.00 32.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 57.0000 -30.0000 101
#__ type_ start__ end____ width___ exp.time_
4 omega 23.00 97.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 41.0749 -125.0000 120.0000 74
#__ type_ start__ end____ width___ exp.time_
5 omega 1.00 82.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 41.0749 -99.0000 30.0000 81
#__ type_ start__ end____ width___ exp.time_
6 omega 77.00 178.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 61.0000 120.0000 101
#__ type_ start__ end____ width___ exp.time_
7 omega 33.00 98.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -45.0000 -180.0000 65
#__ type_ start__ end____ width___ exp.time_
8 omega 24.00 109.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -94.0000 150.0000 85
#__ type_ start__ end____ width___ exp.time_
9 omega 24.00 109.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -94.0000 30.0000 85
#__ type_ start__ end____ width___ exp.time_
10 omega 33.00 98.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -45.0000 120.0000 65
#__ type_ start__ end____ width___ exp.time_
11 omega 33.00 121.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -125.0000 -60.0000 88
#__ type_ start__ end____ width___ exp.time_
12 omega 33.00 98.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -45.0000 0.0000 65
#__ type_ start__ end____ width___ exp.time_
13 omega 24.00 109.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -94.0000 90.0000 85
#__ type_ start__ end____ width___ exp.time_
14 omega 30.00 91.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -30.0000 -150.0000 61
#__ type_ start__ end____ width___ exp.time_
15 omega 30.00 139.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -77.0000 -60.0000 109
#__ type_ start__ end____ width___ exp.time_
16 omega 30.00 91.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -30.0000 -90.0000 61
#__ type_ start__ end____ width___ exp.time_
17 omega 18.00 178.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 106.3615 0.0000 -90.0000 160
#__ type_ start__ end____ width___ exp.time_
18 omega -114.00 -13.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 -57.0000 90.0000 101
#__ type_ start__ end____ width___ exp.time_
19 omega -114.00 -13.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 -57.0000 0.0000 101
#__ type_ start__ end____ width___ exp.time_
20 omega 8.00 98.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 41.0749 77.0000 -60.0000 90
;
_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 0.0022996000
_diffrn_orient_matrix_UB_12 0.0984820000
_diffrn_orient_matrix_UB_13 0.1202557000
_diffrn_orient_matrix_UB_21 -0.1151581000
_diffrn_orient_matrix_UB_22 -0.1013455000
_diffrn_orient_matrix_UB_23 0.0041326000
_diffrn_orient_matrix_UB_31 0.0968272000
_diffrn_orient_matrix_UB_32 -0.0347120000
_diffrn_orient_matrix_UB_33 0.0659716000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.710
_diffrn_source 'sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5636
_reflns_number_total 5966
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max 0.734
_refine_diff_density_min -0.683
_refine_diff_density_rms 0.066
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.092
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 448
_refine_ls_number_reflns 5966
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0298
_refine_ls_R_factor_gt 0.0277
_refine_ls_restrained_S_all 1.092
_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^)+(0.0400P)^2^+0.7360P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0737
_refine_ls_wR_factor_ref 0.0753
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Others
Fixed Sof: N6(0.5) H6A(0.5) H6B(0.5) N5(0.5) H5A(0.5) H5B(0.5)
3.a Rotating group:
N6(H6A,H6B), N5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
C1(H1), C7(H7), C16(H16), C20(H20), C32(H32), C28(H28)
3.c Idealised Me refined as rotating group:
C25(H25A,H25B,H25C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C)
;
_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
Cd1 Cd 0.16473(2) 0.21420(2) 0.18918(2) 0.02819(6) Uani 1 1 d . . . . .
O2 O 0.0525(2) 0.23660(18) 0.03135(16) 0.0461(4) Uani 1 1 d . . . . .
O3 O 0.3518(2) 0.2243(2) 0.13232(19) 0.0503(5) Uani 1 1 d . . . . .
O4 O 0.2161(2) 0.0400(2) 0.1005(2) 0.0597(6) Uani 1 1 d . . . . .
N1 N 0.2576(2) 0.3398(2) 0.39214(18) 0.0394(5) Uani 1 1 d . . . . .
O6 O 0.5395(2) 0.3730(2) 0.65711(16) 0.0497(5) Uani 1 1 d . . . . .
O1 O 0.1454(2) 0.4021(2) 0.20589(17) 0.0551(5) Uani 1 1 d . . . . .
N3 N -0.0109(2) 0.0952(2) 0.2161(2) 0.0427(5) Uani 1 1 d . . . . .
N2 N 0.3053(2) 0.4666(2) 0.43207(18) 0.0372(5) Uani 1 1 d . . . . .
O7 O -0.0999(2) 0.1242(3) 0.5335(2) 0.0690(7) Uani 1 1 d . . . . .
O5 O 0.2472(2) 0.5487(2) 0.76198(17) 0.0529(5) Uani 1 1 d . . . . .
N7 N 0.3923(2) 0.4603(2) 0.70853(17) 0.0364(4) Uani 1 1 d . . . . .
O8 O -0.4176(3) -0.0990(3) 0.1763(2) 0.0876(9) Uani 1 1 d . . . . .
N4 N -0.0462(2) -0.0309(2) 0.1758(2) 0.0467(5) Uani 1 1 d . . . . .
C18 C 0.4790(2) 0.4935(2) 0.94193(19) 0.0312(5) Uani 1 1 d . . . . .
C12 C 0.2812(3) 0.3223(3) 0.4885(2) 0.0405(6) Uani 1 1 d . . . . .
N8 N -0.2580(2) 0.0185(3) 0.3542(2) 0.0506(6) Uani 1 1 d . . . . .
C22 C -0.0817(3) 0.1296(3) 0.2876(3) 0.0473(6) Uani 1 1 d . . . . .
C17 C 0.3791(2) 0.5330(2) 0.9134(2) 0.0334(5) Uani 1 1 d . . . . .
C3 C 0.0370(2) 0.4286(2) 0.0497(2) 0.0383(5) Uani 1 1 d . . . . .
C10 C 0.3608(3) 0.5309(3) 0.5503(2) 0.0371(5) Uani 1 1 d . . . . .
C1 C 0.0120(3) 0.6198(3) 0.0727(2) 0.0432(6) Uani 1 1 d . . . . .
H1 H 0.0209 0.7014 0.1217 0.052 Uiso 1 1 calc R . . . .
C4 C 0.0804(3) 0.3504(3) 0.0981(2) 0.0380(5) Uani 1 1 d . . . . .
C29 C -0.3187(3) 0.0586(3) 0.5389(3) 0.0448(6) Uani 1 1 d . . . . .
C5 C 0.3214(3) 0.1079(3) 0.0958(2) 0.0415(6) Uani 1 1 d . . . . .
C8 C 0.6284(3) 0.0816(3) 0.0202(2) 0.0427(6) Uani 1 1 d . . . . .
C7 C 0.5383(3) 0.1275(3) 0.0649(2) 0.0435(6) Uani 1 1 d . . . . .
H7 H 0.5641 0.2142 0.1092 0.052 Uiso 1 1 calc R . . . .
C24 C -0.1400(3) -0.0772(3) 0.2194(3) 0.0529(7) Uani 1 1 d . . . . .
C6 C 0.4124(3) 0.0495(3) 0.0462(2) 0.0398(5) Uani 1 1 d . . . . .
C19 C 0.5376(2) 0.4393(2) 0.8568(2) 0.0338(5) Uani 1 1 d . . . . .
C14 C 0.3327(2) 0.5168(2) 0.7917(2) 0.0367(5) Uani 1 1 d . . . . .
C16 C 0.3226(3) 0.5842(3) 0.9980(2) 0.0414(6) Uani 1 1 d . . . . .
H16 H 0.2562 0.6096 0.9787 0.050 Uiso 1 1 calc R . . . .
C11 C 0.3467(3) 0.4400(3) 0.5888(2) 0.0369(5) Uani 1 1 d . . . . .
C2 C 0.0484(3) 0.5501(3) 0.1248(2) 0.0435(6) Uani 1 1 d . . . . .
C30 C -0.4515(3) 0.0045(3) 0.4705(2) 0.0410(6) Uani 1 1 d . . . . .
C15 C 0.4937(2) 0.4213(2) 0.7340(2) 0.0365(5) Uani 1 1 d . . . . .
C20 C 0.6354(3) 0.4018(3) 0.8862(2) 0.0411(6) Uani 1 1 d . . . . .
H20 H 0.6740 0.3669 0.8293 0.049 Uiso 1 1 calc R . . . .
C23 C -0.1622(3) 0.0234(3) 0.2921(3) 0.0483(6) Uani 1 1 d . . . . .
C25 C -0.2004(5) -0.2141(4) 0.1864(5) 0.0941(16) Uani 1 1 d . . . . .
H25A H -0.1757 -0.2617 0.1202 0.141 Uiso 1 1 calc GR . . . .
H25B H -0.2937 -0.2416 0.1647 0.141 Uiso 1 1 calc GR . . . .
H25C H -0.1706 -0.2274 0.2531 0.141 Uiso 1 1 calc GR . . . .
C26 C -0.2153(3) 0.0711(3) 0.4782(3) 0.0487(7) Uani 1 1 d . . . . .
C31 C -0.4899(3) -0.0420(3) 0.3465(3) 0.0475(6) Uani 1 1 d . . . . .
C9 C 0.4184(3) 0.6706(3) 0.6132(3) 0.0506(7) Uani 1 1 d . . . . .
H9A H 0.4495 0.7024 0.5608 0.076 Uiso 1 1 calc GR . . . .
H9B H 0.4898 0.6990 0.6820 0.076 Uiso 1 1 calc GR . . . .
H9C H 0.3532 0.7010 0.6378 0.076 Uiso 1 1 calc GR . . . .
C13 C 0.2399(4) 0.1936(3) 0.4797(3) 0.0667(10) Uani 1 1 d . . . . .
H13A H 0.1731 0.1813 0.5178 0.100 Uiso 1 1 calc GR . . . .
H13B H 0.3136 0.1843 0.5183 0.100 Uiso 1 1 calc GR . . . .
H13C H 0.2064 0.1319 0.3974 0.100 Uiso 1 1 calc GR . . . .
C32 C -0.6192(3) -0.0908(3) 0.2822(3) 0.0547(7) Uani 1 1 d . . . . .
H32 H -0.6431 -0.1185 0.2004 0.066 Uiso 1 1 calc R . . . .
C21 C -0.0718(4) 0.2623(3) 0.3480(4) 0.0739(11) Uani 1 1 d . . . . .
H21A H -0.0078 0.3061 0.4250 0.111 Uiso 1 1 calc GR . . . .
H21B H -0.1551 0.2622 0.3572 0.111 Uiso 1 1 calc GR . . . .
H21C H -0.0462 0.3040 0.3008 0.111 Uiso 1 1 calc GR . . . .
C28 C -0.2850(3) 0.0984(3) 0.6584(3) 0.0524(7) Uani 1 1 d . . . . .
H28 H -0.1974 0.1310 0.7016 0.063 Uiso 1 1 calc R . . . .
C27 C -0.3900(3) -0.0438(3) 0.2829(3) 0.0555(8) Uani 1 1 d . . . . .
N6 N 0.0907(6) 0.6068(5) 0.2509(4) 0.0566(13) Uani 0.5 1 d . . P . .
H6A H 0.0520 0.6568 0.2794 0.068 Uiso 0.5 1 d GR . P . .
H6B H 0.0716 0.5487 0.2736 0.068 Uiso 0.5 1 d GR . P . .
N5 N 0.7482(5) 0.1691(5) 0.0419(5) 0.0533(12) Uani 0.5 1 d . . P . .
H5A H 0.8019 0.1322 0.0278 0.064 Uiso 0.5 1 d GR . P . .
H5B H 0.7419 0.2037 -0.0042 0.064 Uiso 0.5 1 d GR . P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.03264(10) 0.03330(10) 0.02509(9) 0.01540(7) 0.01177(7) 0.01695(7)
O2 0.0614(12) 0.0427(10) 0.0380(9) 0.0196(8) 0.0083(9) 0.0270(9)
O3 0.0532(12) 0.0482(11) 0.0548(12) 0.0188(9) 0.0249(10) 0.0291(10)
O4 0.0538(12) 0.0536(12) 0.0798(16) 0.0258(11) 0.0412(12) 0.0277(10)
N1 0.0519(13) 0.0408(11) 0.0255(10) 0.0166(9) 0.0079(9) 0.0177(10)
O6 0.0584(12) 0.0724(14) 0.0307(9) 0.0265(9) 0.0205(9) 0.0342(11)
O1 0.0755(14) 0.0498(11) 0.0370(10) 0.0191(9) -0.0030(10) 0.0310(11)
N3 0.0416(12) 0.0434(12) 0.0499(13) 0.0237(10) 0.0247(10) 0.0167(10)
N2 0.0467(12) 0.0388(11) 0.0272(10) 0.0176(9) 0.0097(9) 0.0154(9)
O7 0.0401(11) 0.0909(18) 0.0605(14) 0.0261(13) 0.0201(10) 0.0145(11)
O5 0.0593(12) 0.0777(15) 0.0365(10) 0.0305(10) 0.0130(9) 0.0407(11)
N7 0.0434(11) 0.0458(12) 0.0239(9) 0.0197(9) 0.0087(8) 0.0179(9)
O8 0.0623(15) 0.150(3) 0.0443(13) 0.0398(16) 0.0266(12) 0.0343(17)
N4 0.0502(13) 0.0409(12) 0.0474(13) 0.0178(10) 0.0254(11) 0.0139(10)
C18 0.0313(11) 0.0341(12) 0.0255(11) 0.0155(9) 0.0068(9) 0.0074(9)
C12 0.0513(15) 0.0422(14) 0.0309(12) 0.0203(11) 0.0099(11) 0.0185(12)
N8 0.0447(13) 0.0591(15) 0.0497(14) 0.0248(12) 0.0260(11) 0.0171(11)
C22 0.0463(15) 0.0505(16) 0.0521(16) 0.0237(13) 0.0260(13) 0.0221(13)
C17 0.0347(12) 0.0392(12) 0.0268(11) 0.0174(10) 0.0087(9) 0.0120(10)
C3 0.0397(13) 0.0394(13) 0.0367(13) 0.0200(11) 0.0047(10) 0.0165(11)
C10 0.0413(13) 0.0458(14) 0.0283(11) 0.0195(10) 0.0118(10) 0.0183(11)
C1 0.0503(15) 0.0392(13) 0.0375(13) 0.0168(11) 0.0038(12) 0.0197(12)
C4 0.0421(13) 0.0431(14) 0.0359(12) 0.0226(11) 0.0113(11) 0.0198(11)
C29 0.0393(13) 0.0479(15) 0.0467(15) 0.0204(12) 0.0190(12) 0.0151(12)
C5 0.0441(14) 0.0527(16) 0.0315(12) 0.0157(11) 0.0146(11) 0.0269(12)
C8 0.0398(13) 0.0469(15) 0.0406(14) 0.0165(12) 0.0163(11) 0.0187(11)
C7 0.0456(14) 0.0409(13) 0.0410(14) 0.0122(11) 0.0170(12) 0.0198(12)
C24 0.0571(17) 0.0459(16) 0.0558(17) 0.0223(14) 0.0311(15) 0.0145(13)
C6 0.0420(13) 0.0476(15) 0.0337(12) 0.0165(11) 0.0159(11) 0.0231(11)
C19 0.0345(12) 0.0410(13) 0.0256(11) 0.0178(10) 0.0084(9) 0.0112(10)
C14 0.0407(13) 0.0429(13) 0.0282(11) 0.0183(10) 0.0098(10) 0.0161(11)
C16 0.0421(14) 0.0546(16) 0.0339(13) 0.0224(12) 0.0109(11) 0.0244(12)
C11 0.0438(13) 0.0459(14) 0.0238(11) 0.0185(10) 0.0091(10) 0.0181(11)
C2 0.0478(15) 0.0451(14) 0.0350(12) 0.0191(11) 0.0017(11) 0.0188(12)
C30 0.0427(14) 0.0447(14) 0.0410(14) 0.0222(12) 0.0188(12) 0.0176(11)
C15 0.0384(12) 0.0452(14) 0.0269(11) 0.0192(10) 0.0106(10) 0.0136(11)
C20 0.0431(14) 0.0559(16) 0.0309(12) 0.0209(11) 0.0160(11) 0.0241(12)
C23 0.0476(15) 0.0531(16) 0.0498(16) 0.0251(13) 0.0270(13) 0.0188(13)
C25 0.110(3) 0.048(2) 0.127(4) 0.035(2) 0.083(3) 0.018(2)
C26 0.0433(15) 0.0523(16) 0.0480(15) 0.0204(13) 0.0202(13) 0.0158(13)
C31 0.0467(15) 0.0557(17) 0.0412(14) 0.0227(13) 0.0194(12) 0.0175(13)
C9 0.0640(18) 0.0432(15) 0.0387(14) 0.0163(12) 0.0136(13) 0.0173(14)
C13 0.100(3) 0.0440(17) 0.0458(16) 0.0256(14) 0.0003(17) 0.0176(17)
C32 0.0478(16) 0.074(2) 0.0399(15) 0.0238(14) 0.0155(13) 0.0222(15)
C21 0.082(2) 0.057(2) 0.104(3) 0.038(2) 0.061(2) 0.0378(19)
C28 0.0417(15) 0.0651(19) 0.0432(15) 0.0188(14) 0.0143(12) 0.0189(14)
C27 0.0513(17) 0.080(2) 0.0413(15) 0.0315(15) 0.0223(13) 0.0237(16)
N6 0.083(4) 0.050(3) 0.039(3) 0.021(2) 0.006(3) 0.034(3)
N5 0.048(3) 0.051(3) 0.066(3) 0.023(2) 0.027(2) 0.027(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O2 2.3711(17) . ?
Cd1 O3 2.308(2) . ?
Cd1 O4 2.317(2) . ?
Cd1 N1 2.310(2) . ?
Cd1 O1 2.349(2) . ?
Cd1 N3 2.252(2) . ?
Cd1 C4 2.701(2) . ?
Cd1 C5 2.660(3) . ?
O2 C4 1.247(3) . ?
O3 C5 1.255(3) . ?
O4 C5 1.259(3) . ?
N1 N2 1.356(3) . ?
N1 C12 1.333(3) . ?
O6 C15 1.211(3) . ?
O1 C4 1.255(3) . ?
N3 N4 1.355(3) . ?
N3 C22 1.329(3) . ?
N2 C10 1.340(3) . ?
O7 C26 1.214(4) . ?
O5 C14 1.209(3) . ?
N7 C14 1.409(3) . ?
N7 C11 1.433(3) . ?
N7 C15 1.410(3) . ?
O8 C27 1.201(4) . ?
N4 C24 1.347(4) . ?
C18 C18 1.416(4) 2_667 ?
C18 C17 1.409(3) . ?
C18 C19 1.407(3) . ?
C12 C11 1.399(4) . ?
C12 C13 1.485(4) . ?
N8 C23 1.429(3) . ?
N8 C26 1.397(4) . ?
N8 C27 1.413(4) . ?
C22 C23 1.392(4) . ?
C22 C21 1.490(5) . ?
C17 C14 1.477(3) . ?
C17 C16 1.374(4) . ?
C3 C1 1.388(4) 2_565 ?
C3 C4 1.495(3) . ?
C3 C2 1.397(4) . ?
C10 C11 1.377(3) . ?
C10 C9 1.480(4) . ?
C1 C3 1.388(4) 2_565 ?
C1 C2 1.394(4) . ?
C29 C30 1.416(4) . ?
C29 C26 1.492(4) . ?
C29 C28 1.360(4) . ?
C5 C6 1.501(4) . ?
C8 C7 1.394(4) . ?
C8 C6 1.402(4) 2_655 ?
C8 N5 1.365(6) . ?
C7 C6 1.380(4) . ?
C24 C23 1.361(4) . ?
C24 C25 1.491(5) . ?
C6 C8 1.402(4) 2_655 ?
C19 C15 1.477(3) . ?
C19 C20 1.374(4) . ?
C16 C20 1.408(3) 2_667 ?
C2 N6 1.417(5) . ?
C30 C30 1.416(5) 2_456 ?
C30 C31 1.401(4) . ?
C20 C16 1.408(3) 2_667 ?
C31 C32 1.374(4) . ?
C31 C27 1.481(4) . ?
C32 C28 1.407(4) 2_456 ?
C28 C32 1.407(4) 2_456 ?
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
O2 Cd1 C4 27.49(7) . . ?
O2 Cd1 C5 103.19(7) . . ?
O3 Cd1 O2 96.43(7) . . ?
O3 Cd1 O4 56.39(7) . . ?
O3 Cd1 N1 99.60(8) . . ?
O3 Cd1 O1 102.98(8) . . ?
O3 Cd1 C4 100.81(8) . . ?
O3 Cd1 C5 28.15(8) . . ?
O4 Cd1 O2 106.21(8) . . ?
O4 Cd1 O1 153.01(8) . . ?
O4 Cd1 C4 131.17(8) . . ?
O4 Cd1 C5 28.25(8) . . ?
N1 Cd1 O2 134.79(7) . . ?
N1 Cd1 O4 117.90(8) . . ?
N1 Cd1 O1 80.05(7) . . ?
N1 Cd1 C4 107.56(8) . . ?
N1 Cd1 C5 110.73(8) . . ?
O1 Cd1 O2 55.16(6) . . ?
O1 Cd1 C4 27.67(7) . . ?
O1 Cd1 C5 129.38(9) . . ?
N3 Cd1 O2 97.86(8) . . ?
N3 Cd1 O3 146.58(8) . . ?
N3 Cd1 O4 90.56(8) . . ?
N3 Cd1 N1 91.40(8) . . ?
N3 Cd1 O1 109.99(9) . . ?
N3 Cd1 C4 105.77(8) . . ?
N3 Cd1 C5 118.64(9) . . ?
C5 Cd1 C4 118.97(8) . . ?
C4 O2 Cd1 91.15(15) . . ?
C5 O3 Cd1 91.67(17) . . ?
C5 O4 Cd1 91.19(17) . . ?
N2 N1 Cd1 117.24(14) . . ?
C12 N1 Cd1 136.83(18) . . ?
C12 N1 N2 105.9(2) . . ?
C4 O1 Cd1 91.99(16) . . ?
N4 N3 Cd1 122.14(17) . . ?
C22 N3 Cd1 130.0(2) . . ?
C22 N3 N4 106.6(2) . . ?
C10 N2 N1 112.60(19) . . ?
C14 N7 C11 118.1(2) . . ?
C14 N7 C15 124.81(19) . . ?
C15 N7 C11 117.1(2) . . ?
C24 N4 N3 111.0(2) . . ?
C17 C18 C18 119.8(3) . 2_667 ?
C19 C18 C18 118.8(3) . 2_667 ?
C19 C18 C17 121.4(2) . . ?
N1 C12 C11 108.9(2) . . ?
N1 C12 C13 121.4(2) . . ?
C11 C12 C13 129.7(2) . . ?
C26 N8 C23 118.4(2) . . ?
C26 N8 C27 125.3(2) . . ?
C27 N8 C23 116.3(2) . . ?
N3 C22 C23 108.8(3) . . ?
N3 C22 C21 122.5(3) . . ?
C23 C22 C21 128.7(3) . . ?
C18 C17 C14 120.1(2) . . ?
C16 C17 C18 120.1(2) . . ?
C16 C17 C14 119.8(2) . . ?
C1 C3 C4 118.9(2) 2_565 . ?
C1 C3 C2 119.7(2) 2_565 . ?
C2 C3 C4 121.4(2) . . ?
N2 C10 C11 105.2(2) . . ?
N2 C10 C9 121.8(2) . . ?
C11 C10 C9 133.0(2) . . ?
C3 C1 C2 122.2(3) 2_565 . ?
O2 C4 Cd1 61.35(13) . . ?
O2 C4 O1 121.7(2) . . ?
O2 C4 C3 119.8(2) . . ?
O1 C4 Cd1 60.34(13) . . ?
O1 C4 C3 118.5(2) . . ?
C3 C4 Cd1 178.50(19) . . ?
C30 C29 C26 119.2(2) . . ?
C28 C29 C30 120.7(3) . . ?
C28 C29 C26 120.1(3) . . ?
O3 C5 Cd1 60.18(14) . . ?
O3 C5 O4 120.7(3) . . ?
O3 C5 C6 119.3(3) . . ?
O4 C5 Cd1 60.57(14) . . ?
O4 C5 C6 119.9(3) . . ?
C6 C5 Cd1 178.49(18) . . ?
C7 C8 C6 117.7(3) . 2_655 ?
N5 C8 C7 116.8(3) . . ?
N5 C8 C6 125.4(3) . 2_655 ?
C6 C7 C8 122.7(3) . . ?
N4 C24 C23 106.1(3) . . ?
N4 C24 C25 122.5(3) . . ?
C23 C24 C25 131.4(3) . . ?
C8 C6 C5 121.6(2) 2_655 . ?
C7 C6 C5 118.9(3) . . ?
C7 C6 C8 119.5(3) . 2_655 ?
C18 C19 C15 120.2(2) . . ?
C20 C19 C18 120.7(2) . . ?
C20 C19 C15 119.2(2) . . ?
O5 C14 N7 120.1(2) . . ?
O5 C14 C17 123.1(2) . . ?
N7 C14 C17 116.8(2) . . ?
C17 C16 C20 120.3(2) . 2_667 ?
C12 C11 N7 125.6(2) . . ?
C10 C11 N7 127.0(2) . . ?
C10 C11 C12 107.4(2) . . ?
C3 C2 N6 124.7(3) . . ?
C1 C2 C3 118.1(2) . . ?
C1 C2 N6 117.2(3) . . ?
C30 C30 C29 118.7(3) 2_456 . ?
C31 C30 C29 122.2(2) . . ?
C31 C30 C30 119.2(3) . 2_456 ?
O6 C15 N7 120.7(2) . . ?
O6 C15 C19 122.5(2) . . ?
N7 C15 C19 116.7(2) . . ?
C19 C20 C16 120.3(2) . 2_667 ?
C22 C23 N8 126.5(3) . . ?
C24 C23 N8 125.9(3) . . ?
C24 C23 C22 107.4(2) . . ?
O7 C26 N8 121.5(3) . . ?
O7 C26 C29 121.9(3) . . ?
N8 C26 C29 116.6(2) . . ?
C30 C31 C27 119.5(3) . . ?
C32 C31 C30 121.2(3) . . ?
C32 C31 C27 119.3(3) . . ?
C31 C32 C28 119.3(3) . 2_456 ?
C29 C28 C32 120.9(3) . 2_456 ?
O8 C27 N8 120.6(3) . . ?
O8 C27 C31 122.7(3) . . ?
N8 C27 C31 116.7(3) . . ?
_shelx_res_file
;
TITL
CELL 0.71 11.241931 12.471994 12.765812 112.8103 98.5236 107.3333
ZERR 2 0.000373 0.000414 0.000417 0.0031 0.0027 0.0029
LATT 1
SFAC C H Cd N O
UNIT 64 40 2 14 16
L.S. 20 0 0
PLAN 20
fmap 2 53
acta
REM
REM
REM
WGHT 0.040000 0.736000
FVAR 5.83293
CD1 3 0.164734 0.214199 0.189179 11.00000 0.03264 0.03330 =
0.02509 0.01540 0.01177 0.01695
O2 5 0.052512 0.236605 0.031353 11.00000 0.06142 0.04268 =
0.03795 0.01956 0.00831 0.02700
O3 5 0.351763 0.224303 0.132323 11.00000 0.05323 0.04823 =
0.05479 0.01883 0.02489 0.02912
O4 5 0.216127 0.040048 0.100531 11.00000 0.05379 0.05364 =
0.07977 0.02579 0.04125 0.02767
N1 4 0.257606 0.339827 0.392143 11.00000 0.05190 0.04079 =
0.02551 0.01660 0.00792 0.01772
O6 5 0.539473 0.372969 0.657115 11.00000 0.05837 0.07243 =
0.03075 0.02650 0.02052 0.03421
O1 5 0.145365 0.402128 0.205889 11.00000 0.07555 0.04976 =
0.03699 0.01912 -0.00304 0.03101
N3 4 -0.010929 0.095212 0.216071 11.00000 0.04160 0.04345 =
0.04988 0.02375 0.02472 0.01674
N2 4 0.305293 0.466648 0.432070 11.00000 0.04674 0.03880 =
0.02717 0.01761 0.00968 0.01537
O7 5 -0.099934 0.124154 0.533520 11.00000 0.04011 0.09093 =
0.06050 0.02615 0.02012 0.01447
O5 5 0.247177 0.548658 0.761975 11.00000 0.05931 0.07770 =
0.03651 0.03054 0.01300 0.04067
N7 4 0.392265 0.460347 0.708528 11.00000 0.04339 0.04580 =
0.02394 0.01975 0.00874 0.01788
O8 5 -0.417586 -0.098987 0.176326 11.00000 0.06230 0.14979 =
0.04435 0.03980 0.02655 0.03432
N4 4 -0.046211 -0.030902 0.175789 11.00000 0.05016 0.04091 =
0.04739 0.01777 0.02537 0.01386
C18 1 0.479030 0.493459 0.941934 11.00000 0.03134 0.03405 =
0.02549 0.01548 0.00682 0.00745
C12 1 0.281175 0.322283 0.488494 11.00000 0.05131 0.04223 =
0.03087 0.02026 0.00991 0.01846
N8 4 -0.258046 0.018495 0.354165 11.00000 0.04473 0.05914 =
0.04967 0.02481 0.02605 0.01706
C22 1 -0.081715 0.129598 0.287616 11.00000 0.04630 0.05050 =
0.05206 0.02365 0.02596 0.02211
C17 1 0.379090 0.532993 0.913448 11.00000 0.03465 0.03916 =
0.02679 0.01736 0.00873 0.01197
C3 1 0.036976 0.428599 0.049718 11.00000 0.03967 0.03945 =
0.03667 0.01998 0.00466 0.01649
C10 1 0.360815 0.530876 0.550307 11.00000 0.04126 0.04582 =
0.02833 0.01953 0.01183 0.01825
C1 1 0.012018 0.619764 0.072714 11.00000 0.05034 0.03918 =
0.03751 0.01678 0.00377 0.01973
AFIX 43
H1 2 0.020881 0.701402 0.121668 11.00000 -1.20000
AFIX 0
C4 1 0.080375 0.350354 0.098131 11.00000 0.04210 0.04311 =
0.03593 0.02264 0.01133 0.01983
C29 1 -0.318668 0.058612 0.538897 11.00000 0.03934 0.04791 =
0.04666 0.02036 0.01904 0.01505
C5 1 0.321442 0.107851 0.095751 11.00000 0.04409 0.05273 =
0.03146 0.01572 0.01455 0.02692
C8 1 0.628350 0.081590 0.020164 11.00000 0.03983 0.04695 =
0.04061 0.01648 0.01627 0.01868
C7 1 0.538278 0.127462 0.064911 11.00000 0.04563 0.04089 =
0.04101 0.01222 0.01700 0.01977
AFIX 43
H7 2 0.564065 0.214230 0.109209 11.00000 -1.20000
AFIX 0
C24 1 -0.139992 -0.077207 0.219360 11.00000 0.05712 0.04585 =
0.05581 0.02227 0.03113 0.01453
C6 1 0.412412 0.049511 0.046237 11.00000 0.04198 0.04757 =
0.03368 0.01652 0.01590 0.02311
C19 1 0.537624 0.439329 0.856802 11.00000 0.03450 0.04104 =
0.02558 0.01785 0.00838 0.01120
C14 1 0.332667 0.516829 0.791716 11.00000 0.04068 0.04290 =
0.02822 0.01830 0.00977 0.01607
C16 1 0.322559 0.584152 0.998002 11.00000 0.04210 0.05455 =
0.03386 0.02242 0.01094 0.02441
AFIX 43
H16 2 0.256229 0.609599 0.978662 11.00000 -1.20000
AFIX 0
C11 1 0.346701 0.440021 0.588762 11.00000 0.04380 0.04589 =
0.02376 0.01850 0.00913 0.01812
C2 1 0.048401 0.550079 0.124803 11.00000 0.04778 0.04510 =
0.03504 0.01909 0.00173 0.01883
C30 1 -0.451528 0.004468 0.470488 11.00000 0.04272 0.04469 =
0.04102 0.02216 0.01878 0.01759
C15 1 0.493741 0.421281 0.734007 11.00000 0.03843 0.04522 =
0.02688 0.01916 0.01058 0.01363
C20 1 0.635397 0.401777 0.886197 11.00000 0.04313 0.05590 =
0.03094 0.02089 0.01599 0.02411
AFIX 43
H20 2 0.673958 0.366914 0.829327 11.00000 -1.20000
AFIX 0
C23 1 -0.162221 0.023397 0.292094 11.00000 0.04761 0.05306 =
0.04977 0.02509 0.02696 0.01881
C25 1 -0.200369 -0.214147 0.186417 11.00000 0.10957 0.04788 =
0.12718 0.03520 0.08275 0.01763
AFIX 137
H25A 2 -0.175669 -0.261682 0.120238 11.00000 -1.50000
H25B 2 -0.293723 -0.241560 0.164689 11.00000 -1.50000
H25C 2 -0.170598 -0.227387 0.253109 11.00000 -1.50000
AFIX 0
C26 1 -0.215345 0.071059 0.478235 11.00000 0.04330 0.05225 =
0.04802 0.02038 0.02023 0.01585
C31 1 -0.489873 -0.042011 0.346545 11.00000 0.04671 0.05567 =
0.04119 0.02270 0.01940 0.01751
C9 1 0.418392 0.670595 0.613241 11.00000 0.06401 0.04315 =
0.03870 0.01635 0.01359 0.01734
AFIX 137
H9A 2 0.449511 0.702433 0.560773 11.00000 -1.50000
H9B 2 0.489848 0.698970 0.681992 11.00000 -1.50000
H9C 2 0.353175 0.701035 0.637793 11.00000 -1.50000
AFIX 0
C13 1 0.239914 0.193586 0.479700 11.00000 0.09964 0.04402 =
0.04581 0.02556 0.00028 0.01763
AFIX 137
H13A 2 0.173071 0.181350 0.517771 11.00000 -1.50000
H13B 2 0.313557 0.184320 0.518282 11.00000 -1.50000
H13C 2 0.206442 0.131893 0.397363 11.00000 -1.50000
AFIX 0
C32 1 -0.619178 -0.090802 0.282243 11.00000 0.04775 0.07381 =
0.03991 0.02380 0.01550 0.02222
AFIX 43
H32 2 -0.643077 -0.118515 0.200390 11.00000 -1.20000
AFIX 0
C21 1 -0.071808 0.262257 0.348018 11.00000 0.08219 0.05731 =
0.10381 0.03795 0.06123 0.03780
AFIX 137
H21A 2 -0.007811 0.306053 0.424990 11.00000 -1.50000
H21B 2 -0.155053 0.262230 0.357156 11.00000 -1.50000
H21C 2 -0.046177 0.303961 0.300827 11.00000 -1.50000
AFIX 0
C28 1 -0.284999 0.098375 0.658441 11.00000 0.04174 0.06510 =
0.04322 0.01876 0.01434 0.01887
AFIX 43
H28 2 -0.197429 0.131028 0.701599 11.00000 -1.20000
AFIX 0
C27 1 -0.390018 -0.043835 0.282900 11.00000 0.05129 0.07956 =
0.04135 0.03149 0.02231 0.02372
N6 4 0.090703 0.606791 0.250936 10.50000 0.08306 0.05043 =
0.03915 0.02143 0.00599 0.03417
AFIX 7
H6A 2 0.051963 0.656781 0.279446 10.50000 -1.20000
H6B 2 0.071584 0.548681 0.273616 10.50000 -1.20000
AFIX 0
N5 4 0.748237 0.169090 0.041921 10.50000 0.04841 0.05097 =
0.06623 0.02343 0.02740 0.02657
AFIX 7
H5A 2 0.801917 0.132220 0.027781 10.50000 -1.20000
H5B 2 0.741857 0.203650 -0.004249 10.50000 -1.20000
AFIX 0
HKLF 4
REM
REM R1 = 0.0277 for 5636 Fo > 4sig(Fo) and 0.0298 for all 5966 data
REM 448 parameters refined using 0 restraints
END
WGHT 0.0384 0.7810
REM Highest difference peak 0.734, deepest hole -0.683, 1-sigma level 0.066
Q1 1 0.2999 0.4972 0.3818 11.00000 0.05 0.73
Q2 1 -0.0162 -0.0796 0.1139 11.00000 0.05 0.56
Q3 1 0.4972 0.6433 0.5630 11.00000 0.05 0.35
Q4 1 0.7718 0.2576 0.1039 11.00000 0.05 0.32
Q5 1 -0.2624 -0.2220 0.2406 11.00000 0.05 0.32
Q6 1 -0.3808 0.0062 0.2104 11.00000 0.05 0.28
Q7 1 0.5180 0.4345 0.8068 11.00000 0.05 0.25
Q8 1 0.5000 0.5000 1.0000 10.50000 0.05 0.25
Q9 1 0.0998 0.2039 0.2147 11.00000 0.05 0.25
Q10 1 0.1935 0.3471 0.2011 11.00000 0.05 0.24
Q11 1 0.2629 0.2014 0.5555 11.00000 0.05 0.24
Q12 1 0.1144 0.0452 0.0729 11.00000 0.05 0.24
Q13 1 0.1036 0.7398 0.1252 11.00000 0.05 0.23
Q14 1 0.3704 0.4621 0.6446 11.00000 0.05 0.23
Q15 1 0.1606 0.1789 0.0452 11.00000 0.05 0.23
Q16 1 0.7665 0.1544 0.1011 11.00000 0.05 0.23
Q17 1 -0.0331 0.7168 0.1662 11.00000 0.05 0.22
Q18 1 0.1712 0.1038 0.1760 11.00000 0.05 0.22
Q19 1 0.0346 0.1105 0.1816 11.00000 0.05 0.22
Q20 1 0.1253 0.3594 0.2623 11.00000 0.05 0.21
;
_shelx_res_checksum 31542
_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_FJU-69
_database_code_depnum_ccdc_archive 'CCDC 1851267'
_audit_update_record
;
2018-06-24 deposited with the CCDC.
2018-10-30 downloaded from the CCDC.
;
_audit_creation_date 2018-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelxl_version_number 2013-2
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C36 H24 Cd N6 O8, H2 O'
_chemical_formula_sum 'C36 H26 Cd N6 O9'
_chemical_formula_weight 799.03
_chemical_absolute_configuration ?
_chemical_melting_point ?
_chemical_oxdiff_formula 'C1 H1 O1 N1 Cd1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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 7
_space_group_name_H-M_alt 'P 1 n 1'
_space_group_name_Hall 'P -2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z+1/2'
_cell_length_a 8.9688(2)
_cell_length_b 13.3571(3)
_cell_length_c 13.4352(3)
_cell_angle_alpha 90
_cell_angle_beta 102.071(2)
_cell_angle_gamma 90
_cell_volume 1573.91(6)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 5262
_cell_measurement_temperature 296.61(10)
_cell_measurement_theta_max 73.6660
_cell_measurement_theta_min 4.6890
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 6.166
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.56926
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.686
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description pale
_exptl_crystal_F_000 808
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0244
_diffrn_reflns_av_unetI/netI 0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 9067
_diffrn_reflns_point_group_measured_fraction_full 0.695
_diffrn_reflns_point_group_measured_fraction_max 0.667
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 74.107
_diffrn_reflns_theta_min 3.309
_diffrn_ambient_environment air
_diffrn_ambient_temperature 296.61(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.5148
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -50.00 33.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 38.0000 0.0000 83
#__ type_ start__ end____ width___ exp.time_
2 omega -50.00 33.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 38.0000 150.0000 83
#__ type_ start__ end____ width___ exp.time_
3 omega -74.00 35.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 77.0000 -120.0000 109
#__ type_ start__ end____ width___ exp.time_
4 omega 23.00 97.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 41.0749 -125.0000 30.0000 74
#__ type_ start__ end____ width___ exp.time_
5 omega 94.00 178.00 1.0000 1.2000
omega____ theta____ kappa____ phi______ frames
- 106.3615 125.0000 30.0000 84
#__ type_ start__ end____ width___ exp.time_
6 omega 24.00 109.00 1.0000 1.2000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -94.0000 0.0000 85
#__ type_ start__ end____ width___ exp.time_
7 omega 33.00 121.00 1.0000 1.2000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -125.0000 -180.0000 88
#__ type_ start__ end____ width___ exp.time_
8 omega 30.00 91.00 1.0000 1.2000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -30.0000 60.0000 61
#__ type_ start__ end____ width___ exp.time_
9 omega 30.00 91.00 1.0000 1.2000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -30.0000 -120.0000 61
#__ type_ start__ end____ width___ exp.time_
10 omega 77.00 178.00 1.0000 1.2000
omega____ theta____ kappa____ phi______ frames
- 106.3615 61.0000 30.0000 101
#__ type_ start__ end____ width___ exp.time_
11 omega 30.00 91.00 1.0000 1.2000
omega____ theta____ kappa____ phi______ frames
- 106.3615 -30.0000 0.0000 61
#__ type_ start__ end____ width___ exp.time_
12 omega -114.00 -13.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -41.0749 -57.0000 -150.0000 101
;
_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 0.0331218000
_diffrn_orient_matrix_UB_12 -0.0891148000
_diffrn_orient_matrix_UB_13 -0.0648753000
_diffrn_orient_matrix_UB_21 -0.1030661000
_diffrn_orient_matrix_UB_22 -0.0672850000
_diffrn_orient_matrix_UB_23 0.0500604000
_diffrn_orient_matrix_UB_31 -0.1382938000
_diffrn_orient_matrix_UB_32 0.0288001000
_diffrn_orient_matrix_UB_33 -0.0839026000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.366
_reflns_Friedel_fraction_full 0.389
_reflns_Friedel_fraction_max 0.358
_reflns_number_gt 3943
_reflns_number_total 4255
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.513
_refine_diff_density_min -0.531
_refine_diff_density_rms 0.060
_refine_ls_abs_structure_details
;
Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack 0.06(3)
_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 476
_refine_ls_number_reflns 4255
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0295
_refine_ls_R_factor_gt 0.0257
_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^)+(0.0360P)^2^+0.5446P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0644
_refine_ls_wR_factor_ref 0.0677
_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, All O(H,H) groups
2.a Free rotating group:
O9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
N2(H2), N4(H4), C5(H5), C12(H12), C8(H8), C26(H26), C10(H10), C4(H4A),
C22(H22), C27(H27), C31(H31), C9(H9)
2.c Idealised Me refined as rotating group:
C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C36(H36A,H36B,H36C), C19(H19A,H19B,
H19C)
;
_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
Cd1 Cd 0.66760(15) 1.12972(2) 0.37424(11) 0.02710(9) Uani 1 1 d . . . . .
O9 O 0.1656(17) 0.11324(19) 0.3731(12) 0.0395(7) Uani 1 1 d . . . . .
H9A H 0.0925 0.1473 0.3388 0.059 Uiso 1 1 d G . . . .
H9B H 0.2356 0.1525 0.4027 0.059 Uiso 1 1 d G . . . .
O8 O 0.3203(11) 0.2067(5) 0.2017(6) 0.042(2) Uani 1 1 d . . . . .
O2 O 0.6543(10) 1.2614(6) 0.2637(8) 0.050(3) Uani 1 1 d . . . . .
O3 O 0.6787(10) 1.2598(6) 0.4873(8) 0.052(3) Uani 1 1 d . . . . .
O5 O 0.5153(10) 0.7929(5) 0.0468(6) 0.0357(18) Uani 1 1 d . . . . .
C30 C 0.3696(14) 0.3776(6) 0.1784(8) 0.028(2) Uani 1 1 d . . . . .
O4 O 0.4625(11) 1.1823(6) 0.4578(7) 0.043(2) Uani 1 1 d . . . . .
O1 O 0.8748(10) 1.1820(6) 0.2898(7) 0.043(2) Uani 1 1 d . . . . .
C17 C 0.4453(13) 0.8578(7) 0.2231(9) 0.025(2) Uani 1 1 d . . . . .
C34 C 0.3952(15) 0.1407(7) 0.0252(9) 0.030(2) Uani 1 1 d . . . . .
N5 N 0.4421(12) 0.7549(6) 0.1957(7) 0.0288(19) Uani 1 1 d . . . . .
C25 C 0.4602(14) 0.6217(7) 0.0720(8) 0.027(2) Uani 1 1 d . . . . .
N6 N 0.3949(11) 0.2452(5) 0.0547(7) 0.029(2) Uani 1 1 d . . . . .
N2 N 0.9614(10) 1.0018(6) 0.4756(7) 0.029(2) Uani 1 1 d . . . . .
H2 H 1.0164 1.0494 0.4593 0.035 Uiso 1 1 calc R . . . .
N4 N 0.3706(11) 1.0009(6) 0.2724(8) 0.031(2) Uani 1 1 d . . . . .
H4 H 0.3148 1.0473 0.2899 0.038 Uiso 1 1 calc R . . . .
N3 N 0.5246(11) 1.0115(6) 0.2755(7) 0.0285(19) Uani 1 1 d . . . . .
N1 N 0.8136(11) 1.0105(6) 0.4726(7) 0.031(2) Uani 1 1 d . . . . .
O7 O 0.4489(14) 0.2861(6) -0.0998(7) 0.057(3) Uani 1 1 d . . . . .
C5 C 1.0043(15) 1.3856(7) 0.0784(10) 0.038(3) Uani 1 1 d . . . . .
H5 H 1.0629 1.3681 0.0315 0.045 Uiso 1 1 calc R . . . .
C3 C 0.8525(13) 1.3357(7) 0.1989(9) 0.030(2) Uani 1 1 d . . . . .
C23 C 0.3925(15) 0.5786(7) 0.2303(9) 0.032(3) Uani 1 1 d . . . . .
C12 C 1.0251(14) 1.5668(8) 0.0401(9) 0.030(2) Uani 1 1 d . . . . .
H12 H 1.0934 1.5522 -0.0012 0.036 Uiso 1 1 calc R . . . .
C24 C 0.4214(14) 0.5517(7) 0.1389(8) 0.027(2) Uani 1 1 d . . . . .
C28 C 0.4416(14) 0.4204(7) 0.0121(8) 0.028(2) Uani 1 1 d . . . . .
C7 C 0.8684(12) 1.5133(7) 0.1577(8) 0.028(2) Uani 1 1 d . . . . .
C20 C 0.4733(14) 0.7306(7) 0.0991(9) 0.031(3) Uani 1 1 d . . . . .
C33 C 0.4278(15) 0.3138(7) -0.0164(8) 0.033(3) Uani 1 1 d . . . . .
C8 C 0.8087(14) 1.4328(7) 0.2085(9) 0.030(2) Uani 1 1 d . . . . .
H8 H 0.7387 1.4469 0.2489 0.036 Uiso 1 1 calc R . . . .
C6 C 0.9678(13) 1.4894(6) 0.0913(8) 0.025(2) Uani 1 1 d . . . . .
C29 C 0.4117(13) 0.4493(7) 0.1105(8) 0.025(2) Uani 1 1 d . . . . .
C14 C 1.1798(16) 0.8838(9) 0.5198(11) 0.047(3) Uani 1 1 d . . . . .
H14A H 1.2335 0.9034 0.5865 0.070 Uiso 1 1 calc GR . . . .
H14B H 1.2233 0.9173 0.4694 0.070 Uiso 1 1 calc GR . . . .
H14C H 1.1881 0.8127 0.5122 0.070 Uiso 1 1 calc GR . . . .
C26 C 0.4940(14) 0.5930(7) -0.0208(9) 0.032(2) Uani 1 1 d . . . . .
H26 H 0.5233 0.6398 -0.0642 0.038 Uiso 1 1 calc R . . . .
C1 C 0.7902(15) 1.2531(7) 0.2538(9) 0.032(3) Uani 1 1 d . . . . .
C32 C 0.3590(13) 0.2709(7) 0.1474(8) 0.027(2) Uani 1 1 d . . . . .
C2 C 0.5440(14) 1.2554(8) 0.4936(9) 0.032(2) Uani 1 1 d . . . . .
C18 C 0.3174(14) 0.9103(7) 0.2391(9) 0.030(2) Uani 1 1 d . . . . .
C15 C 0.7289(14) 0.9064(8) 0.2375(10) 0.040(3) Uani 1 1 d . . . . .
H15A H 0.7770 0.8614 0.2903 0.060 Uiso 1 1 calc GR . . . .
H15B H 0.7828 0.9690 0.2445 0.060 Uiso 1 1 calc GR . . . .
H15C H 0.7306 0.8777 0.1723 0.060 Uiso 1 1 calc GR . . . .
C21 C 0.4031(16) 0.6855(7) 0.2661(9) 0.038(3) Uani 1 1 d . . . . .
C36 C 0.1044(14) 0.0968(9) 0.0100(10) 0.041(3) Uani 1 1 d . . . . .
H36A H 0.0944 0.0888 0.0793 0.061 Uiso 1 1 calc GR . . . .
H36B H 0.0396 0.0495 -0.0324 0.061 Uiso 1 1 calc GR . . . .
H36C H 0.0752 0.1636 -0.0125 0.061 Uiso 1 1 calc GR . . . .
C35 C 0.2689(12) 0.0787(6) 0.0027(8) 0.0248(19) Uani 1 1 d . . . . .
C10 C 0.8827(14) 1.6871(8) 0.1152(9) 0.039(3) Uani 1 1 d . . . . .
H10 H 0.8545 1.7532 0.1227 0.047 Uiso 1 1 calc R . . . .
C4 C 0.9538(13) 1.3134(7) 0.1340(9) 0.032(2) Uani 1 1 d . . . . .
H4A H 0.9864 1.2478 0.1295 0.039 Uiso 1 1 calc R . . . .
C22 C 0.3512(13) 0.5071(7) 0.2992(8) 0.032(2) Uani 1 1 d . . . . .
H22 H 0.3306 0.5265 0.3614 0.038 Uiso 1 1 calc R . . . .
C27 C 0.4820(15) 0.4898(7) -0.0463(8) 0.041(3) Uani 1 1 d . . . . .
H27 H 0.5041 0.4701 -0.1080 0.049 Uiso 1 1 calc R . . . .
O6 O 0.3858(14) 0.7122(6) 0.3465(7) 0.060(3) Uani 1 1 d . . . . .
C11 C 0.9816(13) 1.6638(7) 0.0502(9) 0.029(2) Uani 1 1 d . . . . .
C16 C 0.5720(14) 0.9233(7) 0.2459(9) 0.032(2) Uani 1 1 d . . . . .
C13 C 1.0163(14) 0.9120(7) 0.5065(9) 0.032(2) Uani 1 1 d . . . . .
C31 C 0.3433(15) 0.4074(8) 0.2688(9) 0.037(3) Uani 1 1 d . . . . .
H31 H 0.3188 0.3593 0.3129 0.045 Uiso 1 1 calc R . . . .
C9 C 0.8277(14) 1.6123(8) 0.1677(9) 0.033(2) Uani 1 1 d . . . . .
H9 H 0.7621 1.6283 0.2106 0.039 Uiso 1 1 calc R . . . .
C19 C 0.1547(16) 0.8841(9) 0.2289(11) 0.047(3) Uani 1 1 d . . . . .
H19A H 0.1175 0.8533 0.1639 0.070 Uiso 1 1 calc GR . . . .
H19B H 0.0970 0.9437 0.2343 0.070 Uiso 1 1 calc GR . . . .
H19C H 0.1439 0.8383 0.2820 0.070 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
Cd1 0.03794(15) 0.01281(12) 0.03261(15) 0.0001(4) 0.01207(10) 0.0001(4)
O9 0.0369(16) 0.0314(14) 0.0538(19) -0.001(5) 0.0179(13) -0.003(5)
O8 0.071(6) 0.013(3) 0.045(5) 0.005(3) 0.021(4) -0.002(4)
O2 0.041(5) 0.045(5) 0.075(6) 0.025(4) 0.033(4) 0.011(3)
O3 0.042(6) 0.040(5) 0.069(6) -0.025(4) 0.005(4) 0.011(4)
O5 0.053(5) 0.018(3) 0.038(4) -0.002(3) 0.013(4) -0.008(3)
C30 0.044(7) 0.006(4) 0.035(5) 0.009(3) 0.009(5) -0.005(3)
O4 0.045(5) 0.031(4) 0.056(6) -0.018(4) 0.017(4) -0.004(4)
O1 0.038(5) 0.031(4) 0.058(6) 0.017(4) 0.010(4) 0.003(3)
C17 0.029(5) 0.015(4) 0.032(5) 0.000(3) 0.010(4) 0.005(3)
C34 0.044(6) 0.012(4) 0.031(5) -0.005(4) 0.001(4) -0.003(4)
N5 0.046(6) 0.014(4) 0.025(4) -0.006(3) 0.006(4) 0.000(3)
C25 0.037(6) 0.020(4) 0.021(4) -0.009(3) 0.001(4) 0.003(4)
N6 0.046(6) 0.008(4) 0.033(5) -0.002(3) 0.007(4) -0.001(3)
N2 0.034(6) 0.015(4) 0.037(5) 0.005(3) 0.006(4) -0.003(3)
N4 0.035(6) 0.016(4) 0.044(6) -0.005(4) 0.008(4) 0.005(4)
N3 0.026(5) 0.019(4) 0.039(5) -0.007(3) 0.004(3) 0.003(3)
N1 0.038(6) 0.013(4) 0.040(6) 0.001(3) 0.008(4) 0.001(3)
O7 0.115(10) 0.025(4) 0.037(5) -0.006(3) 0.027(6) -0.009(5)
C5 0.038(7) 0.022(5) 0.057(8) -0.007(4) 0.018(6) 0.001(4)
C3 0.031(6) 0.031(5) 0.028(5) 0.001(4) 0.006(4) -0.007(4)
C23 0.051(7) 0.008(4) 0.036(7) 0.000(4) 0.004(5) 0.000(4)
C12 0.036(7) 0.027(5) 0.029(6) 0.000(4) 0.012(5) -0.008(4)
C24 0.039(7) 0.013(4) 0.028(5) 0.006(3) 0.001(4) 0.000(4)
C28 0.044(6) 0.019(4) 0.022(6) -0.005(4) 0.007(4) 0.002(4)
C7 0.026(5) 0.029(5) 0.031(6) -0.001(4) 0.008(4) -0.002(4)
C20 0.036(7) 0.012(4) 0.040(7) 0.001(4) 0.002(5) 0.003(4)
C33 0.058(8) 0.021(5) 0.020(5) -0.004(3) 0.007(4) 0.001(4)
C8 0.033(6) 0.024(5) 0.034(6) 0.005(4) 0.008(5) 0.000(4)
C6 0.030(5) 0.016(4) 0.029(5) 0.003(3) 0.004(4) -0.003(3)
C29 0.034(6) 0.015(4) 0.023(5) -0.007(3) 0.003(4) 0.001(3)
C14 0.041(8) 0.039(6) 0.057(9) 0.015(6) 0.003(6) 0.003(5)
C26 0.050(7) 0.016(5) 0.032(6) 0.002(4) 0.015(5) -0.001(4)
C1 0.045(7) 0.019(5) 0.033(6) 0.002(4) 0.006(5) -0.005(4)
C32 0.041(7) 0.017(5) 0.022(5) -0.005(3) 0.005(5) -0.002(4)
C2 0.033(7) 0.029(5) 0.032(6) -0.004(4) 0.001(5) 0.012(4)
C18 0.041(7) 0.016(5) 0.032(6) -0.003(4) 0.002(5) -0.009(4)
C15 0.046(8) 0.029(6) 0.048(7) -0.015(5) 0.019(6) 0.004(5)
C21 0.060(9) 0.012(4) 0.043(7) 0.000(4) 0.011(6) -0.002(4)
C36 0.036(8) 0.033(6) 0.053(8) -0.009(5) 0.010(6) 0.001(5)
C35 0.028(5) 0.021(4) 0.027(5) 0.000(3) 0.008(3) 0.012(3)
C10 0.047(7) 0.023(5) 0.053(7) 0.003(5) 0.020(6) 0.001(5)
C4 0.035(6) 0.016(4) 0.048(7) -0.003(4) 0.011(5) -0.001(4)
C22 0.054(7) 0.018(4) 0.026(4) 0.010(3) 0.015(4) -0.001(4)
C27 0.070(8) 0.026(5) 0.027(5) -0.013(4) 0.012(5) -0.001(5)
O6 0.131(11) 0.016(4) 0.039(5) -0.008(3) 0.032(6) 0.000(5)
C11 0.034(6) 0.016(5) 0.036(6) 0.007(4) 0.005(5) -0.003(4)
C16 0.046(6) 0.012(4) 0.034(5) -0.007(4) 0.004(4) -0.010(4)
C13 0.037(6) 0.022(5) 0.035(6) 0.001(4) 0.007(5) -0.007(4)
C31 0.061(8) 0.023(5) 0.026(6) 0.001(4) 0.006(5) -0.005(5)
C9 0.036(7) 0.033(5) 0.032(6) 0.005(4) 0.017(5) -0.002(5)
C19 0.040(8) 0.042(7) 0.059(9) -0.011(6) 0.011(6) -0.010(5)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O2 2.289(9) . ?
Cd1 O3 2.296(8) . ?
Cd1 O4 2.450(8) . ?
Cd1 O1 2.472(9) . ?
Cd1 N3 2.278(9) . ?
Cd1 N1 2.296(9) . ?
Cd1 C1 2.700(11) . ?
Cd1 C2 2.713(11) . ?
O9 H9A 0.8501 . ?
O9 H9B 0.8500 . ?
O8 C32 1.222(13) . ?
O2 C1 1.259(15) . ?
O3 C2 1.230(15) . ?
O5 C20 1.200(13) . ?
C30 C29 1.427(14) . ?
C30 C32 1.482(12) . ?
C30 C31 1.346(16) . ?
O4 C2 1.254(14) . ?
O1 C1 1.248(14) . ?
C17 N5 1.421(12) . ?
C17 C18 1.398(16) . ?
C17 C16 1.416(14) . ?
C34 N6 1.451(11) . ?
C34 C35 1.384(15) . ?
C34 C13 1.361(17) 2_464 ?
N5 C20 1.421(15) . ?
N5 C21 1.419(14) . ?
C25 C24 1.391(15) . ?
C25 C20 1.499(12) . ?
C25 C26 1.397(15) . ?
N6 C33 1.399(13) . ?
N6 C32 1.393(14) . ?
N2 H2 0.8600 . ?
N2 N1 1.323(13) . ?
N2 C13 1.330(13) . ?
N4 H4 0.8600 . ?
N4 N3 1.380(12) . ?
N4 C18 1.342(12) . ?
N3 C16 1.340(13) . ?
N1 C35 1.346(12) 2_565 ?
O7 C33 1.233(14) . ?
C5 H5 0.9300 . ?
C5 C6 1.444(12) . ?
C5 C4 1.355(16) . ?
C3 C8 1.370(14) . ?
C3 C1 1.498(14) . ?
C3 C4 1.416(16) . ?
C23 C24 1.355(16) . ?
C23 C21 1.503(13) . ?
C23 C22 1.432(14) . ?
C12 H12 0.9300 . ?
C12 C6 1.397(13) . ?
C12 C11 1.368(14) . ?
C24 C29 1.418(5) . ?
C28 C33 1.473(13) . ?
C28 C29 1.456(14) . ?
C28 C27 1.313(15) . ?
C7 C8 1.436(14) . ?
C7 C6 1.423(5) . ?
C7 C9 1.386(14) . ?
C8 H8 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14 C13 1.488(18) . ?
C26 H26 0.9300 . ?
C26 C27 1.419(13) . ?
C2 C11 1.494(14) 2_485 ?
C18 C19 1.480(17) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 C16 1.453(16) . ?
C21 O6 1.178(14) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C36 C35 1.518(15) . ?
C35 N1 1.346(12) 2_464 ?
C10 H10 0.9300 . ?
C10 C11 1.404(17) . ?
C10 C9 1.373(15) . ?
C4 H4A 0.9300 . ?
C22 H22 0.9300 . ?
C22 C31 1.391(14) . ?
C27 H27 0.9300 . ?
C11 C2 1.494(14) 2_584 ?
C13 C34 1.361(17) 2_565 ?
C31 H31 0.9300 . ?
C9 H9 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cd1 O3 80.61(15) . . ?
O2 Cd1 O4 97.7(3) . . ?
O2 Cd1 O1 55.1(3) . . ?
O2 Cd1 N1 148.5(3) . . ?
O2 Cd1 C1 27.7(3) . . ?
O2 Cd1 C2 86.3(3) . . ?
O3 Cd1 O4 54.0(3) . . ?
O3 Cd1 O1 99.0(3) . . ?
O3 Cd1 N1 101.7(3) . . ?
O3 Cd1 C1 88.2(3) . . ?
O3 Cd1 C2 26.8(3) . . ?
O4 Cd1 O1 146.93(9) . . ?
O4 Cd1 C1 122.6(3) . . ?
O4 Cd1 C2 27.5(3) . . ?
O1 Cd1 C1 27.5(3) . . ?
O1 Cd1 C2 122.4(3) . . ?
N3 Cd1 O2 102.0(4) . . ?
N3 Cd1 O3 148.3(3) . . ?
N3 Cd1 O4 94.6(3) . . ?
N3 Cd1 O1 108.3(3) . . ?
N3 Cd1 N1 92.18(11) . . ?
N3 Cd1 C1 108.9(3) . . ?
N3 Cd1 C2 121.6(4) . . ?
N1 Cd1 O4 109.1(3) . . ?
N1 Cd1 O1 93.9(3) . . ?
N1 Cd1 C1 120.9(4) . . ?
N1 Cd1 C2 110.1(3) . . ?
C1 Cd1 C2 104.17(12) . . ?
H9A O9 H9B 109.4 . . ?
C1 O2 Cd1 94.6(7) . . ?
C2 O3 Cd1 95.9(7) . . ?
C29 C30 C32 118.4(10) . . ?
C31 C30 C29 119.9(8) . . ?
C31 C30 C32 121.7(9) . . ?
C2 O4 Cd1 88.0(7) . . ?
C1 O1 Cd1 86.5(8) . . ?
C18 C17 N5 123.5(10) . . ?
C18 C17 C16 107.7(9) . . ?
C16 C17 N5 128.7(10) . . ?
C35 C34 N6 126.0(11) . . ?
C13 C34 N6 126.5(11) 2_464 . ?
C13 C34 C35 107.3(9) 2_464 . ?
C20 N5 C17 117.4(8) . . ?
C21 N5 C17 117.0(9) . . ?
C21 N5 C20 125.6(8) . . ?
C24 C25 C20 120.9(10) . . ?
C24 C25 C26 121.5(9) . . ?
C26 C25 C20 117.6(10) . . ?
C33 N6 C34 115.5(9) . . ?
C32 N6 C34 119.7(9) . . ?
C32 N6 C33 124.7(8) . . ?
N1 N2 H2 123.5 . . ?
N1 N2 C13 113.1(9) . . ?
C13 N2 H2 123.5 . . ?
N3 N4 H4 123.6 . . ?
C18 N4 H4 123.6 . . ?
C18 N4 N3 112.7(9) . . ?
N4 N3 Cd1 121.8(6) . . ?
C16 N3 Cd1 127.4(8) . . ?
C16 N3 N4 106.2(8) . . ?
N2 N1 Cd1 121.7(6) . . ?
N2 N1 C35 105.8(8) . 2_565 ?
C35 N1 Cd1 128.1(8) 2_565 . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C4 C5 C6 120.5(11) . . ?
C8 C3 C1 120.5(10) . . ?
C8 C3 C4 119.4(10) . . ?
C4 C3 C1 120.1(10) . . ?
C24 C23 C21 122.1(10) . . ?
C24 C23 C22 122.2(9) . . ?
C22 C23 C21 115.7(10) . . ?
C6 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C11 C12 C6 120.7(11) . . ?
C25 C24 C29 119.0(7) . . ?
C23 C24 C25 121.9(9) . . ?
C23 C24 C29 119.2(6) . . ?
C29 C28 C33 118.0(9) . . ?
C27 C28 C33 123.1(9) . . ?
C27 C28 C29 118.8(9) . . ?
C6 C7 C8 118.4(7) . . ?
C9 C7 C8 122.4(10) . . ?
C9 C7 C6 119.1(7) . . ?
O5 C20 N5 121.5(9) . . ?
O5 C20 C25 123.3(11) . . ?
N5 C20 C25 115.0(9) . . ?
N6 C33 C28 118.4(8) . . ?
O7 C33 N6 121.2(9) . . ?
O7 C33 C28 120.4(10) . . ?
C3 C8 C7 121.4(11) . . ?
C3 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C12 C6 C5 122.4(10) . . ?
C12 C6 C7 119.1(7) . . ?
C7 C6 C5 118.5(7) . . ?
C30 C29 C28 121.8(9) . . ?
C24 C29 C30 119.0(6) . . ?
C24 C29 C28 119.2(6) . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
C25 C26 H26 121.2 . . ?
C25 C26 C27 117.5(9) . . ?
C27 C26 H26 121.2 . . ?
O2 C1 Cd1 57.7(6) . . ?
O2 C1 C3 117.2(10) . . ?
O1 C1 Cd1 66.0(6) . . ?
O1 C1 O2 123.3(11) . . ?
O1 C1 C3 119.5(12) . . ?
C3 C1 Cd1 170.1(8) . . ?
O8 C32 C30 121.1(10) . . ?
O8 C32 N6 120.5(9) . . ?
N6 C32 C30 118.4(9) . . ?
O3 C2 Cd1 57.3(6) . . ?
O3 C2 O4 120.8(10) . . ?
O3 C2 C11 118.6(11) . 2_485 ?
O4 C2 Cd1 64.5(6) . . ?
O4 C2 C11 120.5(12) . 2_485 ?
C11 C2 Cd1 171.9(8) 2_485 . ?
C17 C18 C19 133.8(10) . . ?
N4 C18 C17 104.9(10) . . ?
N4 C18 C19 121.3(11) . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
N5 C21 C23 114.5(9) . . ?
O6 C21 N5 120.7(9) . . ?
O6 C21 C23 124.7(10) . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
C34 C35 C36 130.7(9) . . ?
N1 C35 C34 108.3(9) 2_464 . ?
N1 C35 C36 121.0(10) 2_464 . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 120.0(10) . . ?
C5 C4 C3 121.5(10) . . ?
C5 C4 H4A 119.3 . . ?
C3 C4 H4A 119.3 . . ?
C23 C22 H22 121.5 . . ?
C31 C22 C23 117.0(10) . . ?
C31 C22 H22 121.5 . . ?
C28 C27 C26 123.9(10) . . ?
C28 C27 H27 118.1 . . ?
C26 C27 H27 118.1 . . ?
C12 C11 C2 119.3(10) . 2_584 ?
C12 C11 C10 120.1(10) . . ?
C10 C11 C2 120.6(10) . 2_584 ?
C17 C16 C15 129.3(9) . . ?
N3 C16 C17 108.5(10) . . ?
N3 C16 C15 122.1(10) . . ?
C34 C13 C14 130.7(10) 2_565 . ?
N2 C13 C34 105.5(10) . 2_565 ?
N2 C13 C14 123.8(10) . . ?
C30 C31 C22 122.7(10) . . ?
C30 C31 H31 118.7 . . ?
C22 C31 H31 118.7 . . ?
C7 C9 H9 119.5 . . ?
C10 C9 C7 120.9(10) . . ?
C10 C9 H9 119.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 O2 C1 O1 7.5(14) . . . . ?
Cd1 O2 C1 C3 -170.2(9) . . . . ?
Cd1 O3 C2 O4 11.6(13) . . . . ?
Cd1 O3 C2 C11 -171.9(9) . . . 2_485 ?
Cd1 O4 C2 O3 -10.8(12) . . . . ?
Cd1 O4 C2 C11 172.7(10) . . . 2_485 ?
Cd1 O1 C1 O2 -6.9(13) . . . . ?
Cd1 O1 C1 C3 170.7(10) . . . . ?
Cd1 N3 C16 C17 156.4(8) . . . . ?
Cd1 N3 C16 C15 -25.6(17) . . . . ?
C17 N5 C20 O5 7.2(18) . . . . ?
C17 N5 C20 C25 -176.9(10) . . . . ?
C17 N5 C21 C23 176.5(10) . . . . ?
C17 N5 C21 O6 -5.5(19) . . . . ?
C34 N6 C33 O7 2.9(18) . . . . ?
C34 N6 C33 C28 -175.1(11) . . . . ?
C34 N6 C32 O8 -3.6(19) . . . . ?
C34 N6 C32 C30 176.1(10) . . . . ?
N5 C17 C18 N4 174.4(10) . . . . ?
N5 C17 C18 C19 -4(2) . . . . ?
N5 C17 C16 N3 -175.2(11) . . . . ?
N5 C17 C16 C15 7(2) . . . . ?
C25 C24 C29 C30 -179.0(16) . . . . ?
C25 C24 C29 C28 -0.4(9) . . . . ?
C25 C26 C27 C28 0(2) . . . . ?
N6 C34 C35 N1 176.2(11) . . . 2_464 ?
N6 C34 C35 C36 -5(2) . . . . ?
N4 N3 C16 C17 0.7(13) . . . . ?
N4 N3 C16 C15 178.7(10) . . . . ?
N3 N4 C18 C17 2.2(13) . . . . ?
N3 N4 C18 C19 -179.3(11) . . . . ?
N1 N2 C13 C34 -0.3(14) . . . 2_565 ?
N1 N2 C13 C14 -177.9(11) . . . . ?
C23 C24 C29 C30 0.9(10) . . . . ?
C23 C24 C29 C28 179.6(16) . . . . ?
C23 C22 C31 C30 -1(2) . . . . ?
C24 C25 C20 O5 175.3(12) . . . . ?
C24 C25 C20 N5 -0.5(17) . . . . ?
C24 C25 C26 C27 2.2(19) . . . . ?
C24 C23 C21 N5 1.4(18) . . . . ?
C24 C23 C21 O6 -176.5(15) . . . . ?
C24 C23 C22 C31 1(2) . . . . ?
C20 N5 C21 C23 -1.3(18) . . . . ?
C20 N5 C21 O6 176.6(14) . . . . ?
C20 C25 C24 C23 1(2) . . . . ?
C20 C25 C24 C29 -179.4(8) . . . . ?
C20 C25 C26 C27 179.8(11) . . . . ?
C33 N6 C32 O8 174.4(12) . . . . ?
C33 N6 C32 C30 -6.0(19) . . . . ?
C33 C28 C29 C30 -0.2(18) . . . . ?
C33 C28 C29 C24 -178.8(8) . . . . ?
C33 C28 C27 C26 179.1(12) . . . . ?
C8 C3 C1 O2 35.0(17) . . . . ?
C8 C3 C1 O1 -142.8(13) . . . . ?
C8 C3 C4 C5 -2.4(19) . . . . ?
C8 C7 C6 C5 -0.2(10) . . . . ?
C8 C7 C6 C12 179.1(16) . . . . ?
C8 C7 C9 C10 -177.7(12) . . . . ?
C6 C5 C4 C3 6.1(19) . . . . ?
C6 C12 C11 C2 -179.4(11) . . . 2_584 ?
C6 C12 C11 C10 2(2) . . . . ?
C6 C7 C8 C3 3.9(15) . . . . ?
C6 C7 C9 C10 -0.5(16) . . . . ?
C29 C30 C32 O8 -178.5(12) . . . . ?
C29 C30 C32 N6 1.9(18) . . . . ?
C29 C30 C31 C22 2(2) . . . . ?
C29 C28 C33 N6 -3.5(17) . . . . ?
C29 C28 C33 O7 178.5(13) . . . . ?
C29 C28 C27 C26 -2(2) . . . . ?
C26 C25 C24 C23 178.2(12) . . . . ?
C26 C25 C24 C29 -1.9(15) . . . . ?
C26 C25 C20 O5 -2.3(19) . . . . ?
C26 C25 C20 N5 -178.1(11) . . . . ?
C1 C3 C8 C7 179.2(11) . . . . ?
C1 C3 C4 C5 175.7(12) . . . . ?
C32 C30 C29 C24 179.6(8) . . . . ?
C32 C30 C29 C28 1.0(19) . . . . ?
C32 C30 C31 C22 -179.4(12) . . . . ?
C32 N6 C33 O7 -175.2(13) . . . . ?
C32 N6 C33 C28 6.8(19) . . . . ?
C18 C17 N5 C20 116.0(13) . . . . ?
C18 C17 N5 C21 -62.0(16) . . . . ?
C18 C17 C16 N3 0.6(13) . . . . ?
C18 C17 C16 C15 -177.2(12) . . . . ?
C18 N4 N3 Cd1 -159.3(8) . . . . ?
C18 N4 N3 C16 -1.9(13) . . . . ?
C21 N5 C20 O5 -175.0(12) . . . . ?
C21 N5 C20 C25 1.0(18) . . . . ?
C21 C23 C24 C25 -1(2) . . . . ?
C21 C23 C24 C29 179.0(9) . . . . ?
C21 C23 C22 C31 -178.8(11) . . . . ?
C35 C34 N6 C33 -111.7(14) . . . . ?
C35 C34 N6 C32 66.5(16) . . . . ?
C4 C5 C6 C12 176.0(13) . . . . ?
C4 C5 C6 C7 -4.7(16) . . . . ?
C4 C3 C8 C7 -2.8(19) . . . . ?
C4 C3 C1 O2 -143.1(12) . . . . ?
C4 C3 C1 O1 39.1(17) . . . . ?
C22 C23 C24 C25 179.4(12) . . . . ?
C22 C23 C24 C29 -0.5(16) . . . . ?
C22 C23 C21 N5 -179.1(12) . . . . ?
C22 C23 C21 O6 3(2) . . . . ?
C27 C28 C33 N6 175.3(13) . . . . ?
C27 C28 C33 O7 -3(2) . . . . ?
C27 C28 C29 C30 -179.0(13) . . . . ?
C27 C28 C29 C24 2.3(15) . . . . ?
C11 C12 C6 C5 176.6(12) . . . . ?
C11 C12 C6 C7 -2.7(15) . . . . ?
C11 C10 C9 C7 0(2) . . . . ?
C16 C17 N5 C20 -68.7(17) . . . . ?
C16 C17 N5 C21 113.2(14) . . . . ?
C16 C17 C18 N4 -1.7(13) . . . . ?
C16 C17 C18 C19 -179.9(13) . . . . ?
C13 C34 N6 C33 62.6(17) 2_464 . . . ?
C13 C34 N6 C32 -119.2(14) 2_464 . . . ?
C13 C34 C35 N1 1.0(13) 2_464 . . 2_464 ?
C13 C34 C35 C36 179.4(12) 2_464 . . . ?
C13 N2 N1 Cd1 -158.6(8) . . . . ?
C13 N2 N1 C35 -0.3(13) . . . 2_565 ?
C31 C30 C29 C24 -1.6(16) . . . . ?
C31 C30 C29 C28 179.8(12) . . . . ?
C31 C30 C32 O8 3(2) . . . . ?
C31 C30 C32 N6 -176.9(12) . . . . ?
C9 C7 C8 C3 -178.9(12) . . . . ?
C9 C7 C6 C5 -177.5(16) . . . . ?
C9 C7 C6 C12 1.8(10) . . . . ?
C9 C10 C11 C12 -1(2) . . . . ?
C9 C10 C11 C2 -179.2(11) . . . 2_584 ?
_shelx_res_file
;
TITL FJU-69 in Pn #7
REM reset to Pn #7
CELL 1.54184 8.968799 13.357094 13.435198 90 102.0705 90
ZERR 2 0.000206 0.00028 0.000286 0 0.0022 0
LATT -1
SYMM 0.5+X,-Y,0.5+Z
SFAC C H Cd N O
UNIT 72 52 2 12 18
L.S. 20
PLAN 20
BOND
MORE -1
BOND $H
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.036000 0.544600
FVAR 4.00798
CD1 3 0.667599 1.129723 0.374239 11.00000 0.03794 0.01281 =
0.03261 0.00008 0.01207 0.00013
AFIX 6
O9 5 0.165625 0.113242 0.373142 11.00000 0.03693 0.03144 =
0.05382 -0.00098 0.01793 -0.00297
H9A 2 0.092540 0.147286 0.338821 11.00000 -1.50000
H9B 2 0.235570 0.152549 0.402672 11.00000 -1.50000
AFIX 0
O8 5 0.320324 0.206730 0.201710 11.00000 0.07121 0.01303 =
0.04484 0.00451 0.02090 -0.00164
O2 5 0.654271 1.261446 0.263733 11.00000 0.04052 0.04459 =
0.07458 0.02505 0.03274 0.01125
O3 5 0.678682 1.259756 0.487293 11.00000 0.04240 0.04020 =
0.06913 -0.02466 0.00492 0.01085
O5 5 0.515319 0.792926 0.046808 11.00000 0.05312 0.01802 =
0.03753 -0.00234 0.01289 -0.00779
C30 1 0.369568 0.377573 0.178384 11.00000 0.04364 0.00648 =
0.03481 0.00878 0.00865 -0.00538
O4 5 0.462492 1.182263 0.457837 11.00000 0.04550 0.03114 =
0.05578 -0.01771 0.01737 -0.00396
O1 5 0.874795 1.182046 0.289770 11.00000 0.03814 0.03138 =
0.05841 0.01722 0.01034 0.00290
C17 1 0.445278 0.857800 0.223118 11.00000 0.02877 0.01511 =
0.03235 0.00032 0.00963 0.00471
C34 1 0.395175 0.140708 0.025202 11.00000 0.04417 0.01166 =
0.03126 -0.00513 0.00149 -0.00346
N5 4 0.442072 0.754908 0.195732 11.00000 0.04600 0.01417 =
0.02526 -0.00590 0.00553 0.00012
C25 1 0.460189 0.621703 0.071984 11.00000 0.03674 0.01952 =
0.02098 -0.00859 0.00077 0.00347
N6 4 0.394934 0.245172 0.054735 11.00000 0.04624 0.00827 =
0.03272 -0.00211 0.00682 -0.00107
N2 4 0.961411 1.001828 0.475591 11.00000 0.03422 0.01547 =
0.03717 0.00524 0.00609 -0.00349
AFIX 43
H2 2 1.016370 1.049369 0.459256 11.00000 -1.20000
AFIX 0
N4 4 0.370645 1.000861 0.272393 11.00000 0.03503 0.01555 =
0.04354 -0.00469 0.00831 0.00478
AFIX 43
H4 2 0.314810 1.047260 0.289915 11.00000 -1.20000
AFIX 0
N3 4 0.524635 1.011468 0.275499 11.00000 0.02601 0.01927 =
0.03922 -0.00726 0.00436 0.00276
N1 4 0.813585 1.010522 0.472579 11.00000 0.03839 0.01301 =
0.04036 0.00095 0.00758 0.00093
O7 5 0.448881 0.286103 -0.099832 11.00000 0.11459 0.02513 =
0.03656 -0.00575 0.02708 -0.00918
C5 1 1.004313 1.385556 0.078374 11.00000 0.03765 0.02179 =
0.05676 -0.00741 0.01776 0.00053
AFIX 43
H5 2 1.062912 1.368093 0.031538 11.00000 -1.20000
AFIX 0
C3 1 0.852496 1.335659 0.198901 11.00000 0.03074 0.03096 =
0.02822 0.00097 0.00575 -0.00672
C23 1 0.392503 0.578645 0.230303 11.00000 0.05103 0.00840 =
0.03558 0.00019 0.00388 0.00019
C12 1 1.025064 1.566807 0.040125 11.00000 0.03597 0.02713 =
0.02941 0.00015 0.01183 -0.00772
AFIX 43
H12 2 1.093445 1.552202 -0.001203 11.00000 -1.20000
AFIX 0
C24 1 0.421385 0.551674 0.138934 11.00000 0.03857 0.01286 =
0.02754 0.00621 0.00138 -0.00010
C28 1 0.441619 0.420416 0.012076 11.00000 0.04430 0.01860 =
0.02189 -0.00490 0.00676 0.00223
C7 1 0.868420 1.513304 0.157712 11.00000 0.02628 0.02923 =
0.03098 -0.00104 0.00850 -0.00243
C20 1 0.473269 0.730636 0.099106 11.00000 0.03628 0.01236 =
0.04035 0.00063 0.00186 0.00336
C33 1 0.427755 0.313811 -0.016359 11.00000 0.05779 0.02101 =
0.02005 -0.00404 0.00665 0.00100
C8 1 0.808698 1.432801 0.208525 11.00000 0.03263 0.02391 =
0.03438 0.00499 0.00822 -0.00027
AFIX 43
H8 2 0.738749 1.446936 0.248850 11.00000 -1.20000
AFIX 0
C6 1 0.967821 1.489436 0.091264 11.00000 0.02997 0.01590 =
0.02873 0.00331 0.00438 -0.00305
C29 1 0.411680 0.449268 0.110524 11.00000 0.03450 0.01467 =
0.02337 -0.00660 0.00251 0.00147
C14 1 1.179803 0.883848 0.519833 11.00000 0.04129 0.03879 =
0.05732 0.01470 0.00254 0.00346
AFIX 137
H14A 2 1.233500 0.903366 0.586493 11.00000 -1.50000
H14B 2 1.223322 0.917296 0.469403 11.00000 -1.50000
H14C 2 1.188079 0.812727 0.512212 11.00000 -1.50000
AFIX 0
C26 1 0.494020 0.593031 -0.020792 11.00000 0.05033 0.01614 =
0.03199 0.00222 0.01515 -0.00078
AFIX 43
H26 2 0.523314 0.639840 -0.064244 11.00000 -1.20000
AFIX 0
C1 1 0.790233 1.253131 0.253769 11.00000 0.04458 0.01857 =
0.03250 0.00156 0.00595 -0.00530
C32 1 0.358962 0.270928 0.147362 11.00000 0.04135 0.01736 =
0.02213 -0.00505 0.00474 -0.00227
C2 1 0.543972 1.255365 0.493629 11.00000 0.03289 0.02903 =
0.03207 -0.00408 0.00135 0.01223
C18 1 0.317445 0.910293 0.239064 11.00000 0.04071 0.01582 =
0.03226 -0.00346 0.00161 -0.00863
C15 1 0.728914 0.906413 0.237546 11.00000 0.04626 0.02879 =
0.04831 -0.01496 0.01865 0.00392
AFIX 137
H15A 2 0.777012 0.861417 0.290290 11.00000 -1.50000
H15B 2 0.782821 0.968962 0.244529 11.00000 -1.50000
H15C 2 0.730604 0.877682 0.172295 11.00000 -1.50000
AFIX 0
C21 1 0.403099 0.685482 0.266119 11.00000 0.06016 0.01237 =
0.04313 0.00025 0.01123 -0.00162
C36 1 0.104429 0.096801 0.009961 11.00000 0.03622 0.03343 =
0.05272 -0.00909 0.00966 0.00106
AFIX 137
H36A 2 0.094439 0.088779 0.079274 11.00000 -1.50000
H36B 2 0.039641 0.049516 -0.032355 11.00000 -1.50000
H36C 2 0.075180 0.163555 -0.012468 11.00000 -1.50000
AFIX 0
C35 1 0.268941 0.078694 0.002738 11.00000 0.02758 0.02051 =
0.02734 -0.00019 0.00788 0.01198
C10 1 0.882713 1.687127 0.115183 11.00000 0.04660 0.02253 =
0.05281 0.00270 0.01968 0.00135
AFIX 43
H10 2 0.854461 1.753242 0.122678 11.00000 -1.20000
AFIX 0
C4 1 0.953808 1.313382 0.134006 11.00000 0.03456 0.01607 =
0.04776 -0.00337 0.01138 -0.00131
AFIX 43
H4A 2 0.986381 1.247753 0.129488 11.00000 -1.20000
AFIX 0
C22 1 0.351192 0.507142 0.299203 11.00000 0.05439 0.01752 =
0.02640 0.00971 0.01488 -0.00063
AFIX 43
H22 2 0.330576 0.526517 0.361436 11.00000 -1.20000
AFIX 0
C27 1 0.482037 0.489801 -0.046311 11.00000 0.07045 0.02564 =
0.02710 -0.01320 0.01193 -0.00128
AFIX 43
H27 2 0.504122 0.470136 -0.108046 11.00000 -1.20000
AFIX 0
O6 5 0.385761 0.712235 0.346500 11.00000 0.13082 0.01586 =
0.03909 -0.00843 0.03245 0.00019
C11 1 0.981637 1.663821 0.050171 11.00000 0.03365 0.01606 =
0.03643 0.00734 0.00528 -0.00295
C16 1 0.572010 0.923327 0.245907 11.00000 0.04633 0.01228 =
0.03422 -0.00656 0.00370 -0.00979
C13 1 1.016253 0.911992 0.506485 11.00000 0.03676 0.02222 =
0.03534 0.00083 0.00683 -0.00732
C31 1 0.343285 0.407355 0.268837 11.00000 0.06060 0.02334 =
0.02609 0.00095 0.00603 -0.00473
AFIX 43
H31 2 0.318831 0.359266 0.312868 11.00000 -1.20000
AFIX 0
C9 1 0.827666 1.612335 0.167702 11.00000 0.03634 0.03324 =
0.03235 0.00528 0.01658 -0.00225
AFIX 43
H9 2 0.762114 1.628338 0.210582 11.00000 -1.20000
AFIX 0
C19 1 0.154664 0.884065 0.228945 11.00000 0.03952 0.04201 =
0.05904 -0.01103 0.01086 -0.00981
AFIX 137
H19A 2 0.117487 0.853267 0.163928 11.00000 -1.50000
H19B 2 0.097012 0.943655 0.234291 11.00000 -1.50000
H19C 2 0.143888 0.838257 0.282049 11.00000 -1.50000
AFIX 0
HKLF 4
REM FJU-69 in Pn #7
REM R1 = 0.0257 for 3943 Fo > 4sig(Fo) and 0.0295 for all 4255 data
REM 476 parameters refined using 2 restraints
END
WGHT 0.0360 0.5445
REM Highest difference peak 0.513, deepest hole -0.531, 1-sigma level 0.060
Q1 1 1.1695 1.3911 -0.1253 11.00000 0.05 0.51
Q2 1 0.7615 1.0607 0.4622 11.00000 0.05 0.27
Q3 1 0.4236 1.1562 0.5014 11.00000 0.05 0.26
Q4 1 0.9096 1.1617 0.2487 11.00000 0.05 0.26
Q5 1 0.5786 1.0596 0.2934 11.00000 0.05 0.26
Q6 1 0.4708 0.6722 0.0869 11.00000 0.05 0.26
Q7 1 0.3617 0.3265 0.1655 11.00000 0.05 0.23
Q8 1 0.3879 0.6256 0.2458 11.00000 0.05 0.23
Q9 1 0.4361 0.3698 0.0060 11.00000 0.05 0.22
Q10 1 0.8255 1.1248 0.4244 11.00000 0.05 0.22
Q11 1 0.3243 0.1210 0.0155 11.00000 0.05 0.21
Q12 1 0.5140 0.8800 0.2427 11.00000 0.05 0.21
Q13 1 0.5091 1.1256 0.3273 11.00000 0.05 0.21
Q14 1 0.6328 1.2865 0.4236 11.00000 0.05 0.21
Q15 1 0.7042 1.2846 0.3259 11.00000 0.05 0.21
Q16 1 0.2899 0.0306 -0.0041 11.00000 0.05 0.20
Q17 1 0.5475 0.9662 0.2583 11.00000 0.05 0.20
Q18 1 0.7933 1.0289 0.5207 11.00000 0.05 0.20
Q19 1 0.7397 1.1977 0.4622 11.00000 0.05 0.20
Q20 1 0.3920 0.1897 0.0405 11.00000 0.05 0.19
;
_shelx_res_checksum 97119
_olex2_submission_special_instructions 'No special instructions were received'