# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_Complex_1
_database_code_depnum_ccdc_archive 'CCDC 1993505'
loop_
_audit_author_name
_audit_author_address
'Krishna K. Damodaran'
;University of Iceland
Iceland
;
_audit_update_record
;
2020-03-29 deposited with the CCDC. 2020-12-09 downloaded from the CCDC.
;
_audit_creation_date 2019-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H26 N8 O2 Zn'
_chemical_formula_sum 'C36 H26 N8 O2 Zn'
_chemical_formula_weight 668.02
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Zn Zn 0.2839 1.4301 '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 15
_space_group_name_H-M_alt 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 18.2863(11)
_cell_length_b 11.3902(6)
_cell_length_c 30.447(2)
_cell_angle_alpha 90
_cell_angle_beta 106.745(2)
_cell_angle_gamma 90
_cell_volume 6072.7(6)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 9997
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 29.58
_cell_measurement_theta_min 3.04
_shelx_estimated_absorpt_T_max 0.919
_shelx_estimated_absorpt_T_min 0.709
_exptl_absorpt_coefficient_mu 0.858
_exptl_absorpt_correction_T_max 0.7459
_exptl_absorpt_correction_T_min 0.6668
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0553 before and 0.0442 after correction. The Ratio of minimum to maximum transmission is 0.8940. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.461
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 2752
_exptl_crystal_size_max 0.43
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0535
_diffrn_reflns_av_unetI/netI 0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 42
_diffrn_reflns_limit_l_min -42
_diffrn_reflns_number 83125
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.665
_diffrn_reflns_theta_min 3.040
_diffrn_ambient_temperature 149.98
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7283
_reflns_number_total 8546
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT V8.38A (?, 2016)'
_computing_data_collection 'SAINT V8.38A (?, 2016)'
_computing_data_reduction 'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max 0.600
_refine_diff_density_min -0.377
_refine_diff_density_rms 0.056
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.018
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 424
_refine_ls_number_reflns 8546
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0447
_refine_ls_R_factor_gt 0.0341
_refine_ls_restrained_S_all 1.018
_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^)+(0.0435P)^2^+7.3384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0842
_refine_ls_wR_factor_ref 0.0880
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27),
C28(H28), C32(H32), C33(H33), C34(H34), C35(H35), C41(H41), C42(H42),
C43(H43), C44(H44), C45(H45)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.32393(2) 0.65805(2) 0.61785(2) 0.01774(5) Uani 1 1 d . . . . .
N1 N 0.44764(8) 0.68619(12) 0.65951(5) 0.0245(3) Uani 1 1 d . . . . .
C2 C 0.48293(11) 0.78727(15) 0.67478(7) 0.0316(4) Uani 1 1 d . . . . .
H2 H 0.457110 0.858781 0.664192 0.038 Uiso 1 1 calc R . . . .
C3 C 0.55572(11) 0.79243(18) 0.70544(7) 0.0397(5) Uani 1 1 d . . . . .
H3 H 0.579167 0.865777 0.715730 0.048 Uiso 1 1 calc R . . . .
C4 C 0.59299(12) 0.68854(19) 0.72054(8) 0.0425(5) Uani 1 1 d . . . . .
H4 H 0.642315 0.689310 0.742062 0.051 Uiso 1 1 calc R . . . .
C5 C 0.55808(10) 0.58261(17) 0.70414(7) 0.0338(4) Uani 1 1 d . . . . .
H5 H 0.583564 0.510200 0.713537 0.041 Uiso 1 1 calc R . . . .
C6 C 0.48483(9) 0.58490(14) 0.67358(6) 0.0243(3) Uani 1 1 d . . . . .
C7 C 0.44067(9) 0.47626(14) 0.65720(5) 0.0228(3) Uani 1 1 d . . . . .
C8 C 0.47835(9) 0.35967(15) 0.65844(6) 0.0278(3) Uani 1 1 d . . . . .
C9 C 0.44898(13) 0.25745(19) 0.67122(12) 0.0607(8) Uani 1 1 d . . . . .
H9 H 0.405755 0.260096 0.682570 0.073 Uiso 1 1 calc R . . . .
C10 C 0.48346(16) 0.1512(2) 0.66724(15) 0.0851(13) Uani 1 1 d . . . . .
H10 H 0.463470 0.080071 0.675339 0.102 Uiso 1 1 calc R . . . .
C11 C 0.54607(15) 0.1494(2) 0.65167(11) 0.0617(8) Uani 1 1 d . . . . .
H11 H 0.569979 0.077375 0.648137 0.074 Uiso 1 1 calc R . . . .
C12 C 0.57361(15) 0.2539(2) 0.64126(8) 0.0488(6) Uani 1 1 d . . . . .
H12 H 0.618574 0.252911 0.631582 0.059 Uiso 1 1 calc R . . . .
N13 N 0.54068(10) 0.35811(15) 0.64393(6) 0.0384(4) Uani 1 1 d . . . . .
N14 N 0.36772(7) 0.49291(11) 0.64103(4) 0.0199(2) Uani 1 1 d . . . . .
N15 N 0.31895(7) 0.40027(11) 0.62890(5) 0.0210(2) Uani 1 1 d . . . . .
C16 C 0.24739(8) 0.44028(12) 0.60969(5) 0.0178(3) Uani 1 1 d . . . . .
C17 C 0.18743(8) 0.34784(12) 0.60321(5) 0.0173(2) Uani 1 1 d . . . . .
C18 C 0.20739(9) 0.23162(13) 0.61615(6) 0.0236(3) Uani 1 1 d . . . . .
H18 H 0.259644 0.210870 0.628380 0.028 Uiso 1 1 calc R . . . .
C19 C 0.15129(10) 0.14646(13) 0.61122(6) 0.0274(3) Uani 1 1 d . . . . .
H19 H 0.165276 0.067816 0.620219 0.033 Uiso 1 1 calc R . . . .
C20 C 0.07509(10) 0.17576(15) 0.59324(6) 0.0287(3) Uani 1 1 d . . . . .
H20 H 0.036709 0.117379 0.589652 0.034 Uiso 1 1 calc R . . . .
C21 C 0.05511(10) 0.29071(16) 0.58052(7) 0.0316(4) Uani 1 1 d . . . . .
H21 H 0.002786 0.311166 0.568412 0.038 Uiso 1 1 calc R . . . .
C22 C 0.11093(9) 0.37642(14) 0.58531(6) 0.0245(3) Uani 1 1 d . . . . .
H22 H 0.096596 0.454929 0.576276 0.029 Uiso 1 1 calc R . . . .
O23 O 0.22867(6) 0.54552(9) 0.59848(4) 0.0234(2) Uani 1 1 d . . . . .
N24 N 0.35000(7) 0.65324(10) 0.55233(4) 0.0191(2) Uani 1 1 d . . . . .
C25 C 0.36113(10) 0.55637(14) 0.53052(6) 0.0266(3) Uani 1 1 d . . . . .
H25 H 0.361365 0.482644 0.545146 0.032 Uiso 1 1 calc R . . . .
C26 C 0.37236(12) 0.55867(15) 0.48754(6) 0.0324(4) Uani 1 1 d . . . . .
H26 H 0.381922 0.488435 0.473294 0.039 Uiso 1 1 calc R . . . .
C27 C 0.36928(12) 0.66600(16) 0.46583(6) 0.0324(4) Uani 1 1 d . . . . .
H27 H 0.375303 0.670054 0.435898 0.039 Uiso 1 1 calc R . . . .
C28 C 0.35736(9) 0.76796(14) 0.48793(5) 0.0233(3) Uani 1 1 d . . . . .
H28 H 0.354727 0.842202 0.473338 0.028 Uiso 1 1 calc R . . . .
C29 C 0.34939(8) 0.75891(12) 0.53185(5) 0.0166(2) Uani 1 1 d . . . . .
C30 C 0.33889(8) 0.86198(12) 0.55959(5) 0.0163(2) Uani 1 1 d . . . . .
C31 C 0.35766(9) 0.98325(12) 0.54826(5) 0.0185(3) Uani 1 1 d . . . . .
C32 C 0.31407(10) 1.07965(13) 0.55328(6) 0.0258(3) Uani 1 1 d . . . . .
H32 H 0.269019 1.069515 0.562453 0.031 Uiso 1 1 calc R . . . .
C33 C 0.33764(12) 1.19100(14) 0.54463(7) 0.0336(4) Uani 1 1 d . . . . .
H33 H 0.308818 1.258382 0.547606 0.040 Uiso 1 1 calc R . . . .
C34 C 0.40367(12) 1.20207(15) 0.53164(7) 0.0356(4) Uani 1 1 d . . . . .
H34 H 0.421614 1.277174 0.525937 0.043 Uiso 1 1 calc R . . . .
C35 C 0.44325(11) 1.10098(14) 0.52709(6) 0.0298(3) Uani 1 1 d . . . . .
H35 H 0.488516 1.109012 0.517988 0.036 Uiso 1 1 calc R . . . .
N36 N 0.42124(8) 0.99323(11) 0.53480(5) 0.0229(3) Uani 1 1 d . . . . .
N37 N 0.31731(7) 0.83344(10) 0.59512(4) 0.0176(2) Uani 1 1 d . . . . .
N38 N 0.30928(8) 0.91561(10) 0.62630(4) 0.0192(2) Uani 1 1 d . . . . .
C39 C 0.29126(9) 0.85960(12) 0.66053(5) 0.0190(3) Uani 1 1 d . . . . .
C40 C 0.28528(9) 0.93334(12) 0.69938(5) 0.0190(3) Uani 1 1 d . . . . .
C41 C 0.31970(11) 1.04320(14) 0.70751(6) 0.0289(3) Uani 1 1 d . . . . .
H41 H 0.343377 1.075779 0.686314 0.035 Uiso 1 1 calc R . . . .
C42 C 0.31932(13) 1.10502(16) 0.74669(7) 0.0378(4) Uani 1 1 d . . . . .
H42 H 0.344379 1.178843 0.752747 0.045 Uiso 1 1 calc R . . . .
C43 C 0.28287(11) 1.06036(16) 0.77699(6) 0.0325(4) Uani 1 1 d . . . . .
H43 H 0.282257 1.103899 0.803497 0.039 Uiso 1 1 calc R . . . .
C44 C 0.24737(10) 0.95241(15) 0.76867(6) 0.0282(3) Uani 1 1 d . . . . .
H44 H 0.222037 0.921467 0.789331 0.034 Uiso 1 1 calc R . . . .
C45 C 0.24884(10) 0.88911(14) 0.72989(6) 0.0262(3) Uani 1 1 d . . . . .
H45 H 0.224565 0.814616 0.724264 0.031 Uiso 1 1 calc R . . . .
O46 O 0.28140(8) 0.74947(9) 0.66329(4) 0.0270(2) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.02223(9) 0.01360(8) 0.01882(8) -0.00096(6) 0.00817(6) -0.00263(6)
N1 0.0221(6) 0.0252(6) 0.0246(6) -0.0006(5) 0.0043(5) -0.0041(5)
C2 0.0278(8) 0.0271(8) 0.0360(9) -0.0047(7) 0.0031(7) -0.0053(6)
C3 0.0300(9) 0.0345(9) 0.0467(11) -0.0106(8) -0.0016(8) -0.0118(7)
C4 0.0274(9) 0.0429(10) 0.0453(11) -0.0043(9) -0.0082(8) -0.0083(8)
C5 0.0242(8) 0.0333(9) 0.0365(9) 0.0019(7) -0.0030(7) -0.0033(7)
C6 0.0207(7) 0.0270(7) 0.0236(7) 0.0010(6) 0.0038(6) -0.0042(6)
C7 0.0197(7) 0.0244(7) 0.0226(7) 0.0050(5) 0.0035(5) -0.0021(5)
C8 0.0197(7) 0.0272(7) 0.0325(8) 0.0066(6) 0.0012(6) 0.0001(6)
C9 0.0298(10) 0.0339(10) 0.121(3) 0.0282(13) 0.0265(13) 0.0067(8)
C10 0.0397(13) 0.0308(11) 0.179(4) 0.0251(16) 0.0220(18) 0.0074(10)
C11 0.0451(13) 0.0383(11) 0.084(2) -0.0054(12) -0.0091(13) 0.0181(10)
C12 0.0501(13) 0.0614(14) 0.0354(11) 0.0101(10) 0.0128(10) 0.0265(11)
N13 0.0374(9) 0.0436(9) 0.0374(9) 0.0139(7) 0.0160(7) 0.0134(7)
N14 0.0199(6) 0.0188(5) 0.0203(6) 0.0001(4) 0.0046(5) -0.0040(4)
N15 0.0200(6) 0.0166(5) 0.0250(6) -0.0004(4) 0.0043(5) -0.0022(4)
C16 0.0198(6) 0.0182(6) 0.0158(6) -0.0020(5) 0.0057(5) -0.0040(5)
C17 0.0168(6) 0.0174(6) 0.0177(6) -0.0015(5) 0.0052(5) -0.0027(5)
C18 0.0201(7) 0.0182(6) 0.0319(8) 0.0005(6) 0.0067(6) 0.0008(5)
C19 0.0307(8) 0.0169(6) 0.0364(9) -0.0009(6) 0.0122(7) -0.0035(6)
C20 0.0269(8) 0.0282(8) 0.0324(8) -0.0043(6) 0.0107(7) -0.0114(6)
C21 0.0172(7) 0.0342(9) 0.0409(10) 0.0012(7) 0.0046(7) -0.0044(6)
C22 0.0190(7) 0.0229(7) 0.0295(8) 0.0031(6) 0.0035(6) 0.0017(5)
O23 0.0225(5) 0.0175(5) 0.0280(6) 0.0023(4) 0.0040(4) -0.0011(4)
N24 0.0229(6) 0.0167(5) 0.0189(5) -0.0024(4) 0.0076(5) -0.0027(4)
C25 0.0362(9) 0.0191(6) 0.0265(8) -0.0048(6) 0.0122(7) -0.0024(6)
C26 0.0458(10) 0.0271(8) 0.0289(8) -0.0115(6) 0.0182(8) -0.0041(7)
C27 0.0445(10) 0.0345(9) 0.0222(7) -0.0071(6) 0.0162(7) -0.0062(7)
C28 0.0263(8) 0.0262(7) 0.0181(7) -0.0013(5) 0.0076(6) -0.0037(6)
C29 0.0145(6) 0.0188(6) 0.0165(6) -0.0012(5) 0.0041(5) -0.0018(5)
C30 0.0155(6) 0.0157(6) 0.0178(6) 0.0007(5) 0.0052(5) 0.0004(4)
C31 0.0214(7) 0.0162(6) 0.0183(6) 0.0011(5) 0.0064(5) -0.0002(5)
C32 0.0307(8) 0.0193(7) 0.0314(8) 0.0014(6) 0.0154(7) 0.0033(6)
C33 0.0476(11) 0.0176(7) 0.0420(10) 0.0030(6) 0.0232(9) 0.0057(7)
C34 0.0513(12) 0.0178(7) 0.0445(10) 0.0028(7) 0.0247(9) -0.0046(7)
C35 0.0312(8) 0.0239(7) 0.0387(9) 0.0042(6) 0.0173(7) -0.0031(6)
N36 0.0232(6) 0.0199(6) 0.0285(7) 0.0028(5) 0.0120(5) -0.0002(5)
N37 0.0197(6) 0.0168(5) 0.0174(5) -0.0016(4) 0.0072(4) -0.0001(4)
N38 0.0249(6) 0.0163(5) 0.0190(6) -0.0013(4) 0.0105(5) 0.0009(4)
C39 0.0214(6) 0.0179(6) 0.0198(6) -0.0020(5) 0.0092(5) -0.0008(5)
C40 0.0227(7) 0.0178(6) 0.0177(6) -0.0009(5) 0.0076(5) 0.0036(5)
C41 0.0421(10) 0.0196(7) 0.0305(8) -0.0031(6) 0.0194(7) -0.0014(6)
C42 0.0544(12) 0.0247(8) 0.0400(10) -0.0126(7) 0.0227(9) -0.0062(8)
C43 0.0406(10) 0.0330(8) 0.0266(8) -0.0098(7) 0.0139(7) 0.0054(7)
C44 0.0318(8) 0.0336(8) 0.0228(7) -0.0012(6) 0.0139(6) 0.0042(7)
C45 0.0321(8) 0.0256(7) 0.0248(7) -0.0039(6) 0.0148(6) -0.0026(6)
O46 0.0427(7) 0.0171(5) 0.0288(6) -0.0033(4) 0.0225(5) -0.0065(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
Zn1 N1 2.2751(14) . ?
Zn1 N14 2.0861(13) . ?
Zn1 O23 2.1056(11) . ?
Zn1 N24 2.1812(13) . ?
Zn1 N37 2.1062(12) . ?
Zn1 O46 2.0551(11) . ?
N1 C2 1.336(2) . ?
N1 C6 1.345(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.390(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.377(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.394(2) . ?
C6 C7 1.483(2) . ?
C7 C8 1.492(2) . ?
C7 N14 1.296(2) . ?
C8 C9 1.384(3) . ?
C8 N13 1.336(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.386(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.360(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.365(4) . ?
C12 H12 0.9500 . ?
C12 N13 1.344(3) . ?
N14 N15 1.3621(17) . ?
N15 C16 1.3495(19) . ?
C16 C17 1.4916(19) . ?
C16 O23 1.2662(17) . ?
C17 C18 1.399(2) . ?
C17 C22 1.386(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.388(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.383(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.384(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.389(2) . ?
C22 H22 0.9500 . ?
N24 C25 1.3333(19) . ?
N24 C29 1.3541(18) . ?
C25 H25 0.9500 . ?
C25 C26 1.382(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.383(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.391(2) . ?
C28 H28 0.9500 . ?
C28 C29 1.390(2) . ?
C29 C30 1.4906(19) . ?
C30 C31 1.4876(19) . ?
C30 N37 1.2952(18) . ?
C31 C32 1.391(2) . ?
C31 N36 1.3445(19) . ?
C32 H32 0.9500 . ?
C32 C33 1.389(2) . ?
C33 H33 0.9500 . ?
C33 C34 1.380(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.388(2) . ?
C35 H35 0.9500 . ?
C35 N36 1.333(2) . ?
N37 N38 1.3709(16) . ?
N38 C39 1.3414(18) . ?
C39 C40 1.4803(19) . ?
C39 O46 1.2734(17) . ?
C40 C41 1.390(2) . ?
C40 C45 1.385(2) . ?
C41 H41 0.9500 . ?
C41 C42 1.387(2) . ?
C42 H42 0.9500 . ?
C42 C43 1.381(3) . ?
C43 H43 0.9500 . ?
C43 C44 1.379(3) . ?
C44 H44 0.9500 . ?
C44 C45 1.390(2) . ?
C45 H45 0.9500 . ?
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
N14 Zn1 N1 73.46(5) . . ?
N14 Zn1 O23 75.63(5) . . ?
N14 Zn1 N24 97.06(5) . . ?
N14 Zn1 N37 161.18(5) . . ?
O23 Zn1 N1 148.37(5) . . ?
O23 Zn1 N24 96.30(5) . . ?
O23 Zn1 N37 121.38(5) . . ?
N24 Zn1 N1 93.98(5) . . ?
N37 Zn1 N1 90.19(5) . . ?
N37 Zn1 N24 74.36(5) . . ?
O46 Zn1 N1 93.53(5) . . ?
O46 Zn1 N14 114.33(5) . . ?
O46 Zn1 O23 93.10(5) . . ?
O46 Zn1 N24 148.57(5) . . ?
O46 Zn1 N37 75.14(5) . . ?
C2 N1 Zn1 128.19(12) . . ?
C2 N1 C6 118.63(15) . . ?
C6 N1 Zn1 112.77(10) . . ?
N1 C2 H2 118.5 . . ?
N1 C2 C3 122.91(17) . . ?
C3 C2 H2 118.5 . . ?
C2 C3 H3 120.8 . . ?
C4 C3 C2 118.31(17) . . ?
C4 C3 H3 120.8 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.64(17) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 120.7 . . ?
C4 C5 C6 118.52(17) . . ?
C6 C5 H5 120.7 . . ?
N1 C6 C5 121.95(15) . . ?
N1 C6 C7 115.61(14) . . ?
C5 C6 C7 122.30(15) . . ?
C6 C7 C8 122.11(14) . . ?
N14 C7 C6 114.00(14) . . ?
N14 C7 C8 123.87(14) . . ?
C9 C8 C7 122.83(17) . . ?
N13 C8 C7 115.81(15) . . ?
N13 C8 C9 121.26(18) . . ?
C8 C9 H9 120.4 . . ?
C8 C9 C10 119.1(2) . . ?
C10 C9 H9 120.4 . . ?
C9 C10 H10 120.2 . . ?
C11 C10 C9 119.6(2) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 120.9 . . ?
C10 C11 C12 118.2(2) . . ?
C12 C11 H11 120.9 . . ?
C11 C12 H12 118.2 . . ?
N13 C12 C11 123.7(2) . . ?
N13 C12 H12 118.2 . . ?
C8 N13 C12 118.13(19) . . ?
C7 N14 Zn1 120.88(10) . . ?
C7 N14 N15 120.77(13) . . ?
N15 N14 Zn1 116.70(9) . . ?
C16 N15 N14 109.47(12) . . ?
N15 C16 C17 113.77(12) . . ?
O23 C16 N15 126.13(13) . . ?
O23 C16 C17 120.09(13) . . ?
C18 C17 C16 120.56(13) . . ?
C22 C17 C16 120.43(13) . . ?
C22 C17 C18 119.00(14) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 C17 120.39(15) . . ?
C19 C18 H18 119.8 . . ?
C18 C19 H19 119.9 . . ?
C20 C19 C18 120.20(15) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 120.2 . . ?
C19 C20 C21 119.57(15) . . ?
C21 C20 H20 120.2 . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C22 120.57(16) . . ?
C22 C21 H21 119.7 . . ?
C17 C22 C21 120.27(15) . . ?
C17 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C16 O23 Zn1 111.30(9) . . ?
C25 N24 Zn1 125.54(11) . . ?
C25 N24 C29 119.23(13) . . ?
C29 N24 Zn1 115.08(9) . . ?
N24 C25 H25 118.6 . . ?
N24 C25 C26 122.79(15) . . ?
C26 C25 H25 118.6 . . ?
C25 C26 H26 120.9 . . ?
C25 C26 C27 118.20(15) . . ?
C27 C26 H26 120.9 . . ?
C26 C27 H27 120.1 . . ?
C26 C27 C28 119.82(15) . . ?
C28 C27 H27 120.1 . . ?
C27 C28 H28 120.7 . . ?
C29 C28 C27 118.56(15) . . ?
C29 C28 H28 120.7 . . ?
N24 C29 C28 121.31(13) . . ?
N24 C29 C30 115.12(12) . . ?
C28 C29 C30 123.57(13) . . ?
C31 C30 C29 121.60(12) . . ?
N37 C30 C29 113.30(12) . . ?
N37 C30 C31 124.95(13) . . ?
C32 C31 C30 121.98(14) . . ?
N36 C31 C30 115.27(12) . . ?
N36 C31 C32 122.69(14) . . ?
C31 C32 H32 120.6 . . ?
C33 C32 C31 118.75(16) . . ?
C33 C32 H32 120.6 . . ?
C32 C33 H33 120.6 . . ?
C34 C33 C32 118.85(16) . . ?
C34 C33 H33 120.6 . . ?
C33 C34 H34 120.7 . . ?
C33 C34 C35 118.50(16) . . ?
C35 C34 H34 120.7 . . ?
C34 C35 H35 118.2 . . ?
N36 C35 C34 123.61(16) . . ?
N36 C35 H35 118.2 . . ?
C35 N36 C31 117.58(14) . . ?
C30 N37 Zn1 120.66(9) . . ?
C30 N37 N38 121.76(12) . . ?
N38 N37 Zn1 115.31(9) . . ?
C39 N38 N37 108.22(11) . . ?
N38 C39 C40 116.24(12) . . ?
O46 C39 N38 126.22(13) . . ?
O46 C39 C40 117.50(13) . . ?
C41 C40 C39 121.27(14) . . ?
C45 C40 C39 119.36(13) . . ?
C45 C40 C41 119.25(14) . . ?
C40 C41 H41 120.1 . . ?
C42 C41 C40 119.72(16) . . ?
C42 C41 H41 120.1 . . ?
C41 C42 H42 119.7 . . ?
C43 C42 C41 120.70(17) . . ?
C43 C42 H42 119.7 . . ?
C42 C43 H43 120.1 . . ?
C44 C43 C42 119.84(16) . . ?
C44 C43 H43 120.1 . . ?
C43 C44 H44 120.2 . . ?
C43 C44 C45 119.67(16) . . ?
C45 C44 H44 120.2 . . ?
C40 C45 C44 120.79(15) . . ?
C40 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
C39 O46 Zn1 111.49(10) . . ?
_iucr_refine_instructions_details
;
TITL DT_ZnNO3_1to1_0ma_a.res in C2/c
dt_znno3_1to1_0ma_a.res
created by SHELXL-2017/1 at 16:00:04 on 01-Aug-2019
CELL 0.71073 18.2863 11.3902 30.447 90 106.745 90
ZERR 8 0.0011 0.0006 0.002 0 0.002 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H N O Zn
UNIT 288 208 64 16 8
L.S. 10
PLAN 20
SIZE 0.1 0.24 0.43
TEMP -123.17
BOND $H
LIST 6
fmap 2
acta
REM
REM
REM
WGHT 0.043500 7.338400
FVAR 0.11101
ZN1 5 0.323931 0.658054 0.617848 11.00000 0.02223 0.01360 =
0.01882 -0.00096 0.00817 -0.00263
N1 3 0.447644 0.686192 0.659514 11.00000 0.02205 0.02518 =
0.02463 -0.00062 0.00427 -0.00411
C2 1 0.482928 0.787271 0.674776 11.00000 0.02784 0.02709 =
0.03599 -0.00471 0.00306 -0.00530
AFIX 43
H2 2 0.457110 0.858781 0.664192 11.00000 -1.20000
AFIX 0
C3 1 0.555717 0.792432 0.705443 11.00000 0.02996 0.03453 =
0.04674 -0.01062 -0.00159 -0.01178
AFIX 43
H3 2 0.579167 0.865777 0.715730 11.00000 -1.20000
AFIX 0
C4 1 0.592987 0.688544 0.720541 11.00000 0.02738 0.04292 =
0.04534 -0.00431 -0.00817 -0.00833
AFIX 43
H4 2 0.642315 0.689310 0.742062 11.00000 -1.20000
AFIX 0
C5 1 0.558076 0.582610 0.704138 11.00000 0.02416 0.03331 =
0.03645 0.00189 -0.00299 -0.00329
AFIX 43
H5 2 0.583564 0.510200 0.713537 11.00000 -1.20000
AFIX 0
C6 1 0.484831 0.584902 0.673585 11.00000 0.02072 0.02700 =
0.02358 0.00100 0.00377 -0.00416
C7 1 0.440673 0.476261 0.657196 11.00000 0.01973 0.02444 =
0.02256 0.00503 0.00349 -0.00207
C8 1 0.478350 0.359672 0.658438 11.00000 0.01970 0.02718 =
0.03254 0.00660 0.00118 0.00012
C9 1 0.448979 0.257454 0.671219 11.00000 0.02980 0.03392 =
0.12126 0.02817 0.02650 0.00668
AFIX 43
H9 2 0.405755 0.260096 0.682570 11.00000 -1.20000
AFIX 0
C10 1 0.483458 0.151188 0.667239 11.00000 0.03967 0.03081 =
0.17890 0.02510 0.02202 0.00743
AFIX 43
H10 2 0.463470 0.080071 0.675339 11.00000 -1.20000
AFIX 0
C11 1 0.546067 0.149377 0.651671 11.00000 0.04514 0.03834 =
0.08428 -0.00541 -0.00909 0.01811
AFIX 43
H11 2 0.569979 0.077375 0.648137 11.00000 -1.20000
AFIX 0
C12 1 0.573612 0.253893 0.641259 11.00000 0.05010 0.06136 =
0.03536 0.01008 0.01285 0.02653
AFIX 43
H12 2 0.618574 0.252911 0.631582 11.00000 -1.20000
AFIX 0
N13 3 0.540684 0.358114 0.643931 11.00000 0.03740 0.04362 =
0.03741 0.01389 0.01596 0.01339
N14 3 0.367722 0.492906 0.641026 11.00000 0.01991 0.01883 =
0.02034 0.00012 0.00458 -0.00401
N15 3 0.318950 0.400273 0.628905 11.00000 0.01999 0.01658 =
0.02501 -0.00044 0.00434 -0.00221
C16 1 0.247387 0.440276 0.609686 11.00000 0.01980 0.01816 =
0.01580 -0.00201 0.00568 -0.00397
C17 1 0.187433 0.347839 0.603206 11.00000 0.01684 0.01740 =
0.01773 -0.00148 0.00523 -0.00266
C18 1 0.207391 0.231620 0.616148 11.00000 0.02009 0.01822 =
0.03189 0.00051 0.00668 0.00082
AFIX 43
H18 2 0.259644 0.210870 0.628380 11.00000 -1.20000
AFIX 0
C19 1 0.151289 0.146458 0.611219 11.00000 0.03066 0.01686 =
0.03636 -0.00086 0.01218 -0.00349
AFIX 43
H19 2 0.165276 0.067816 0.620219 11.00000 -1.20000
AFIX 0
C20 1 0.075089 0.175763 0.593243 11.00000 0.02692 0.02818 =
0.03236 -0.00428 0.01066 -0.01137
AFIX 43
H20 2 0.036709 0.117379 0.589652 11.00000 -1.20000
AFIX 0
C21 1 0.055111 0.290707 0.580521 11.00000 0.01720 0.03421 =
0.04089 0.00123 0.00462 -0.00443
AFIX 43
H21 2 0.002786 0.311166 0.568412 11.00000 -1.20000
AFIX 0
C22 1 0.110930 0.376417 0.585308 11.00000 0.01896 0.02290 =
0.02947 0.00309 0.00351 0.00170
AFIX 43
H22 2 0.096596 0.454929 0.576276 11.00000 -1.20000
AFIX 0
O23 4 0.228669 0.545515 0.598476 11.00000 0.02253 0.01750 =
0.02798 0.00228 0.00400 -0.00111
N24 3 0.349995 0.653242 0.552330 11.00000 0.02288 0.01670 =
0.01887 -0.00242 0.00765 -0.00274
C25 1 0.361134 0.556374 0.530520 11.00000 0.03619 0.01906 =
0.02646 -0.00476 0.01216 -0.00236
AFIX 43
H25 2 0.361365 0.482644 0.545146 11.00000 -1.20000
AFIX 0
C26 1 0.372356 0.558672 0.487542 11.00000 0.04580 0.02709 =
0.02890 -0.01148 0.01818 -0.00406
AFIX 43
H26 2 0.381922 0.488435 0.473294 11.00000 -1.20000
AFIX 0
C27 1 0.369285 0.666005 0.465829 11.00000 0.04455 0.03446 =
0.02223 -0.00708 0.01621 -0.00618
AFIX 43
H27 2 0.375303 0.670054 0.435898 11.00000 -1.20000
AFIX 0
C28 1 0.357363 0.767965 0.487934 11.00000 0.02634 0.02622 =
0.01807 -0.00126 0.00764 -0.00374
AFIX 43
H28 2 0.354727 0.842202 0.473338 11.00000 -1.20000
AFIX 0
C29 1 0.349387 0.758909 0.531849 11.00000 0.01445 0.01878 =
0.01648 -0.00125 0.00414 -0.00183
C30 1 0.338888 0.861982 0.559588 11.00000 0.01553 0.01571 =
0.01780 0.00066 0.00515 0.00044
C31 1 0.357659 0.983247 0.548259 11.00000 0.02140 0.01619 =
0.01829 0.00113 0.00638 -0.00022
C32 1 0.314068 1.079645 0.553280 11.00000 0.03067 0.01927 =
0.03144 0.00136 0.01544 0.00332
AFIX 43
H32 2 0.269019 1.069515 0.562453 11.00000 -1.20000
AFIX 0
C33 1 0.337639 1.191001 0.544631 11.00000 0.04761 0.01761 =
0.04198 0.00304 0.02325 0.00567
AFIX 43
H33 2 0.308818 1.258382 0.547606 11.00000 -1.20000
AFIX 0
C34 1 0.403669 1.202066 0.531638 11.00000 0.05132 0.01785 =
0.04452 0.00280 0.02472 -0.00457
AFIX 43
H34 2 0.421614 1.277174 0.525937 11.00000 -1.20000
AFIX 0
C35 1 0.443252 1.100982 0.527091 11.00000 0.03124 0.02386 =
0.03872 0.00416 0.01732 -0.00310
AFIX 43
H35 2 0.488516 1.109012 0.517988 11.00000 -1.20000
AFIX 0
N36 3 0.421244 0.993233 0.534796 11.00000 0.02324 0.01988 =
0.02850 0.00284 0.01197 -0.00018
N37 3 0.317311 0.833440 0.595120 11.00000 0.01966 0.01681 =
0.01743 -0.00163 0.00715 -0.00014
N38 3 0.309282 0.915610 0.626304 11.00000 0.02486 0.01629 =
0.01899 -0.00133 0.01046 0.00088
C39 1 0.291264 0.859595 0.660530 11.00000 0.02142 0.01793 =
0.01980 -0.00197 0.00920 -0.00079
C40 1 0.285282 0.933340 0.699379 11.00000 0.02271 0.01783 =
0.01769 -0.00087 0.00755 0.00359
C41 1 0.319700 1.043200 0.707507 11.00000 0.04209 0.01963 =
0.03049 -0.00307 0.01944 -0.00137
AFIX 43
H41 2 0.343377 1.075779 0.686314 11.00000 -1.20000
AFIX 0
C42 1 0.319315 1.105016 0.746686 11.00000 0.05436 0.02471 =
0.03997 -0.01263 0.02268 -0.00619
AFIX 43
H42 2 0.344379 1.178843 0.752747 11.00000 -1.20000
AFIX 0
C43 1 0.282869 1.060364 0.776991 11.00000 0.04063 0.03304 =
0.02661 -0.00977 0.01392 0.00536
AFIX 43
H43 2 0.282257 1.103899 0.803497 11.00000 -1.20000
AFIX 0
C44 1 0.247368 0.952406 0.768668 11.00000 0.03182 0.03364 =
0.02276 -0.00122 0.01387 0.00420
AFIX 43
H44 2 0.222037 0.921467 0.789331 11.00000 -1.20000
AFIX 0
C45 1 0.248844 0.889106 0.729894 11.00000 0.03214 0.02563 =
0.02483 -0.00394 0.01477 -0.00264
AFIX 43
H45 2 0.224565 0.814616 0.724264 11.00000 -1.20000
AFIX 0
O46 4 0.281405 0.749471 0.663291 11.00000 0.04265 0.01712 =
0.02883 -0.00326 0.02249 -0.00651
HKLF 4
REM DT_ZnNO3_1to1_0ma_a.res in C2/c
REM R1 = 0.0341 for 7283 Fo > 4sig(Fo) and 0.0447 for all 8546 data
REM 424 parameters refined using 0 restraints
END
WGHT 0.0435 7.3384
REM Highest difference peak 0.600, deepest hole -0.377, 1-sigma level 0.056
Q1 1 0.1810 0.5640 0.5949 11.00000 0.05 0.60
Q2 1 0.4997 0.1807 0.7026 11.00000 0.05 0.48
Q3 1 0.4587 0.5309 0.6709 11.00000 0.05 0.48
Q4 1 0.4996 0.3360 0.6332 11.00000 0.05 0.48
Q5 1 0.4678 0.2974 0.7014 11.00000 0.05 0.48
Q6 1 0.1499 0.3564 0.5963 11.00000 0.05 0.40
Q7 1 0.3607 0.5594 0.5066 11.00000 0.05 0.39
Q8 1 0.3383 0.8141 0.5424 11.00000 0.05 0.39
Q9 1 0.2890 0.8974 0.6823 11.00000 0.05 0.38
Q10 1 0.5352 0.1610 0.6782 11.00000 0.05 0.38
Q11 1 0.2194 0.4897 0.6084 11.00000 0.05 0.38
Q12 1 0.1134 0.1618 0.6029 11.00000 0.05 0.38
Q13 1 0.0703 0.2290 0.5804 11.00000 0.05 0.36
Q14 1 0.5649 0.6363 0.7240 11.00000 0.05 0.35
Q15 1 0.2140 0.3908 0.6062 11.00000 0.05 0.35
Q16 1 0.3435 0.7599 0.5076 11.00000 0.05 0.35
Q17 1 0.4679 0.7313 0.6815 11.00000 0.05 0.34
Q18 1 0.3474 0.9197 0.5536 11.00000 0.05 0.33
Q19 1 0.3717 0.6146 0.4787 11.00000 0.05 0.32
Q20 1 0.3517 0.6025 0.5387 11.00000 0.05 0.32
REM The information below was added by Olex2.
REM
REM R1 = 0.0341 for 7283 Fo > 4sig(Fo) and 0.0447 for all 85133 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.60, deepest hole -0.38
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0447
REM R1_gt = 0.0341
REM wR_ref = 0.0880
REM GOOF = 1.018
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 85133
REM Reflections_gt = 7283
REM Parameters = n/a
REM Hole = -0.38
REM Peak = 0.60
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_Ligand_HL2
_database_code_depnum_ccdc_archive 'CCDC 1993510'
loop_
_audit_author_name
_audit_author_address
'Krishna K. Damodaran'
;University of Iceland
Iceland
;
_audit_update_record
;
2020-03-29 deposited with the CCDC. 2020-12-09 downloaded from the CCDC.
;
_audit_creation_date 2019-08-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C18 H15 N5 O'
_chemical_formula_sum 'C18 H15 N5 O'
_chemical_formula_weight 317.35
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
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 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 3.84640(10)
_cell_length_b 11.0679(3)
_cell_length_c 35.2718(9)
_cell_angle_alpha 90
_cell_angle_beta 91.8120(10)
_cell_angle_gamma 90
_cell_volume 1500.83(7)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9993
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 78.36
_cell_measurement_theta_min 2.51
_shelx_estimated_absorpt_T_max 0.978
_shelx_estimated_absorpt_T_min 0.807
_exptl_absorpt_coefficient_mu 0.745
_exptl_absorpt_correction_T_max 0.7542
_exptl_absorpt_correction_T_min 0.6174
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1232 before and 0.0727 after correction. The Ratio of minimum to maximum transmission is 0.8186. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.404
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 664
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_min 0.03
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0639
_diffrn_reflns_av_unetI/netI 0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max 4
_diffrn_reflns_limit_h_min -4
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 44
_diffrn_reflns_limit_l_min -44
_diffrn_reflns_number 30671
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 79.080
_diffrn_reflns_theta_min 2.507
_diffrn_ambient_temperature 149.97
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2729
_reflns_number_total 3206
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max 0.304
_refine_diff_density_min -0.327
_refine_diff_density_rms 0.053
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 225
_refine_ls_number_reflns 3206
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0562
_refine_ls_R_factor_gt 0.0460
_refine_ls_restrained_S_all 1.062
_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^)+(0.0574P)^2^+0.5908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1096
_refine_ls_wR_factor_ref 0.1155
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.2667(4) 0.64639(11) 0.47278(4) 0.0243(3) Uani 1 1 d . . . . .
C2 C 0.1951(4) 0.63311(14) 0.50942(4) 0.0265(3) Uani 1 1 d . . . . .
H2 H 0.264676 0.560280 0.521729 0.032 Uiso 1 1 calc R . . . .
C3 C 0.0253(4) 0.71941(14) 0.53046(4) 0.0268(3) Uani 1 1 d . . . . .
H3 H -0.015310 0.706945 0.556603 0.032 Uiso 1 1 calc R . . . .
C4 C -0.0838(4) 0.82464(14) 0.51224(4) 0.0265(3) Uani 1 1 d . . . . .
H4 H -0.207745 0.884654 0.525537 0.032 Uiso 1 1 calc R . . . .
C5 C -0.0094(4) 0.84091(13) 0.47441(4) 0.0241(3) Uani 1 1 d . . . . .
H5 H -0.080073 0.912501 0.461456 0.029 Uiso 1 1 calc R . . . .
C6 C 0.1705(4) 0.75083(13) 0.45561(4) 0.0218(3) Uani 1 1 d . . . . .
C7 C 0.2633(4) 0.76620(13) 0.41525(4) 0.0226(3) Uani 1 1 d . . . . .
C8 C 0.2392(4) 0.88791(13) 0.39687(4) 0.0223(3) Uani 1 1 d . . . . .
C9 C 0.0880(4) 0.89944(14) 0.36061(4) 0.0265(3) Uani 1 1 d . . . . .
H9 H -0.013902 0.831518 0.348097 0.032 Uiso 1 1 calc R . . . .
C10 C 0.0885(4) 1.01127(15) 0.34315(4) 0.0303(4) Uani 1 1 d . . . . .
H10 H -0.014912 1.021662 0.318552 0.036 Uiso 1 1 calc R . . . .
C11 C 0.2426(4) 1.10792(15) 0.36215(5) 0.0303(4) Uani 1 1 d . . . . .
H11 H 0.250314 1.185562 0.350721 0.036 Uiso 1 1 calc R . . . .
C12 C 0.3852(4) 1.08866(14) 0.39822(4) 0.0271(3) Uani 1 1 d . . . . .
H12 H 0.489590 1.155272 0.411188 0.033 Uiso 1 1 calc R . . . .
N13 N 0.3841(4) 0.98135(11) 0.41586(4) 0.0243(3) Uani 1 1 d . . . . .
N14 N 0.3717(4) 0.68446(11) 0.39232(3) 0.0250(3) Uani 1 1 d . . . . .
N15 N 0.4127(4) 0.56769(12) 0.40363(4) 0.0286(3) Uani 1 1 d . . . . .
H15 H 0.374(5) 0.5496(18) 0.4282(6) 0.033(5) Uiso 1 1 d . . . . .
C16 C 0.5519(4) 0.48490(14) 0.37877(4) 0.0265(3) Uani 1 1 d . . . . .
O17 O 0.5956(4) 0.38011(10) 0.38832(3) 0.0345(3) Uani 1 1 d . . . . .
N18 N 0.6288(4) 0.53479(12) 0.34479(4) 0.0275(3) Uani 1 1 d . . . . .
H18 H 0.589(6) 0.612(2) 0.3428(6) 0.034(5) Uiso 1 1 d . . . . .
C19 C 0.7676(4) 0.47929(14) 0.31288(4) 0.0250(3) Uani 1 1 d . . . . .
C20 C 0.8519(5) 0.55453(15) 0.28282(5) 0.0300(3) Uani 1 1 d . . . . .
H20 H 0.818744 0.639302 0.284874 0.036 Uiso 1 1 calc R . . . .
C21 C 0.9837(5) 0.50651(16) 0.24999(5) 0.0324(4) Uani 1 1 d . . . . .
H21 H 1.037892 0.558415 0.229554 0.039 Uiso 1 1 calc R . . . .
C22 C 1.0369(5) 0.38312(16) 0.24677(5) 0.0333(4) Uani 1 1 d . . . . .
H22 H 1.127468 0.349988 0.224283 0.040 Uiso 1 1 calc R . . . .
C23 C 0.9559(5) 0.30883(15) 0.27687(5) 0.0329(4) Uani 1 1 d . . . . .
H23 H 0.992968 0.224247 0.274844 0.039 Uiso 1 1 calc R . . . .
C24 C 0.8218(4) 0.35541(14) 0.30992(4) 0.0282(3) Uani 1 1 d . . . . .
H24 H 0.767700 0.303235 0.330295 0.034 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0298(7) 0.0204(6) 0.0227(6) 0.0010(5) 0.0000(5) -0.0009(5)
C2 0.0330(9) 0.0229(7) 0.0235(7) 0.0042(5) -0.0018(6) -0.0022(6)
C3 0.0316(8) 0.0285(8) 0.0202(7) 0.0017(6) 0.0009(6) -0.0053(6)
C4 0.0296(8) 0.0257(7) 0.0245(7) -0.0038(6) 0.0031(6) -0.0017(6)
C5 0.0274(8) 0.0206(7) 0.0242(7) 0.0022(5) 0.0000(6) -0.0007(6)
C6 0.0242(7) 0.0203(6) 0.0207(7) 0.0005(5) -0.0002(5) -0.0035(5)
C7 0.0259(8) 0.0208(7) 0.0212(7) 0.0005(5) -0.0002(5) -0.0001(5)
C8 0.0252(7) 0.0210(7) 0.0210(7) 0.0014(5) 0.0041(5) 0.0024(5)
C9 0.0285(8) 0.0277(8) 0.0234(7) 0.0000(6) 0.0022(6) 0.0006(6)
C10 0.0314(9) 0.0360(9) 0.0236(7) 0.0080(6) 0.0015(6) 0.0051(7)
C11 0.0334(9) 0.0250(8) 0.0329(8) 0.0104(6) 0.0068(6) 0.0040(6)
C12 0.0317(9) 0.0205(7) 0.0295(7) 0.0001(6) 0.0065(6) 0.0011(6)
N13 0.0296(7) 0.0206(6) 0.0231(6) 0.0004(5) 0.0035(5) 0.0017(5)
N14 0.0325(7) 0.0190(6) 0.0235(6) 0.0015(5) 0.0008(5) 0.0012(5)
N15 0.0450(8) 0.0193(6) 0.0217(6) 0.0014(5) 0.0050(5) 0.0027(5)
C16 0.0349(9) 0.0210(7) 0.0233(7) -0.0003(5) -0.0019(6) 0.0008(6)
O17 0.0565(8) 0.0204(5) 0.0269(6) 0.0015(4) 0.0031(5) 0.0056(5)
N18 0.0400(8) 0.0186(6) 0.0239(6) 0.0005(5) 0.0022(5) 0.0042(5)
C19 0.0259(8) 0.0258(7) 0.0231(7) -0.0022(6) -0.0015(6) 0.0016(6)
C20 0.0359(9) 0.0262(8) 0.0277(8) -0.0004(6) -0.0006(6) -0.0006(6)
C21 0.0355(9) 0.0361(9) 0.0258(8) 0.0019(6) 0.0024(6) -0.0033(7)
C22 0.0321(9) 0.0407(9) 0.0270(8) -0.0069(7) 0.0027(6) 0.0024(7)
C23 0.0362(9) 0.0281(8) 0.0344(8) -0.0057(6) 0.0009(7) 0.0047(7)
C24 0.0322(9) 0.0255(8) 0.0268(7) 0.0001(6) 0.0004(6) 0.0025(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C2 1.338(2) . ?
N1 C6 1.3512(19) . ?
C2 H2 0.9500 . ?
C2 C3 1.386(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.389(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.385(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(2) . ?
C6 C7 1.488(2) . ?
C7 C8 1.4966(19) . ?
C7 N14 1.2916(19) . ?
C8 C9 1.394(2) . ?
C8 N13 1.344(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.383(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.385(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.386(2) . ?
C12 H12 0.9500 . ?
C12 N13 1.3408(19) . ?
N14 N15 1.3603(18) . ?
N15 H15 0.91(2) . ?
N15 C16 1.387(2) . ?
C16 O17 1.2180(19) . ?
C16 N18 1.361(2) . ?
N18 H18 0.87(2) . ?
N18 C19 1.402(2) . ?
C19 C20 1.395(2) . ?
C19 C24 1.391(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.385(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.386(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.386(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.389(2) . ?
C24 H24 0.9500 . ?
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
C2 N1 C6 117.71(13) . . ?
N1 C2 H2 118.1 . . ?
N1 C2 C3 123.81(14) . . ?
C3 C2 H2 118.1 . . ?
C2 C3 H3 121.0 . . ?
C2 C3 C4 118.08(14) . . ?
C4 C3 H3 121.0 . . ?
C3 C4 H4 120.5 . . ?
C5 C4 C3 119.09(14) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 H5 120.5 . . ?
C4 C5 C6 119.09(14) . . ?
C6 C5 H5 120.5 . . ?
N1 C6 C5 122.14(13) . . ?
N1 C6 C7 117.12(13) . . ?
C5 C6 C7 120.74(13) . . ?
C6 C7 C8 120.26(12) . . ?
N14 C7 C6 127.66(13) . . ?
N14 C7 C8 112.08(12) . . ?
C9 C8 C7 119.88(13) . . ?
N13 C8 C7 117.24(13) . . ?
N13 C8 C9 122.78(13) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 C8 118.96(15) . . ?
C10 C9 H9 120.5 . . ?
C9 C10 H10 120.6 . . ?
C9 C10 C11 118.85(15) . . ?
C11 C10 H10 120.6 . . ?
C10 C11 H11 120.8 . . ?
C10 C11 C12 118.42(14) . . ?
C12 C11 H11 120.8 . . ?
C11 C12 H12 118.1 . . ?
N13 C12 C11 123.73(15) . . ?
N13 C12 H12 118.1 . . ?
C12 N13 C8 117.24(13) . . ?
C7 N14 N15 121.23(13) . . ?
N14 N15 H15 118.0(13) . . ?
N14 N15 C16 119.04(13) . . ?
C16 N15 H15 122.5(13) . . ?
O17 C16 N15 120.45(14) . . ?
O17 C16 N18 126.72(14) . . ?
N18 C16 N15 112.82(13) . . ?
C16 N18 H18 115.2(14) . . ?
C16 N18 C19 128.91(13) . . ?
C19 N18 H18 115.9(14) . . ?
C20 C19 N18 116.89(14) . . ?
C24 C19 N18 123.61(14) . . ?
C24 C19 C20 119.50(14) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 C19 120.45(15) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 H21 119.8 . . ?
C20 C21 C22 120.37(15) . . ?
C22 C21 H21 119.8 . . ?
C21 C22 H22 120.5 . . ?
C23 C22 C21 118.98(15) . . ?
C23 C22 H22 120.5 . . ?
C22 C23 H23 119.3 . . ?
C22 C23 C24 121.41(16) . . ?
C24 C23 H23 119.3 . . ?
C19 C24 H24 120.4 . . ?
C23 C24 C19 119.29(15) . . ?
C23 C24 H24 120.4 . . ?
_iucr_refine_instructions_details
;
TITL cu_DT_ZnSO4L1_0m_a.res in P2(1)/n
cu_dt_znso4l1_0m_a.res
created by SHELXL-2017/1 at 17:13:50 on 07-Aug-2019
REM Old TITL cu_DT_ZnSO4L1_0m in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.113, Rweak 0.007, Alpha 0.022, Orientation as input
REM Formula found by SHELXT: C18 N5 O
REM #####
CELL 1.54178 3.8464 11.0679 35.2718 90 91.812 90
ZERR 4 0.0001 0.0003 0.0009 0 0.001 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 72 60 20 4
L.S. 10
PLAN 20
SIZE 0.03 0.04 0.3
TEMP -123.18
BOND $H
LIST 6
fmap 2
acta
REM
REM
REM
WGHT 0.057400 0.590800
FVAR 0.53857
N1 3 0.266654 0.646388 0.472778 11.00000 0.02976 0.02045 =
0.02274 0.00105 0.00004 -0.00087
C2 1 0.195062 0.633109 0.509422 11.00000 0.03298 0.02294 =
0.02352 0.00423 -0.00183 -0.00224
AFIX 43
H2 2 0.264676 0.560280 0.521729 11.00000 -1.20000
AFIX 0
C3 1 0.025288 0.719408 0.530465 11.00000 0.03160 0.02853 =
0.02019 0.00167 0.00090 -0.00527
AFIX 43
H3 2 -0.015310 0.706945 0.556603 11.00000 -1.20000
AFIX 0
C4 1 -0.083803 0.824644 0.512241 11.00000 0.02961 0.02568 =
0.02447 -0.00377 0.00314 -0.00173
AFIX 43
H4 2 -0.207745 0.884654 0.525537 11.00000 -1.20000
AFIX 0
C5 1 -0.009405 0.840911 0.474406 11.00000 0.02740 0.02063 =
0.02424 0.00221 0.00003 -0.00067
AFIX 43
H5 2 -0.080073 0.912501 0.461456 11.00000 -1.20000
AFIX 0
C6 1 0.170479 0.750834 0.455610 11.00000 0.02420 0.02031 =
0.02073 0.00054 -0.00017 -0.00345
C7 1 0.263280 0.766201 0.415253 11.00000 0.02593 0.02075 =
0.02117 0.00050 -0.00023 -0.00010
C8 1 0.239185 0.887909 0.396866 11.00000 0.02518 0.02100 =
0.02097 0.00144 0.00412 0.00241
C9 1 0.087960 0.899436 0.360612 11.00000 0.02850 0.02774 =
0.02339 -0.00002 0.00225 0.00059
AFIX 43
H9 2 -0.013902 0.831518 0.348097 11.00000 -1.20000
AFIX 0
C10 1 0.088535 1.011274 0.343150 11.00000 0.03142 0.03597 =
0.02357 0.00803 0.00149 0.00510
AFIX 43
H10 2 -0.014912 1.021662 0.318552 11.00000 -1.20000
AFIX 0
C11 1 0.242582 1.107922 0.362148 11.00000 0.03339 0.02501 =
0.03292 0.01038 0.00680 0.00401
AFIX 43
H11 2 0.250314 1.185562 0.350721 11.00000 -1.20000
AFIX 0
C12 1 0.385158 1.088655 0.398222 11.00000 0.03173 0.02045 =
0.02955 0.00014 0.00653 0.00107
AFIX 43
H12 2 0.489590 1.155272 0.411188 11.00000 -1.20000
AFIX 0
N13 3 0.384082 0.981352 0.415862 11.00000 0.02958 0.02056 =
0.02307 0.00039 0.00350 0.00174
N14 3 0.371705 0.684457 0.392318 11.00000 0.03252 0.01904 =
0.02348 0.00152 0.00082 0.00123
N15 3 0.412719 0.567689 0.403635 11.00000 0.04501 0.01926 =
0.02171 0.00142 0.00498 0.00267
H15 2 0.374083 0.549643 0.428226 11.00000 0.03309
C16 1 0.551865 0.484904 0.378771 11.00000 0.03489 0.02102 =
0.02327 -0.00028 -0.00194 0.00076
O17 4 0.595626 0.380109 0.388321 11.00000 0.05650 0.02036 =
0.02688 0.00152 0.00314 0.00558
N18 3 0.628838 0.534786 0.344791 11.00000 0.03995 0.01863 =
0.02395 0.00047 0.00220 0.00425
H18 2 0.589072 0.612082 0.342828 11.00000 0.03370
C19 1 0.767594 0.479294 0.312881 11.00000 0.02586 0.02578 =
0.02311 -0.00222 -0.00154 0.00157
C20 1 0.851920 0.554527 0.282816 11.00000 0.03592 0.02623 =
0.02770 -0.00043 -0.00060 -0.00064
AFIX 43
H20 2 0.818744 0.639302 0.284874 11.00000 -1.20000
AFIX 0
C21 1 0.983674 0.506505 0.249987 11.00000 0.03548 0.03606 =
0.02578 0.00193 0.00239 -0.00334
AFIX 43
H21 2 1.037892 0.558415 0.229554 11.00000 -1.20000
AFIX 0
C22 1 1.036894 0.383123 0.246771 11.00000 0.03214 0.04073 =
0.02702 -0.00693 0.00273 0.00236
AFIX 43
H22 2 1.127468 0.349988 0.224283 11.00000 -1.20000
AFIX 0
C23 1 0.955939 0.308835 0.276866 11.00000 0.03618 0.02815 =
0.03437 -0.00573 0.00092 0.00470
AFIX 43
H23 2 0.992968 0.224247 0.274844 11.00000 -1.20000
AFIX 0
C24 1 0.821819 0.355409 0.309925 11.00000 0.03223 0.02553 =
0.02682 0.00005 0.00036 0.00253
AFIX 43
H24 2 0.767700 0.303235 0.330295 11.00000 -1.20000
AFIX 0
HKLF 4
REM cu_DT_ZnSO4L1_0m_a.res in P2(1)/n
REM R1 = 0.0460 for 2729 Fo > 4sig(Fo) and 0.0562 for all 3206 data
REM 225 parameters refined using 0 restraints
END
WGHT 0.0562 0.6006
REM Highest difference peak 0.304, deepest hole -0.327, 1-sigma level 0.053
Q1 1 0.2404 0.7633 0.4366 11.00000 0.05 0.30
Q2 1 0.2563 0.8265 0.4082 11.00000 0.05 0.24
Q3 1 0.3433 0.5945 0.4589 11.00000 0.05 0.21
Q4 1 0.4289 0.6000 0.3409 11.00000 0.05 0.19
Q5 1 -0.0006 0.7835 0.4630 11.00000 0.05 0.18
Q6 1 0.1674 0.8135 0.4655 11.00000 0.05 0.18
Q7 1 0.1079 0.9005 0.3818 11.00000 0.05 0.17
Q8 1 0.8082 0.4183 0.3120 11.00000 0.05 0.17
Q9 1 0.0427 0.8478 0.4963 11.00000 0.05 0.17
Q10 1 0.8248 0.3341 0.2910 11.00000 0.05 0.17
Q11 1 0.3892 0.9874 0.4416 11.00000 0.05 0.16
Q12 1 0.3462 0.7003 0.3666 11.00000 0.05 0.16
Q13 1 0.6749 0.6619 0.2935 11.00000 0.05 0.16
Q14 1 0.0008 0.7740 0.5230 11.00000 0.05 0.15
Q15 1 0.3897 0.4440 0.2883 11.00000 0.05 0.15
Q16 1 0.1650 0.6882 0.5214 11.00000 0.05 0.15
Q17 1 0.2509 0.8832 0.3754 11.00000 0.05 0.14
Q18 1 0.8750 0.4402 0.2444 11.00000 0.05 0.14
Q19 1 -0.2102 0.9398 0.2906 11.00000 0.05 0.14
Q20 1 -0.2209 0.8235 0.3236 11.00000 0.05 0.14
REM The information below was added by Olex2.
REM
REM R1 = 0.0460 for 2729 Fo > 4sig(Fo) and 0.0562 for all 31445 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.30, deepest hole -0.33
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0562
REM R1_gt = 0.0460
REM wR_ref = 0.1155
REM GOOF = 1.062
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 31445
REM Reflections_gt = 2729
REM Parameters = n/a
REM Hole = -0.33
REM Peak = 0.30
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_mo_Complex_7
_database_code_depnum_ccdc_archive 'CCDC 1993509'
loop_
_audit_author_name
_audit_author_address
'Krishna K. Damodaran'
;University of Iceland
Iceland
;
_audit_update_record
;
2020-03-29 deposited with the CCDC. 2020-12-09 downloaded from the CCDC.
;
_audit_creation_date 2019-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C18 H15 Cd Cl2 N5 O'
_chemical_formula_sum 'C18 H15 Cd Cl2 N5 O'
_chemical_formula_weight 500.65
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 8.1129(5)
_cell_length_b 14.5881(8)
_cell_length_c 15.9877(9)
_cell_angle_alpha 90
_cell_angle_beta 93.220(2)
_cell_angle_gamma 90
_cell_volume 1889.19(19)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9849
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 31.57
_cell_measurement_theta_min 2.88
_shelx_estimated_absorpt_T_max 0.845
_shelx_estimated_absorpt_T_min 0.653
_exptl_absorpt_coefficient_mu 1.457
_exptl_absorpt_correction_T_max 0.7462
_exptl_absorpt_correction_T_min 0.6405
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0543 before and 0.0431 after correction. The Ratio of minimum to maximum transmission is 0.8583. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour YELLOW
_exptl_crystal_density_diffrn 1.760
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description ROD
_exptl_crystal_F_000 992
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.12
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0428
_diffrn_reflns_av_unetI/netI 0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 56749
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 31.587
_diffrn_reflns_theta_min 2.876
_diffrn_ambient_temperature 150.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5451
_reflns_number_total 6321
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection 'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max 0.428
_refine_diff_density_min -0.286
_refine_diff_density_rms 0.063
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.025
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 244
_refine_ls_number_reflns 6321
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0269
_refine_ls_R_factor_gt 0.0189
_refine_ls_restrained_S_all 1.025
_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^)+(0.0222P)^2^+0.5910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0435
_refine_ls_wR_factor_ref 0.0456
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C00O(H00O), C10(H10), C11(H11),
N14(H14), N17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd01 Cd 0.43612(2) 0.72577(2) 0.52334(2) 0.01733(3) Uani 1 1 d . . . . .
Cl1 Cl 0.27080(5) 0.85266(3) 0.56630(2) 0.03006(7) Uani 1 1 d . . . . .
N1 N 0.54256(14) 0.78927(7) 0.40128(7) 0.01879(19) Uani 1 1 d . . . . .
Cl2 Cl 0.68266(4) 0.69726(2) 0.61625(2) 0.02235(6) Uani 1 1 d . . . . .
C2 C 0.61540(17) 0.87176(9) 0.40227(9) 0.0230(2) Uani 1 1 d . . . . .
H2 H 0.594869 0.912719 0.446698 0.028 Uiso 1 1 calc R . . . .
C3 C 0.71964(17) 0.90003(9) 0.34119(9) 0.0246(3) Uani 1 1 d . . . . .
H3 H 0.767595 0.959460 0.342960 0.030 Uiso 1 1 calc R . . . .
C4 C 0.75159(16) 0.83912(9) 0.27771(9) 0.0226(2) Uani 1 1 d . . . . .
H4 H 0.824646 0.855725 0.235844 0.027 Uiso 1 1 calc R . . . .
C5 C 0.67622(14) 0.75358(9) 0.27556(8) 0.0176(2) Uani 1 1 d . . . . .
H5 H 0.697077 0.711183 0.232306 0.021 Uiso 1 1 calc R . . . .
C6 C 0.56948(14) 0.73076(8) 0.33777(7) 0.01479(19) Uani 1 1 d . . . . .
C8 C 0.44309(14) 0.58678(8) 0.26284(7) 0.0149(2) Uani 1 1 d . . . . .
C7 C 0.48236(13) 0.64088(8) 0.34011(7) 0.01397(19) Uani 1 1 d . . . . .
C9 C 0.42620(15) 0.62719(9) 0.18395(8) 0.0187(2) Uani 1 1 d . . . . .
H9 H 0.449935 0.690401 0.176939 0.022 Uiso 1 1 calc R . . . .
C00O C 0.35786(18) 0.44717(10) 0.20831(9) 0.0255(3) Uani 1 1 d . . . . .
H00O H 0.332908 0.384357 0.216872 0.031 Uiso 1 1 calc R . . . .
C10 C 0.37423(17) 0.57379(11) 0.11579(8) 0.0252(3) Uani 1 1 d . . . . .
H10 H 0.362501 0.600023 0.061390 0.030 Uiso 1 1 calc R . . . .
C11 C 0.33951(18) 0.48186(11) 0.12759(9) 0.0273(3) Uani 1 1 d . . . . .
H11 H 0.304228 0.443796 0.081807 0.033 Uiso 1 1 calc R . . . .
N12 N 0.40870(14) 0.49733(8) 0.27457(7) 0.0202(2) Uani 1 1 d . . . . .
N13 N 0.43440(12) 0.61920(7) 0.41394(6) 0.01477(17) Uani 1 1 d . . . . .
N14 N 0.35377(12) 0.54036(7) 0.42788(6) 0.01595(18) Uani 1 1 d . . . . .
H14 H 0.348327 0.495906 0.390619 0.019 Uiso 1 1 calc R . . . .
C15 C 0.27976(14) 0.53256(8) 0.50369(7) 0.0150(2) Uani 1 1 d . . . . .
O16 O 0.28728(11) 0.59424(6) 0.55698(6) 0.01834(16) Uani 1 1 d . . . . .
N17 N 0.20120(13) 0.45193(7) 0.51029(7) 0.01726(18) Uani 1 1 d . . . . .
H17 H 0.206127 0.415333 0.466739 0.021 Uiso 1 1 calc R . . . .
C18 C 0.11214(14) 0.41733(8) 0.57659(8) 0.0160(2) Uani 1 1 d . . . . .
C19 C 0.03315(15) 0.33327(9) 0.56145(8) 0.0198(2) Uani 1 1 d . . . . .
H19 H 0.038932 0.304082 0.508573 0.024 Uiso 1 1 calc R . . . .
C20 C -0.05386(16) 0.29259(10) 0.62407(10) 0.0243(3) Uani 1 1 d . . . . .
H20 H -0.107603 0.235511 0.613787 0.029 Uiso 1 1 calc R . . . .
C21 C -0.06280(16) 0.33463(10) 0.70131(9) 0.0255(3) Uani 1 1 d . . . . .
H21 H -0.120763 0.306107 0.744284 0.031 Uiso 1 1 calc R . . . .
C22 C 0.01329(17) 0.41845(11) 0.71543(9) 0.0253(3) Uani 1 1 d . . . . .
H22 H 0.005224 0.447851 0.768060 0.030 Uiso 1 1 calc R . . . .
C23 C 0.10177(16) 0.46062(10) 0.65365(8) 0.0220(2) Uani 1 1 d . . . . .
H23 H 0.154150 0.518053 0.664081 0.026 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd01 0.02330(4) 0.01554(4) 0.01351(4) -0.00170(3) 0.00414(3) -0.00022(3)
Cl1 0.04314(18) 0.02717(16) 0.02082(15) 0.00099(12) 0.01012(13) 0.01490(14)
N1 0.0248(5) 0.0163(5) 0.0157(5) -0.0007(4) 0.0039(4) -0.0006(4)
Cl2 0.02647(14) 0.01969(13) 0.02059(14) -0.00541(11) -0.00146(11) 0.00032(10)
C2 0.0307(6) 0.0172(5) 0.0211(6) -0.0017(5) 0.0023(5) -0.0026(5)
C3 0.0295(6) 0.0182(6) 0.0261(7) 0.0029(5) 0.0021(5) -0.0053(5)
C4 0.0220(5) 0.0228(6) 0.0232(6) 0.0053(5) 0.0042(5) -0.0036(5)
C5 0.0178(5) 0.0189(5) 0.0162(5) 0.0020(4) 0.0031(4) -0.0002(4)
C6 0.0163(4) 0.0145(5) 0.0136(5) 0.0018(4) 0.0012(4) 0.0010(4)
C8 0.0149(4) 0.0168(5) 0.0131(5) -0.0010(4) 0.0023(4) 0.0020(4)
C7 0.0145(4) 0.0148(5) 0.0127(5) 0.0004(4) 0.0016(4) 0.0008(4)
C9 0.0203(5) 0.0211(5) 0.0147(5) 0.0018(4) 0.0003(4) 0.0015(4)
C00O 0.0355(7) 0.0202(6) 0.0209(6) -0.0058(5) 0.0029(5) -0.0004(5)
C10 0.0285(6) 0.0330(7) 0.0137(6) -0.0005(5) -0.0022(5) 0.0004(5)
C11 0.0333(7) 0.0293(7) 0.0190(6) -0.0085(5) 0.0005(5) -0.0005(5)
N12 0.0279(5) 0.0166(5) 0.0165(5) -0.0021(4) 0.0036(4) 0.0005(4)
N13 0.0162(4) 0.0146(4) 0.0137(4) 0.0011(3) 0.0022(3) -0.0004(3)
N14 0.0219(4) 0.0141(4) 0.0123(4) 0.0003(3) 0.0041(3) -0.0031(4)
C15 0.0157(4) 0.0165(5) 0.0128(5) 0.0019(4) 0.0020(4) 0.0008(4)
O16 0.0235(4) 0.0174(4) 0.0144(4) -0.0019(3) 0.0043(3) -0.0036(3)
N17 0.0223(4) 0.0156(4) 0.0144(4) -0.0006(4) 0.0056(4) -0.0028(4)
C18 0.0152(5) 0.0172(5) 0.0158(5) 0.0040(4) 0.0024(4) 0.0005(4)
C19 0.0197(5) 0.0180(5) 0.0218(6) 0.0034(4) 0.0020(4) -0.0013(4)
C20 0.0192(5) 0.0227(6) 0.0311(7) 0.0105(5) 0.0025(5) -0.0023(4)
C21 0.0190(5) 0.0313(7) 0.0270(7) 0.0137(6) 0.0076(5) 0.0033(5)
C22 0.0268(6) 0.0322(7) 0.0175(6) 0.0055(5) 0.0080(5) 0.0028(5)
C23 0.0251(6) 0.0239(6) 0.0176(6) 0.0003(5) 0.0061(5) -0.0019(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
Cd01 Cl1 2.4085(3) . ?
Cd01 N1 2.3668(11) . ?
Cd01 Cl2 2.4589(4) . ?
Cd01 N13 2.3396(10) . ?
Cd01 O16 2.3457(9) . ?
N1 C2 1.3404(16) . ?
N1 C6 1.3535(15) . ?
C2 H2 0.9500 . ?
C2 C3 1.3898(18) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.3892(17) . ?
C5 H5 0.9500 . ?
C5 C6 1.3953(15) . ?
C6 C7 1.4910(16) . ?
C8 C7 1.4853(16) . ?
C8 C9 1.3920(16) . ?
C8 N12 1.3497(16) . ?
C7 N13 1.3025(14) . ?
C9 H9 0.9500 . ?
C9 C10 1.3858(18) . ?
C00O H00O 0.9500 . ?
C00O C11 1.386(2) . ?
C00O N12 1.3337(17) . ?
C10 H10 0.9500 . ?
C10 C11 1.385(2) . ?
C11 H11 0.9500 . ?
N13 N14 1.3478(13) . ?
N14 H14 0.8800 . ?
N14 C15 1.3872(14) . ?
C15 O16 1.2383(14) . ?
C15 N17 1.3449(15) . ?
N17 H17 0.8800 . ?
N17 C18 1.4095(15) . ?
C18 C19 1.3984(17) . ?
C18 C23 1.3912(18) . ?
C19 H19 0.9500 . ?
C19 C20 1.3901(17) . ?
C20 H20 0.9500 . ?
C20 C21 1.384(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.383(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.3960(17) . ?
C23 H23 0.9500 . ?
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
Cl1 Cd01 Cl2 113.886(13) . . ?
N1 Cd01 Cl1 99.74(3) . . ?
N1 Cd01 Cl2 104.02(3) . . ?
N13 Cd01 Cl1 138.06(3) . . ?
N13 Cd01 N1 68.33(4) . . ?
N13 Cd01 Cl2 108.04(3) . . ?
N13 Cd01 O16 69.29(3) . . ?
O16 Cd01 Cl1 105.14(2) . . ?
O16 Cd01 N1 136.52(3) . . ?
O16 Cd01 Cl2 97.75(2) . . ?
C2 N1 Cd01 121.51(9) . . ?
C2 N1 C6 119.04(11) . . ?
C6 N1 Cd01 116.96(8) . . ?
N1 C2 H2 118.5 . . ?
N1 C2 C3 122.91(13) . . ?
C3 C2 H2 118.5 . . ?
C2 C3 H3 120.9 . . ?
C4 C3 C2 118.10(12) . . ?
C4 C3 H3 120.9 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.63(12) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 120.4 . . ?
C4 C5 C6 119.12(12) . . ?
C6 C5 H5 120.4 . . ?
N1 C6 C5 121.13(11) . . ?
N1 C6 C7 116.04(10) . . ?
C5 C6 C7 122.80(11) . . ?
C9 C8 C7 122.29(11) . . ?
N12 C8 C7 115.75(11) . . ?
N12 C8 C9 121.64(11) . . ?
C8 C7 C6 121.75(10) . . ?
N13 C7 C6 113.73(10) . . ?
N13 C7 C8 124.32(11) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 C8 118.99(12) . . ?
C10 C9 H9 120.5 . . ?
C11 C00O H00O 118.3 . . ?
N12 C00O H00O 118.3 . . ?
N12 C00O C11 123.46(13) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 C9 119.48(13) . . ?
C11 C10 H10 120.3 . . ?
C00O C11 H11 121.0 . . ?
C10 C11 C00O 117.91(13) . . ?
C10 C11 H11 121.0 . . ?
C00O N12 C8 118.51(12) . . ?
C7 N13 Cd01 121.78(8) . . ?
C7 N13 N14 121.97(10) . . ?
N14 N13 Cd01 115.22(7) . . ?
N13 N14 H14 121.6 . . ?
N13 N14 C15 116.89(10) . . ?
C15 N14 H14 121.6 . . ?
O16 C15 N14 122.32(11) . . ?
O16 C15 N17 125.93(11) . . ?
N17 C15 N14 111.75(10) . . ?
C15 O16 Cd01 116.28(7) . . ?
C15 N17 H17 115.2 . . ?
C15 N17 C18 129.60(11) . . ?
C18 N17 H17 115.2 . . ?
C19 C18 N17 115.66(11) . . ?
C23 C18 N17 124.23(11) . . ?
C23 C18 C19 120.10(11) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 C18 119.73(13) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.51(13) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 120.3 . . ?
C22 C21 C20 119.48(12) . . ?
C22 C21 H21 120.3 . . ?
C21 C22 H22 119.4 . . ?
C21 C22 C23 121.12(13) . . ?
C23 C22 H22 119.4 . . ?
C18 C23 C22 119.05(13) . . ?
C18 C23 H23 120.5 . . ?
C22 C23 H23 120.5 . . ?
_iucr_refine_instructions_details
;
TITL mo_DT_CdCl_L2_0m_a.res in P2(1)/n
mo_dt_cdcl_l2_0m_a.res
created by SHELXL-2017/1 at 12:35:56 on 31-Jul-2019
REM Old TITL mo_DT_CdCl_L2_0m in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.076, Rweak 0.006, Alpha 0.062, Orientation as input
REM Formula found by SHELXT: C19 Cd Cl2 N4 O
REM #####
CELL 0.71073 8.1129 14.5881 15.9877 90 93.22 90
ZERR 4 0.0005 0.0008 0.0009 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cd Cl N O
UNIT 72 60 4 8 20 4
L.S. 10
PLAN 20
SIZE 0.12 0.26 0.32
TEMP -123.14
BOND $H
LIST 6
fmap 2
acta
REM
REM
REM
WGHT 0.022200 0.591000
FVAR 0.39065
CD01 3 0.436123 0.725770 0.523344 11.00000 0.02330 0.01554 =
0.01351 -0.00170 0.00414 -0.00022
CL1 4 0.270796 0.852661 0.566299 11.00000 0.04314 0.02717 =
0.02082 0.00099 0.01012 0.01490
N1 5 0.542558 0.789269 0.401277 11.00000 0.02475 0.01626 =
0.01568 -0.00069 0.00390 -0.00061
CL2 4 0.682664 0.697256 0.616248 11.00000 0.02647 0.01969 =
0.02059 -0.00541 -0.00146 0.00032
C2 1 0.615402 0.871762 0.402273 11.00000 0.03068 0.01719 =
0.02111 -0.00169 0.00234 -0.00258
AFIX 43
H2 2 0.594869 0.912719 0.446698 11.00000 -1.20000
AFIX 0
C3 1 0.719638 0.900033 0.341195 11.00000 0.02955 0.01823 =
0.02609 0.00294 0.00212 -0.00530
AFIX 43
H3 2 0.767595 0.959460 0.342960 11.00000 -1.20000
AFIX 0
C4 1 0.751588 0.839120 0.277707 11.00000 0.02205 0.02278 =
0.02317 0.00532 0.00424 -0.00363
AFIX 43
H4 2 0.824646 0.855725 0.235844 11.00000 -1.20000
AFIX 0
C5 1 0.676218 0.753579 0.275560 11.00000 0.01782 0.01894 =
0.01620 0.00196 0.00307 -0.00025
AFIX 43
H5 2 0.697077 0.711183 0.232306 11.00000 -1.20000
AFIX 0
C6 1 0.569478 0.730757 0.337772 11.00000 0.01625 0.01454 =
0.01361 0.00176 0.00120 0.00102
C8 1 0.443093 0.586784 0.262841 11.00000 0.01493 0.01684 =
0.01313 -0.00099 0.00232 0.00204
C7 1 0.482358 0.640879 0.340109 11.00000 0.01453 0.01478 =
0.01269 0.00040 0.00165 0.00085
C9 1 0.426198 0.627186 0.183948 11.00000 0.02033 0.02114 =
0.01466 0.00181 0.00032 0.00149
AFIX 43
H9 2 0.449935 0.690401 0.176939 11.00000 -1.20000
AFIX 0
C00O 1 0.357860 0.447170 0.208308 11.00000 0.03548 0.02024 =
0.02088 -0.00580 0.00288 -0.00039
AFIX 43
H00O 2 0.332908 0.384357 0.216872 11.00000 -1.20000
AFIX 0
C10 1 0.374228 0.573793 0.115786 11.00000 0.02851 0.03296 =
0.01370 -0.00047 -0.00222 0.00044
AFIX 43
H10 2 0.362501 0.600023 0.061390 11.00000 -1.20000
AFIX 0
C11 1 0.339506 0.481865 0.127587 11.00000 0.03335 0.02928 =
0.01905 -0.00849 0.00054 -0.00054
AFIX 43
H11 2 0.304228 0.443796 0.081807 11.00000 -1.20000
AFIX 0
N12 5 0.408701 0.497331 0.274569 11.00000 0.02792 0.01655 =
0.01653 -0.00208 0.00358 0.00051
N13 5 0.434398 0.619201 0.413943 11.00000 0.01617 0.01458 =
0.01373 0.00111 0.00217 -0.00040
N14 5 0.353769 0.540361 0.427878 11.00000 0.02192 0.01405 =
0.01225 0.00031 0.00414 -0.00312
AFIX 43
H14 2 0.348327 0.495906 0.390619 11.00000 -1.20000
AFIX 0
C15 1 0.279765 0.532565 0.503693 11.00000 0.01565 0.01651 =
0.01284 0.00191 0.00198 0.00076
O16 6 0.287275 0.594240 0.556983 11.00000 0.02353 0.01744 =
0.01442 -0.00189 0.00430 -0.00357
N17 5 0.201199 0.451926 0.510286 11.00000 0.02231 0.01557 =
0.01440 -0.00056 0.00558 -0.00280
AFIX 43
H17 2 0.206127 0.415333 0.466739 11.00000 -1.20000
AFIX 0
C18 1 0.112140 0.417326 0.576591 11.00000 0.01521 0.01715 =
0.01582 0.00402 0.00241 0.00053
C19 1 0.033151 0.333269 0.561446 11.00000 0.01972 0.01801 =
0.02177 0.00336 0.00202 -0.00135
AFIX 43
H19 2 0.038932 0.304082 0.508573 11.00000 -1.20000
AFIX 0
C20 1 -0.053862 0.292593 0.624073 11.00000 0.01921 0.02273 =
0.03108 0.01051 0.00251 -0.00235
AFIX 43
H20 2 -0.107603 0.235511 0.613787 11.00000 -1.20000
AFIX 0
C21 1 -0.062803 0.334629 0.701314 11.00000 0.01896 0.03130 =
0.02698 0.01375 0.00760 0.00333
AFIX 43
H21 2 -0.120763 0.306107 0.744284 11.00000 -1.20000
AFIX 0
C22 1 0.013289 0.418451 0.715427 11.00000 0.02681 0.03221 =
0.01752 0.00546 0.00804 0.00279
AFIX 43
H22 2 0.005224 0.447851 0.768060 11.00000 -1.20000
AFIX 0
C23 1 0.101769 0.460617 0.653649 11.00000 0.02509 0.02385 =
0.01759 0.00028 0.00612 -0.00185
AFIX 43
H23 2 0.154150 0.518053 0.664081 11.00000 -1.20000
AFIX 0
HKLF 4
REM mo_DT_CdCl_L2_0m_a.res in P2(1)/n
REM R1 = 0.0189 for 5451 Fo > 4sig(Fo) and 0.0269 for all 6321 data
REM 244 parameters refined using 0 restraints
END
WGHT 0.0222 0.5910
REM Highest difference peak 0.428, deepest hole -0.286, 1-sigma level 0.063
Q1 1 0.3121 0.5356 0.4662 11.00000 0.05 0.43
Q2 1 0.4275 0.6090 0.2227 11.00000 0.05 0.42
Q3 1 0.0564 0.4369 0.6828 11.00000 0.05 0.42
Q4 1 0.4001 0.5954 0.1546 11.00000 0.05 0.40
Q5 1 0.7040 0.8022 0.2766 11.00000 0.05 0.39
Q6 1 0.6105 0.7487 0.3071 11.00000 0.05 0.39
Q7 1 0.4720 0.6097 0.3022 11.00000 0.05 0.38
Q8 1 0.5317 0.6833 0.3431 11.00000 0.05 0.38
Q9 1 0.1064 0.4397 0.6136 11.00000 0.05 0.38
Q10 1 0.0661 0.3782 0.5674 11.00000 0.05 0.37
Q11 1 0.6731 0.8824 0.3709 11.00000 0.05 0.37
Q12 1 0.4292 0.5441 0.2665 11.00000 0.05 0.35
Q13 1 0.3414 0.4676 0.1687 11.00000 0.05 0.35
Q14 1 0.2296 0.4959 0.5074 11.00000 0.05 0.35
Q15 1 0.7424 0.8653 0.3124 11.00000 0.05 0.35
Q16 1 -0.0421 0.3779 0.7119 11.00000 0.05 0.34
Q17 1 -0.0073 0.3117 0.5947 11.00000 0.05 0.33
Q18 1 0.5595 0.7635 0.3726 11.00000 0.05 0.31
Q19 1 0.5108 0.7777 0.4386 11.00000 0.05 0.31
Q20 1 0.4712 0.6210 0.3768 11.00000 0.05 0.30
REM The information below was added by Olex2.
REM
REM R1 = 0.0189 for 5451 Fo > 4sig(Fo) and 0.0269 for all 57851 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.43, deepest hole -0.29
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0269
REM R1_gt = 0.0189
REM wR_ref = 0.0456
REM GOOF = 1.025
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 57851
REM Reflections_gt = 5451
REM Parameters = n/a
REM Hole = -0.29
REM Peak = 0.43
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_Complex_4
_database_code_depnum_ccdc_archive 'CCDC 1993507'
loop_
_audit_author_name
_audit_author_address
'Krishna K. Damodaran'
;University of Iceland
Iceland
;
_audit_update_record
;
2020-03-29 deposited with the CCDC. 2020-12-09 downloaded from the CCDC.
;
_audit_creation_date 2020-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H26 Cd N8 O2'
_chemical_formula_sum 'C36 H26 Cd N8 O2'
_chemical_formula_weight 715.05
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 15.3928(10)
_cell_length_b 10.6783(7)
_cell_length_c 19.4846(12)
_cell_angle_alpha 90
_cell_angle_beta 96.349(2)
_cell_angle_gamma 90
_cell_volume 3183.0(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9849
_cell_measurement_temperature 295(2)
_cell_measurement_theta_max 72.21
_cell_measurement_theta_min 3.88
_shelx_estimated_absorpt_T_max 0.719
_shelx_estimated_absorpt_T_min 0.402
_exptl_absorpt_coefficient_mu 5.874
_exptl_absorpt_correction_T_max 0.7536
_exptl_absorpt_correction_T_min 0.5112
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0984 before and 0.0581 after correction. The Ratio of minimum to maximum transmission is 0.6783. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.492
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description BLOCK
_exptl_crystal_F_000 1448
_exptl_crystal_size_max 0.19
_exptl_crystal_size_mid 0.115
_exptl_crystal_size_min 0.06
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0323
_diffrn_reflns_av_unetI/netI 0.0158
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 64208
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 72.271
_diffrn_reflns_theta_min 3.875
_diffrn_ambient_temperature 295.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5831
_reflns_number_total 6238
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max 0.474
_refine_diff_density_min -0.609
_refine_diff_density_rms 0.049
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.050
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 424
_refine_ls_number_reflns 6238
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0299
_refine_ls_R_factor_gt 0.0278
_refine_ls_restrained_S_all 1.050
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+1.8204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0674
_refine_ls_wR_factor_ref 0.0688
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C12(H12), C11(H11),
C19(H19), C18(H18), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27),
C28(H28), C32(H32), C33(H33), C34(H34), C35(H35), C41(H41), C42(H42),
C43(H43), C44(H44), C45(H45)
;
_atom_sites_solution_hydrogens geom
_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 0.54017(2) 0.50801(2) 0.67944(2) 0.04496(6) Uani 1 1 d . . . . .
N1 N 0.39966(12) 0.59322(17) 0.69792(9) 0.0487(4) Uani 1 1 d . . . . .
C2 C 0.35204(18) 0.5618(3) 0.74870(12) 0.0640(6) Uani 1 1 d . . . . .
H2 H 0.377678 0.511113 0.784110 0.077 Uiso 1 1 calc R . . . .
C3 C 0.2678(2) 0.6002(3) 0.75140(15) 0.0766(8) Uani 1 1 d . . . . .
H3 H 0.236610 0.575263 0.787318 0.092 Uiso 1 1 calc R . . . .
C4 C 0.23057(19) 0.6762(3) 0.69985(16) 0.0797(8) Uani 1 1 d . . . . .
H4 H 0.173392 0.704101 0.700299 0.096 Uiso 1 1 calc R . . . .
C5 C 0.27850(16) 0.7114(3) 0.64704(14) 0.0630(6) Uani 1 1 d . . . . .
H5 H 0.254217 0.763966 0.611977 0.076 Uiso 1 1 calc R . . . .
C7 C 0.41752(12) 0.69728(18) 0.59072(10) 0.0404(4) Uani 1 1 d . . . . .
C6 C 0.36314(13) 0.66738(19) 0.64703(10) 0.0438(4) Uani 1 1 d . . . . .
C8 C 0.39695(13) 0.80664(19) 0.54461(11) 0.0444(4) Uani 1 1 d . . . . .
C9 C 0.39503(16) 0.7991(2) 0.47374(12) 0.0572(6) Uani 1 1 d . . . . .
H9 H 0.400252 0.722298 0.452011 0.069 Uiso 1 1 calc R . . . .
C10 C 0.38513(19) 0.9087(3) 0.43592(15) 0.0760(8) Uani 1 1 d . . . . .
H10 H 0.383827 0.907270 0.388093 0.091 Uiso 1 1 calc R . . . .
N13 N 0.38575(16) 0.91353(19) 0.57793(11) 0.0668(6) Uani 1 1 d . . . . .
C12 C 0.3765(3) 1.0171(3) 0.5399(2) 0.0895(10) Uani 1 1 d . . . . .
H12 H 0.369070 1.092545 0.562341 0.107 Uiso 1 1 calc R . . . .
C11 C 0.3773(2) 1.0195(3) 0.4701(2) 0.0910(11) Uani 1 1 d . . . . .
H11 H 0.372574 1.094942 0.446057 0.109 Uiso 1 1 calc R . . . .
N14 N 0.48526(10) 0.62705(15) 0.58758(8) 0.0384(3) Uani 1 1 d . . . . .
N15 N 0.53925(10) 0.64981(16) 0.53764(8) 0.0409(4) Uani 1 1 d . . . . .
C17 C 0.67013(14) 0.5928(2) 0.49223(10) 0.0463(5) Uani 1 1 d . . . . .
C16 C 0.60964(13) 0.57658(19) 0.54629(10) 0.0412(4) Uani 1 1 d . . . . .
C19 C 0.8112(2) 0.5668(4) 0.45324(18) 0.0963(11) Uani 1 1 d . . . . .
H19 H 0.868827 0.539547 0.461201 0.116 Uiso 1 1 calc R . . . .
C18 C 0.75524(18) 0.5507(3) 0.50360(14) 0.0747(8) Uani 1 1 d . . . . .
H18 H 0.775061 0.511615 0.545035 0.090 Uiso 1 1 calc R . . . .
C20 C 0.7818(2) 0.6229(3) 0.39167(16) 0.0815(9) Uani 1 1 d . . . . .
H20 H 0.819428 0.632892 0.357888 0.098 Uiso 1 1 calc R . . . .
C21 C 0.69769(18) 0.6639(3) 0.37982(13) 0.0629(6) Uani 1 1 d . . . . .
H21 H 0.678091 0.701717 0.337951 0.075 Uiso 1 1 calc R . . . .
C22 C 0.64150(15) 0.6496(2) 0.42972(10) 0.0484(5) Uani 1 1 d . . . . .
H22 H 0.584218 0.678182 0.421457 0.058 Uiso 1 1 calc R . . . .
O23 O 0.63031(11) 0.49942(14) 0.59489(8) 0.0546(4) Uani 1 1 d . . . . .
N24 N 0.62044(13) 0.67961(19) 0.73386(9) 0.0562(5) Uani 1 1 d . . . . .
C25 C 0.6490(2) 0.7775(3) 0.70057(13) 0.0755(8) Uani 1 1 d . . . . .
H25 H 0.633147 0.783144 0.653218 0.091 Uiso 1 1 calc R . . . .
C26 C 0.7005(2) 0.8706(3) 0.73197(14) 0.0815(9) Uani 1 1 d . . . . .
H26 H 0.718626 0.937842 0.706787 0.098 Uiso 1 1 calc R . . . .
C27 C 0.72434(18) 0.8611(3) 0.80160(14) 0.0746(8) Uani 1 1 d . . . . .
H27 H 0.759521 0.922054 0.824650 0.090 Uiso 1 1 calc R . . . .
C28 C 0.69565(16) 0.7602(3) 0.83727(12) 0.0611(6) Uani 1 1 d . . . . .
H28 H 0.711757 0.752599 0.884512 0.073 Uiso 1 1 calc R . . . .
C29 C 0.64270(13) 0.6703(2) 0.80240(10) 0.0478(5) Uani 1 1 d . . . . .
C30 C 0.61186(14) 0.5570(2) 0.83643(10) 0.0471(5) Uani 1 1 d . . . . .
C31 C 0.61266(16) 0.5547(3) 0.91331(11) 0.0569(6) Uani 1 1 d . . . . .
C32 C 0.6439(2) 0.4541(3) 0.95283(15) 0.0824(9) Uani 1 1 d . . . . .
H32 H 0.666761 0.384045 0.932880 0.099 Uiso 1 1 calc R . . . .
C33 C 0.6400(3) 0.4614(5) 1.02427(19) 0.1120(15) Uani 1 1 d . . . . .
H33 H 0.661758 0.396518 1.053070 0.134 Uiso 1 1 calc R . . . .
C34 C 0.6039(3) 0.5644(5) 1.05098(17) 0.1185(17) Uani 1 1 d . . . . .
H34 H 0.599452 0.569976 1.098092 0.142 Uiso 1 1 calc R . . . .
C35 C 0.5748(3) 0.6582(4) 1.00808(15) 0.1006(12) Uani 1 1 d . . . . .
H35 H 0.550226 0.728025 1.027001 0.121 Uiso 1 1 calc R . . . .
N36 N 0.57914(17) 0.6566(2) 0.94009(11) 0.0743(6) Uani 1 1 d . . . . .
N37 N 0.58446(12) 0.46761(18) 0.79465(9) 0.0485(4) Uani 1 1 d . . . . .
N38 N 0.56098(13) 0.35594(18) 0.82010(9) 0.0528(4) Uani 1 1 d . . . . .
C39 C 0.53138(14) 0.2795(2) 0.76690(11) 0.0481(5) Uani 1 1 d . . . . .
C40 C 0.51538(14) 0.1474(2) 0.78762(11) 0.0467(5) Uani 1 1 d . . . . .
C41 C 0.47835(16) 0.0633(2) 0.73920(13) 0.0560(5) Uani 1 1 d . . . . .
H41 H 0.462388 0.089857 0.694106 0.067 Uiso 1 1 calc R . . . .
C42 C 0.46472(18) -0.0595(3) 0.75681(16) 0.0688(7) Uani 1 1 d . . . . .
H42 H 0.438954 -0.114797 0.723743 0.083 Uiso 1 1 calc R . . . .
C43 C 0.48890(18) -0.1006(3) 0.82280(16) 0.0704(7) Uani 1 1 d . . . . .
H43 H 0.480325 -0.183893 0.834309 0.084 Uiso 1 1 calc R . . . .
C44 C 0.5255(2) -0.0192(3) 0.87140(16) 0.0701(7) Uani 1 1 d . . . . .
H44 H 0.541767 -0.047312 0.916158 0.084 Uiso 1 1 calc R . . . .
C45 C 0.53884(17) 0.1057(2) 0.85490(13) 0.0606(6) Uani 1 1 d . . . . .
H45 H 0.563270 0.160881 0.888566 0.073 Uiso 1 1 calc R . . . .
O46 O 0.51691(13) 0.30630(16) 0.70369(8) 0.0665(5) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.05432(10) 0.04406(10) 0.03573(9) 0.00743(5) 0.00146(6) 0.00318(6)
N1 0.0571(10) 0.0504(10) 0.0401(9) 0.0031(7) 0.0117(8) 0.0006(8)
C2 0.0777(17) 0.0712(17) 0.0464(12) 0.0058(11) 0.0211(12) 0.0016(13)
C3 0.0796(19) 0.091(2) 0.0656(16) 0.0015(15) 0.0361(14) -0.0030(16)
C4 0.0592(16) 0.099(2) 0.086(2) 0.0012(17) 0.0318(14) 0.0077(15)
C5 0.0515(13) 0.0719(17) 0.0676(15) 0.0079(12) 0.0152(11) 0.0092(11)
C7 0.0407(10) 0.0401(11) 0.0398(10) 0.0019(8) 0.0022(8) 0.0006(8)
C6 0.0446(11) 0.0425(11) 0.0448(10) -0.0018(8) 0.0077(8) -0.0016(8)
C8 0.0401(10) 0.0415(11) 0.0513(11) 0.0074(9) 0.0032(8) 0.0030(8)
C9 0.0600(14) 0.0598(14) 0.0505(12) 0.0100(10) 0.0007(10) 0.0096(11)
C10 0.0711(17) 0.093(2) 0.0643(16) 0.0355(16) 0.0072(13) 0.0168(15)
N13 0.0856(15) 0.0445(11) 0.0693(13) 0.0024(9) 0.0041(11) 0.0106(10)
C12 0.118(3) 0.0437(16) 0.104(3) 0.0086(15) -0.001(2) 0.0149(15)
C11 0.092(2) 0.069(2) 0.110(3) 0.0486(19) 0.004(2) 0.0107(16)
N14 0.0402(8) 0.0389(9) 0.0360(8) 0.0045(6) 0.0032(6) 0.0008(6)
N15 0.0416(8) 0.0434(9) 0.0383(8) 0.0063(7) 0.0065(7) 0.0027(7)
C17 0.0473(11) 0.0493(12) 0.0428(11) -0.0053(9) 0.0073(9) 0.0023(9)
C16 0.0438(10) 0.0441(11) 0.0351(9) -0.0006(8) 0.0019(8) 0.0017(8)
C19 0.0584(17) 0.145(3) 0.091(2) 0.008(2) 0.0297(16) 0.0240(19)
C18 0.0565(15) 0.108(2) 0.0605(15) 0.0077(15) 0.0122(12) 0.0201(15)
C20 0.0785(19) 0.103(2) 0.0697(18) -0.0055(16) 0.0378(15) -0.0023(17)
C21 0.0774(17) 0.0641(16) 0.0501(13) -0.0001(11) 0.0202(12) -0.0045(13)
C22 0.0570(12) 0.0455(12) 0.0435(11) -0.0019(9) 0.0091(9) -0.0009(9)
O23 0.0563(9) 0.0655(11) 0.0426(8) 0.0122(6) 0.0080(7) 0.0207(7)
N24 0.0644(12) 0.0634(12) 0.0392(9) 0.0017(8) -0.0020(8) -0.0152(9)
C25 0.095(2) 0.083(2) 0.0469(13) 0.0093(12) 0.0000(13) -0.0374(16)
C26 0.089(2) 0.093(2) 0.0630(16) 0.0064(14) 0.0073(14) -0.0463(17)
C27 0.0628(16) 0.091(2) 0.0687(16) -0.0054(14) 0.0022(13) -0.0364(15)
C28 0.0540(13) 0.0814(18) 0.0458(12) -0.0051(11) -0.0035(10) -0.0139(12)
C29 0.0403(10) 0.0610(13) 0.0418(10) -0.0013(9) 0.0030(8) -0.0014(9)
C30 0.0444(11) 0.0559(13) 0.0396(10) -0.0014(9) -0.0014(8) 0.0043(9)
C31 0.0594(13) 0.0677(16) 0.0414(11) 0.0062(11) -0.0038(10) -0.0151(12)
C32 0.093(2) 0.087(2) 0.0607(16) 0.0204(15) -0.0230(15) -0.0170(17)
C33 0.135(3) 0.123(3) 0.068(2) 0.041(2) -0.033(2) -0.046(3)
C34 0.157(4) 0.151(4) 0.0452(17) 0.003(2) 0.002(2) -0.075(3)
C35 0.132(3) 0.122(3) 0.0523(16) -0.0199(18) 0.0269(18) -0.038(2)
N36 0.0953(17) 0.0832(17) 0.0464(11) -0.0112(11) 0.0165(11) -0.0134(13)
N37 0.0526(10) 0.0492(10) 0.0436(9) 0.0058(8) 0.0052(8) 0.0030(8)
N38 0.0630(11) 0.0512(11) 0.0442(9) 0.0096(8) 0.0065(8) -0.0004(9)
C39 0.0485(11) 0.0467(12) 0.0484(12) 0.0061(9) 0.0026(9) 0.0045(9)
C40 0.0458(11) 0.0436(11) 0.0514(11) 0.0058(9) 0.0090(9) 0.0036(9)
C41 0.0597(13) 0.0497(13) 0.0587(13) 0.0009(10) 0.0074(11) 0.0003(10)
C42 0.0657(16) 0.0516(15) 0.090(2) -0.0055(13) 0.0144(14) -0.0053(12)
C43 0.0606(15) 0.0532(15) 0.100(2) 0.0177(14) 0.0224(14) -0.0007(12)
C44 0.0717(17) 0.0681(18) 0.0713(17) 0.0288(14) 0.0118(14) 0.0028(13)
C45 0.0667(15) 0.0592(15) 0.0551(13) 0.0083(11) 0.0039(11) 0.0000(11)
O46 0.0927(13) 0.0508(10) 0.0525(9) 0.0118(7) -0.0075(8) -0.0036(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N1 2.4100(18) . ?
Cd1 N14 2.2801(15) . ?
Cd1 O23 2.2700(16) . ?
Cd1 N24 2.3914(19) . ?
Cd1 N37 2.3134(18) . ?
Cd1 O46 2.2423(17) . ?
N1 C2 1.337(3) . ?
N1 C6 1.343(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.367(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.367(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.383(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.385(3) . ?
C7 C6 1.487(3) . ?
C7 C8 1.486(3) . ?
C7 N14 1.291(2) . ?
C8 C9 1.380(3) . ?
C8 N13 1.334(3) . ?
C9 H9 0.9300 . ?
C9 C10 1.383(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.369(5) . ?
N13 C12 1.330(4) . ?
C12 H12 0.9300 . ?
C12 C11 1.362(5) . ?
C11 H11 0.9300 . ?
N14 N15 1.369(2) . ?
N15 C16 1.332(2) . ?
C17 C16 1.491(3) . ?
C17 C18 1.380(3) . ?
C17 C22 1.388(3) . ?
C16 O23 1.269(2) . ?
C19 H19 0.9300 . ?
C19 C18 1.386(4) . ?
C19 C20 1.372(5) . ?
C18 H18 0.9300 . ?
C20 H20 0.9300 . ?
C20 C21 1.362(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.379(3) . ?
C22 H22 0.9300 . ?
N24 C25 1.330(3) . ?
N24 C29 1.345(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.372(4) . ?
C26 H26 0.9300 . ?
C26 C27 1.370(4) . ?
C27 H27 0.9300 . ?
C27 C28 1.380(4) . ?
C28 H28 0.9300 . ?
C28 C29 1.388(3) . ?
C29 C30 1.482(3) . ?
C30 C31 1.497(3) . ?
C30 N37 1.295(3) . ?
C31 C32 1.377(4) . ?
C31 N36 1.335(4) . ?
C32 H32 0.9300 . ?
C32 C33 1.402(5) . ?
C33 H33 0.9300 . ?
C33 C34 1.361(7) . ?
C34 H34 0.9300 . ?
C34 C35 1.350(6) . ?
C35 H35 0.9300 . ?
C35 N36 1.334(3) . ?
N37 N38 1.356(3) . ?
N38 C39 1.358(3) . ?
C39 C40 1.495(3) . ?
C39 O46 1.260(3) . ?
C40 C41 1.379(3) . ?
C40 C45 1.394(3) . ?
C41 H41 0.9300 . ?
C41 C42 1.377(4) . ?
C42 H42 0.9300 . ?
C42 C43 1.371(4) . ?
C43 H43 0.9300 . ?
C43 C44 1.361(4) . ?
C44 H44 0.9300 . ?
C44 C45 1.392(3) . ?
C45 H45 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N14 Cd1 N1 69.27(6) . . ?
N14 Cd1 N24 92.83(6) . . ?
N14 Cd1 N37 155.45(6) . . ?
O23 Cd1 N1 138.98(5) . . ?
O23 Cd1 N14 69.89(5) . . ?
O23 Cd1 N24 91.46(6) . . ?
O23 Cd1 N37 123.95(6) . . ?
N24 Cd1 N1 94.17(7) . . ?
N37 Cd1 N1 95.65(6) . . ?
N37 Cd1 N24 68.30(6) . . ?
O46 Cd1 N1 99.46(7) . . ?
O46 Cd1 N14 130.31(6) . . ?
O46 Cd1 O23 103.81(6) . . ?
O46 Cd1 N24 136.83(6) . . ?
O46 Cd1 N37 69.71(6) . . ?
C2 N1 Cd1 126.18(16) . . ?
C2 N1 C6 118.4(2) . . ?
C6 N1 Cd1 114.94(13) . . ?
N1 C2 H2 118.2 . . ?
N1 C2 C3 123.6(3) . . ?
C3 C2 H2 118.2 . . ?
C2 C3 H3 120.9 . . ?
C2 C3 C4 118.2(2) . . ?
C4 C3 H3 120.9 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.6(3) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 120.4 . . ?
C4 C5 C6 119.2(2) . . ?
C6 C5 H5 120.4 . . ?
C8 C7 C6 121.02(17) . . ?
N14 C7 C6 115.71(17) . . ?
N14 C7 C8 123.16(17) . . ?
N1 C6 C5 121.1(2) . . ?
N1 C6 C7 116.60(18) . . ?
C5 C6 C7 122.3(2) . . ?
C9 C8 C7 122.56(19) . . ?
N13 C8 C7 114.12(18) . . ?
N13 C8 C9 123.2(2) . . ?
C8 C9 H9 120.9 . . ?
C8 C9 C10 118.2(2) . . ?
C10 C9 H9 120.9 . . ?
C9 C10 H10 120.5 . . ?
C11 C10 C9 118.9(3) . . ?
C11 C10 H10 120.5 . . ?
C12 N13 C8 116.9(2) . . ?
N13 C12 H12 118.0 . . ?
N13 C12 C11 124.1(3) . . ?
C11 C12 H12 118.0 . . ?
C10 C11 H11 120.7 . . ?
C12 C11 C10 118.7(3) . . ?
C12 C11 H11 120.7 . . ?
C7 N14 Cd1 121.18(13) . . ?
C7 N14 N15 119.16(16) . . ?
N15 N14 Cd1 117.08(11) . . ?
C16 N15 N14 110.80(15) . . ?
C18 C17 C16 120.3(2) . . ?
C18 C17 C22 119.1(2) . . ?
C22 C17 C16 120.54(19) . . ?
N15 C16 C17 113.90(17) . . ?
O23 C16 N15 127.52(18) . . ?
O23 C16 C17 118.56(18) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C20 C19 C18 120.1(3) . . ?
C17 C18 C19 120.0(3) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C19 C20 H20 119.9 . . ?
C21 C20 C19 120.3(3) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 H21 119.9 . . ?
C20 C21 C22 120.2(2) . . ?
C22 C21 H21 119.9 . . ?
C17 C22 H22 119.9 . . ?
C21 C22 C17 120.3(2) . . ?
C21 C22 H22 119.9 . . ?
C16 O23 Cd1 113.10(13) . . ?
C25 N24 Cd1 124.63(15) . . ?
C25 N24 C29 118.7(2) . . ?
C29 N24 Cd1 116.48(15) . . ?
N24 C25 H25 118.1 . . ?
N24 C25 C26 123.9(2) . . ?
C26 C25 H25 118.1 . . ?
C25 C26 H26 121.1 . . ?
C27 C26 C25 117.8(3) . . ?
C27 C26 H26 121.1 . . ?
C26 C27 H27 120.3 . . ?
C26 C27 C28 119.4(2) . . ?
C28 C27 H27 120.3 . . ?
C27 C28 H28 120.1 . . ?
C27 C28 C29 119.8(2) . . ?
C29 C28 H28 120.1 . . ?
N24 C29 C28 120.4(2) . . ?
N24 C29 C30 116.45(19) . . ?
C28 C29 C30 123.05(19) . . ?
C29 C30 C31 119.6(2) . . ?
N37 C30 C29 114.74(18) . . ?
N37 C30 C31 125.7(2) . . ?
C32 C31 C30 122.4(3) . . ?
N36 C31 C30 114.7(2) . . ?
N36 C31 C32 122.9(3) . . ?
C31 C32 H32 121.3 . . ?
C31 C32 C33 117.5(4) . . ?
C33 C32 H32 121.3 . . ?
C32 C33 H33 120.4 . . ?
C34 C33 C32 119.2(4) . . ?
C34 C33 H33 120.4 . . ?
C33 C34 H34 120.5 . . ?
C35 C34 C33 119.0(3) . . ?
C35 C34 H34 120.5 . . ?
C34 C35 H35 118.1 . . ?
N36 C35 C34 123.7(4) . . ?
N36 C35 H35 118.1 . . ?
C35 N36 C31 117.6(3) . . ?
C30 N37 Cd1 120.88(15) . . ?
C30 N37 N38 120.00(18) . . ?
N38 N37 Cd1 117.20(14) . . ?
N37 N38 C39 109.26(17) . . ?
N38 C39 C40 114.34(18) . . ?
O46 C39 N38 128.2(2) . . ?
O46 C39 C40 117.5(2) . . ?
C41 C40 C39 119.8(2) . . ?
C41 C40 C45 118.7(2) . . ?
C45 C40 C39 121.5(2) . . ?
C40 C41 H41 119.6 . . ?
C42 C41 C40 120.8(2) . . ?
C42 C41 H41 119.6 . . ?
C41 C42 H42 119.8 . . ?
C43 C42 C41 120.4(3) . . ?
C43 C42 H42 119.8 . . ?
C42 C43 H43 120.1 . . ?
C44 C43 C42 119.8(3) . . ?
C44 C43 H43 120.1 . . ?
C43 C44 H44 119.6 . . ?
C43 C44 C45 120.8(3) . . ?
C45 C44 H44 119.6 . . ?
C40 C45 H45 120.2 . . ?
C44 C45 C40 119.6(2) . . ?
C44 C45 H45 120.2 . . ?
C39 O46 Cd1 114.14(15) . . ?
_iucr_refine_instructions_details
;
TITL cu_DT_Complex5_2_0m_a.res in P2(1)/n
cu_dt_complex5_2_0m_a.res
created by SHELXL-2017/1 at 16:50:56 on 26-Mar-2020
REM Old TITL cu_DT_Complex5_2_0m in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.134, Rweak 0.005, Alpha 0.062, Orientation as input
REM Formula found by SHELXT: C38 Cd N4 O4
REM #####
CELL 1.54178 15.3928 10.6783 19.4846 90 96.349 90
ZERR 4 0.001 0.0007 0.0012 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cd N O
UNIT 144 104 4 32 8
L.S. 10
PLAN 20
SIZE 0.06 0.115 0.19
TEMP 22
BOND $H
LIST 6
fmap 2
acta
REM
REM
REM
WGHT 0.029200 1.820400
FVAR 0.37145
CD1 3 0.540169 0.508009 0.679436 11.00000 0.05432 0.04406 =
0.03573 0.00743 0.00146 0.00318
N1 4 0.399658 0.593217 0.697925 11.00000 0.05710 0.05042 =
0.04010 0.00313 0.01165 0.00063
C2 1 0.352043 0.561830 0.748697 11.00000 0.07772 0.07120 =
0.04637 0.00578 0.02108 0.00160
AFIX 43
H2 2 0.377678 0.511113 0.784110 11.00000 -1.20000
AFIX 0
C3 1 0.267771 0.600194 0.751403 11.00000 0.07963 0.09083 =
0.06555 0.00153 0.03610 -0.00297
AFIX 43
H3 2 0.236610 0.575263 0.787318 11.00000 -1.20000
AFIX 0
C4 1 0.230566 0.676222 0.699854 11.00000 0.05916 0.09927 =
0.08593 0.00120 0.03180 0.00767
AFIX 43
H4 2 0.173392 0.704101 0.700299 11.00000 -1.20000
AFIX 0
C5 1 0.278500 0.711410 0.647039 11.00000 0.05151 0.07195 =
0.06762 0.00789 0.01523 0.00916
AFIX 43
H5 2 0.254217 0.763966 0.611977 11.00000 -1.20000
AFIX 0
C7 1 0.417518 0.697284 0.590716 11.00000 0.04069 0.04009 =
0.03979 0.00191 0.00221 0.00063
C6 1 0.363135 0.667381 0.647028 11.00000 0.04460 0.04247 =
0.04482 -0.00175 0.00771 -0.00162
C8 1 0.396954 0.806643 0.544610 11.00000 0.04009 0.04151 =
0.05125 0.00740 0.00316 0.00299
C9 1 0.395033 0.799050 0.473737 11.00000 0.05999 0.05979 =
0.05052 0.01000 0.00075 0.00963
AFIX 43
H9 2 0.400252 0.722298 0.452011 11.00000 -1.20000
AFIX 0
C10 1 0.385132 0.908750 0.435919 11.00000 0.07110 0.09266 =
0.06432 0.03554 0.00720 0.01681
AFIX 43
H10 2 0.383827 0.907270 0.388093 11.00000 -1.20000
AFIX 0
N13 4 0.385753 0.913526 0.577925 11.00000 0.08557 0.04453 =
0.06926 0.00240 0.00415 0.01058
C12 1 0.376515 1.017103 0.539870 11.00000 0.11781 0.04371 =
0.10402 0.00864 -0.00081 0.01493
AFIX 43
H12 2 0.369070 1.092545 0.562341 11.00000 -1.20000
AFIX 0
C11 1 0.377285 1.019532 0.470060 11.00000 0.09244 0.06915 =
0.10981 0.04864 0.00424 0.01068
AFIX 43
H11 2 0.372574 1.094942 0.446057 11.00000 -1.20000
AFIX 0
N14 4 0.485261 0.627045 0.587578 11.00000 0.04023 0.03889 =
0.03600 0.00455 0.00320 0.00077
N15 4 0.539254 0.649805 0.537642 11.00000 0.04158 0.04336 =
0.03834 0.00627 0.00652 0.00268
C17 1 0.670132 0.592812 0.492226 11.00000 0.04729 0.04934 =
0.04278 -0.00529 0.00734 0.00232
C16 1 0.609641 0.576575 0.546291 11.00000 0.04380 0.04405 =
0.03509 -0.00059 0.00190 0.00170
C19 1 0.811214 0.566818 0.453240 11.00000 0.05842 0.14470 =
0.09066 0.00820 0.02970 0.02396
AFIX 43
H19 2 0.868827 0.539547 0.461201 11.00000 -1.20000
AFIX 0
C18 1 0.755244 0.550741 0.503602 11.00000 0.05652 0.10850 =
0.06051 0.00767 0.01220 0.02006
AFIX 43
H18 2 0.775061 0.511615 0.545035 11.00000 -1.20000
AFIX 0
C20 1 0.781786 0.622879 0.391675 11.00000 0.07849 0.10301 =
0.06967 -0.00553 0.03784 -0.00226
AFIX 43
H20 2 0.819428 0.632892 0.357888 11.00000 -1.20000
AFIX 0
C21 1 0.697691 0.663931 0.379820 11.00000 0.07736 0.06414 =
0.05014 -0.00015 0.02022 -0.00455
AFIX 43
H21 2 0.678091 0.701717 0.337951 11.00000 -1.20000
AFIX 0
C22 1 0.641501 0.649639 0.429721 11.00000 0.05698 0.04549 =
0.04349 -0.00191 0.00912 -0.00085
AFIX 43
H22 2 0.584218 0.678182 0.421457 11.00000 -1.20000
AFIX 0
O23 5 0.630314 0.499419 0.594892 11.00000 0.05632 0.06545 =
0.04261 0.01224 0.00799 0.02065
N24 4 0.620436 0.679607 0.733858 11.00000 0.06444 0.06337 =
0.03915 0.00171 -0.00198 -0.01515
C25 1 0.649009 0.777466 0.700575 11.00000 0.09492 0.08290 =
0.04690 0.00934 -0.00001 -0.03736
AFIX 43
H25 2 0.633147 0.783144 0.653218 11.00000 -1.20000
AFIX 0
C26 1 0.700509 0.870561 0.731967 11.00000 0.08875 0.09268 =
0.06298 0.00643 0.00731 -0.04626
AFIX 43
H26 2 0.718626 0.937842 0.706787 11.00000 -1.20000
AFIX 0
C27 1 0.724337 0.861095 0.801604 11.00000 0.06276 0.09128 =
0.06869 -0.00539 0.00220 -0.03635
AFIX 43
H27 2 0.759521 0.922054 0.824650 11.00000 -1.20000
AFIX 0
C28 1 0.695652 0.760243 0.837271 11.00000 0.05403 0.08135 =
0.04583 -0.00514 -0.00346 -0.01390
AFIX 43
H28 2 0.711757 0.752599 0.884512 11.00000 -1.20000
AFIX 0
C29 1 0.642698 0.670289 0.802396 11.00000 0.04026 0.06099 =
0.04179 -0.00131 0.00302 -0.00142
C30 1 0.611856 0.557020 0.836433 11.00000 0.04444 0.05591 =
0.03958 -0.00143 -0.00135 0.00431
C31 1 0.612657 0.554750 0.913308 11.00000 0.05939 0.06772 =
0.04135 0.00623 -0.00382 -0.01509
C32 1 0.643915 0.454123 0.952826 11.00000 0.09262 0.08702 =
0.06067 0.02045 -0.02298 -0.01704
AFIX 43
H32 2 0.666761 0.384045 0.932880 11.00000 -1.20000
AFIX 0
C33 1 0.639984 0.461351 1.024271 11.00000 0.13480 0.12336 =
0.06789 0.04111 -0.03345 -0.04574
AFIX 43
H33 2 0.661758 0.396518 1.053070 11.00000 -1.20000
AFIX 0
C34 1 0.603931 0.564355 1.050983 11.00000 0.15711 0.15116 =
0.04516 0.00258 0.00223 -0.07497
AFIX 43
H34 2 0.599452 0.569976 1.098092 11.00000 -1.20000
AFIX 0
C35 1 0.574770 0.658233 1.008078 11.00000 0.13158 0.12159 =
0.05227 -0.01986 0.02692 -0.03758
AFIX 43
H35 2 0.550226 0.728025 1.027001 11.00000 -1.20000
AFIX 0
N36 4 0.579145 0.656618 0.940087 11.00000 0.09527 0.08321 =
0.04639 -0.01121 0.01646 -0.01344
N37 4 0.584465 0.467605 0.794646 11.00000 0.05262 0.04920 =
0.04364 0.00583 0.00524 0.00300
N38 4 0.560975 0.355936 0.820105 11.00000 0.06298 0.05120 =
0.04425 0.00957 0.00653 -0.00035
C39 1 0.531381 0.279514 0.766901 11.00000 0.04849 0.04674 =
0.04843 0.00605 0.00261 0.00454
C40 1 0.515377 0.147418 0.787624 11.00000 0.04581 0.04357 =
0.05139 0.00580 0.00898 0.00358
C41 1 0.478347 0.063321 0.739200 11.00000 0.05975 0.04973 =
0.05871 0.00090 0.00738 0.00034
AFIX 43
H41 2 0.462388 0.089857 0.694106 11.00000 -1.20000
AFIX 0
C42 1 0.464716 -0.059479 0.756815 11.00000 0.06572 0.05159 =
0.09036 -0.00551 0.01437 -0.00534
AFIX 43
H42 2 0.438954 -0.114797 0.723743 11.00000 -1.20000
AFIX 0
C43 1 0.488896 -0.100625 0.822795 11.00000 0.06061 0.05319 =
0.10043 0.01768 0.02242 -0.00070
AFIX 43
H43 2 0.480325 -0.183893 0.834309 11.00000 -1.20000
AFIX 0
C44 1 0.525491 -0.019211 0.871404 11.00000 0.07170 0.06806 =
0.07126 0.02876 0.01176 0.00284
AFIX 43
H44 2 0.541767 -0.047312 0.916158 11.00000 -1.20000
AFIX 0
C45 1 0.538840 0.105653 0.854901 11.00000 0.06671 0.05917 =
0.05515 0.00834 0.00389 0.00002
AFIX 43
H45 2 0.563270 0.160881 0.888566 11.00000 -1.20000
AFIX 0
O46 5 0.516908 0.306303 0.703686 11.00000 0.09272 0.05083 =
0.05246 0.01185 -0.00754 -0.00358
HKLF 4
REM cu_DT_Complex5_2_0m_a.res in P2(1)/n
REM R1 = 0.0278 for 5831 Fo > 4sig(Fo) and 0.0299 for all 6238 data
REM 424 parameters refined using 0 restraints
END
WGHT 0.0292 1.8204
REM Highest difference peak 0.474, deepest hole -0.609, 1-sigma level 0.049
Q1 1 0.5555 0.3837 0.7606 11.00000 0.05 0.47
Q2 1 0.5038 0.4921 0.6470 11.00000 0.05 0.35
Q3 1 0.5096 0.2445 0.6709 11.00000 0.05 0.29
Q4 1 0.6745 0.3976 1.0047 11.00000 0.05 0.25
Q5 1 0.5623 0.4302 0.8400 11.00000 0.05 0.23
Q6 1 0.4763 0.5461 0.6008 11.00000 0.05 0.23
Q7 1 0.5996 0.4950 0.9306 11.00000 0.05 0.22
Q8 1 0.4508 0.5577 0.7057 11.00000 0.05 0.22
Q9 1 0.5776 0.6036 0.7244 11.00000 0.05 0.20
Q10 1 0.5972 0.4764 0.6247 11.00000 0.05 0.19
Q11 1 0.5055 0.5970 0.6238 11.00000 0.05 0.19
Q12 1 0.5224 0.2031 0.7763 11.00000 0.05 0.19
Q13 1 0.3987 1.0151 0.5010 11.00000 0.05 0.18
Q14 1 0.4068 0.7502 0.5656 11.00000 0.05 0.18
Q15 1 0.4847 0.3062 0.7267 11.00000 0.05 0.18
Q16 1 0.7494 0.7700 0.8163 11.00000 0.05 0.17
Q17 1 0.6396 0.5780 0.5136 11.00000 0.05 0.17
Q18 1 0.5010 0.5574 0.7484 11.00000 0.05 0.17
Q19 1 0.7189 0.6858 0.8605 11.00000 0.05 0.17
Q20 1 0.7358 0.8080 0.7565 11.00000 0.05 0.17
REM The information below was added by Olex2.
REM
REM R1 = 0.0278 for 5831 Fo > 4sig(Fo) and 0.0299 for all 66024 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.47, deepest hole -0.61
REM Mean Shift 0, Max Shift -0.003.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0299
REM R1_gt = 0.0278
REM wR_ref = 0.0688
REM GOOF = 1.050
REM Shift_max = -0.003
REM Shift_mean = 0
REM Reflections_all = 66024
REM Reflections_gt = 5831
REM Parameters = n/a
REM Hole = -0.61
REM Peak = 0.47
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_Complex_2
_database_code_depnum_ccdc_archive 'CCDC 1993506'
loop_
_audit_author_name
_audit_author_address
'Krishna K. Damodaran'
;University of Iceland
Iceland
;
_audit_update_record
;
2020-03-29 deposited with the CCDC. 2020-12-09 downloaded from the CCDC.
;
_audit_creation_date 2019-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C40 H32 Cd2 N8 O6, 2(H2 O)'
_chemical_formula_sum 'C40 H36 Cd2 N8 O8'
_chemical_formula_weight 981.57
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 tetragonal
_space_group_IT_number 88
_space_group_name_H-M_alt 'I 41/a'
_space_group_name_Hall '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
_cell_length_a 29.630(2)
_cell_length_b 29.630(2)
_cell_length_c 8.9973(7)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 7899.1(14)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 9901
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 29.60
_cell_measurement_theta_min 3.07
_shelx_estimated_absorpt_T_max 0.821
_shelx_estimated_absorpt_T_min 0.671
_exptl_absorpt_coefficient_mu 1.140
_exptl_absorpt_correction_T_max 0.7459
_exptl_absorpt_correction_T_min 0.6249
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0856 before and 0.0761 after correction. The Ratio of minimum to maximum transmission is 0.8378. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.651
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description ROD
_exptl_crystal_F_000 3936
_exptl_crystal_size_max 0.38
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.18
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0865
_diffrn_reflns_av_unetI/netI 0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 41
_diffrn_reflns_limit_h_min -41
_diffrn_reflns_limit_k_max 41
_diffrn_reflns_limit_k_min -41
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 118452
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.650
_diffrn_reflns_theta_min 3.063
_diffrn_ambient_temperature 149.98
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4772
_reflns_number_total 5572
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.706
_refine_diff_density_min -1.055
_refine_diff_density_rms 0.113
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.095
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 271
_refine_ls_number_reflns 5572
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0449
_refine_ls_R_factor_gt 0.0355
_refine_ls_restrained_S_all 1.095
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+48.5240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0859
_refine_ls_wR_factor_ref 0.0888
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
2.b Idealised Me refined as rotating group:
C26(H26A,H26B,H26C)
;
_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
Cd01 Cd 0.92320(2) 0.47441(2) 0.48316(2) 0.01374(6) Uani 1 1 d . . . . .
N1 N 0.92182(8) 0.55034(9) 0.3985(3) 0.0158(5) Uani 1 1 d . . . . .
C2 C 0.88987(10) 0.58084(11) 0.4288(3) 0.0209(6) Uani 1 1 d . . . . .
H2 H 0.865870 0.572470 0.493109 0.025 Uiso 1 1 calc R . . . .
H28A H 0.7779(14) 0.5107(15) 0.722(5) 0.030(11) Uiso 1 1 d . . . . .
C3 C 0.89024(11) 0.62424(11) 0.3703(4) 0.0236(6) Uani 1 1 d . . . . .
H3 H 0.867031 0.645107 0.394439 0.028 Uiso 1 1 calc R . . . .
C4 C 0.92492(12) 0.63638(11) 0.2766(4) 0.0246(6) Uani 1 1 d . . . . .
H4 H 0.925577 0.665543 0.232754 0.030 Uiso 1 1 calc R . . . .
C5 C 0.95894(11) 0.60539(10) 0.2469(3) 0.0205(6) Uani 1 1 d . . . . .
H5 H 0.983589 0.613365 0.184734 0.025 Uiso 1 1 calc R . . . .
C6 C 0.95646(9) 0.56254(10) 0.3095(3) 0.0140(5) Uani 1 1 d . . . . .
H28B H 0.8010(19) 0.5092(18) 0.594(6) 0.058(17) Uiso 1 1 d . . . . .
C7 C 0.99124(9) 0.52775(9) 0.2821(3) 0.0127(5) Uani 1 1 d . . . . .
C8 C 1.03264(9) 0.53746(9) 0.1927(3) 0.0126(5) Uani 1 1 d . . . . .
C9 C 1.02999(10) 0.54766(10) 0.0424(3) 0.0160(5) Uani 1 1 d . . . . .
H9 H 1.001524 0.550825 -0.005066 0.019 Uiso 1 1 calc R . . . .
C10 C 1.07001(10) 0.55317(10) -0.0377(3) 0.0170(5) Uani 1 1 d . . . . .
H10 H 1.069188 0.560214 -0.140672 0.020 Uiso 1 1 calc R . . . .
C11 C 1.11069(10) 0.54823(10) 0.0347(3) 0.0183(5) Uani 1 1 d . . . . .
H11 H 1.138338 0.551519 -0.017615 0.022 Uiso 1 1 calc R . . . .
C12 C 1.11053(9) 0.53845(10) 0.1846(3) 0.0157(5) Uani 1 1 d . . . . .
H12 H 1.138690 0.535119 0.233878 0.019 Uiso 1 1 calc R . . . .
N13 N 1.07260(8) 0.53339(8) 0.2641(2) 0.0129(4) Uani 1 1 d . . . . .
N14 N 0.98397(8) 0.48788(8) 0.3349(2) 0.0127(4) Uani 1 1 d . . . . .
N15 N 1.01332(8) 0.45404(8) 0.3009(3) 0.0140(4) Uani 1 1 d . . . . .
C16 C 1.00083(9) 0.41507(9) 0.3674(3) 0.0135(5) Uani 1 1 d . . . . .
C17 C 1.02801(9) 0.37543(10) 0.3203(3) 0.0160(5) Uani 1 1 d . . . . .
C18 C 1.05960(11) 0.37836(12) 0.2047(3) 0.0222(6) Uani 1 1 d . . . . .
H18 H 1.065245 0.406691 0.158862 0.027 Uiso 1 1 calc R . . . .
C19 C 1.08274(12) 0.34030(13) 0.1564(4) 0.0303(7) Uani 1 1 d . . . . .
H19 H 1.103833 0.342601 0.077219 0.036 Uiso 1 1 calc R . . . .
C20 C 1.07494(12) 0.29873(12) 0.2242(4) 0.0318(8) Uani 1 1 d . . . . .
H20 H 1.090557 0.272590 0.191125 0.038 Uiso 1 1 calc R . . . .
C21 C 1.04427(13) 0.29569(12) 0.3404(5) 0.0338(8) Uani 1 1 d . . . . .
H21 H 1.039283 0.267480 0.387774 0.041 Uiso 1 1 calc R . . . .
C22 C 1.02085(11) 0.33361(11) 0.3876(4) 0.0244(6) Uani 1 1 d . . . . .
H22 H 0.999723 0.331082 0.466606 0.029 Uiso 1 1 calc R . . . .
O23 O 0.96967(7) 0.41007(7) 0.4615(2) 0.0191(4) Uani 1 1 d . . . . .
O24 O 0.87561(8) 0.43172(9) 0.3237(3) 0.0270(5) Uani 1 1 d . . . . .
C25 C 0.84161(10) 0.44377(11) 0.3945(3) 0.0184(6) Uani 1 1 d . . . . .
C26 C 0.79621(11) 0.42430(14) 0.3558(4) 0.0312(8) Uani 1 1 d . . . . .
H26A H 0.790346 0.428709 0.249560 0.047 Uiso 1 1 calc GR . . . .
H26B H 0.772765 0.439541 0.413914 0.047 Uiso 1 1 calc GR . . . .
H26C H 0.795958 0.391959 0.378585 0.047 Uiso 1 1 calc GR . . . .
O27 O 0.84492(8) 0.47167(9) 0.5013(3) 0.0261(5) Uani 1 1 d . . . . .
O28 O 0.78301(10) 0.52499(9) 0.6412(3) 0.0317(6) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd01 0.01052(9) 0.01972(11) 0.01097(9) 0.00215(7) 0.00125(6) -0.00035(7)
N1 0.0114(10) 0.0208(12) 0.0154(11) -0.0001(9) -0.0007(8) 0.0016(9)
C2 0.0132(13) 0.0270(16) 0.0226(14) 0.0001(12) 0.0008(10) 0.0040(11)
C3 0.0175(14) 0.0229(15) 0.0303(16) -0.0019(12) -0.0029(12) 0.0076(11)
C4 0.0272(16) 0.0180(14) 0.0288(16) 0.0037(12) 0.0003(13) 0.0037(12)
C5 0.0214(14) 0.0194(14) 0.0207(14) 0.0036(11) 0.0023(11) 0.0005(11)
C6 0.0124(12) 0.0173(13) 0.0121(11) -0.0002(9) -0.0018(9) 0.0002(10)
C7 0.0109(11) 0.0176(12) 0.0096(11) 0.0016(9) -0.0008(9) 0.0002(9)
C8 0.0126(12) 0.0128(12) 0.0124(11) -0.0008(9) 0.0008(9) -0.0007(9)
C9 0.0161(12) 0.0196(13) 0.0122(12) 0.0010(10) 0.0001(9) -0.0024(10)
C10 0.0214(14) 0.0201(13) 0.0096(11) 0.0005(10) 0.0027(10) -0.0032(10)
C11 0.0174(13) 0.0229(14) 0.0144(12) -0.0012(10) 0.0054(10) -0.0039(11)
C12 0.0121(12) 0.0181(13) 0.0169(12) -0.0016(10) 0.0028(9) -0.0002(10)
N13 0.0120(10) 0.0149(10) 0.0117(10) -0.0008(8) 0.0004(8) -0.0004(8)
N14 0.0105(10) 0.0170(11) 0.0106(10) 0.0001(8) -0.0007(8) 0.0000(8)
N15 0.0117(10) 0.0169(11) 0.0133(10) 0.0010(8) 0.0007(8) 0.0015(8)
C16 0.0122(12) 0.0159(12) 0.0123(11) -0.0012(9) -0.0024(9) -0.0007(9)
C17 0.0119(12) 0.0187(13) 0.0174(12) -0.0027(10) -0.0032(10) 0.0020(10)
C18 0.0192(14) 0.0269(16) 0.0206(14) -0.0004(12) 0.0005(11) 0.0049(12)
C19 0.0247(17) 0.038(2) 0.0285(17) -0.0057(14) 0.0037(13) 0.0120(14)
C20 0.0269(17) 0.0247(17) 0.044(2) -0.0102(15) -0.0034(15) 0.0082(13)
C21 0.0297(18) 0.0189(16) 0.053(2) -0.0025(15) 0.0002(16) 0.0032(13)
C22 0.0197(14) 0.0176(14) 0.0359(17) 0.0009(12) 0.0020(12) -0.0011(11)
O23 0.0195(10) 0.0180(10) 0.0199(10) 0.0043(8) 0.0060(8) 0.0012(8)
O24 0.0184(11) 0.0415(14) 0.0211(11) -0.0055(10) 0.0034(8) -0.0029(10)
C25 0.0138(12) 0.0262(15) 0.0151(12) 0.0060(11) -0.0022(10) -0.0034(11)
C26 0.0178(15) 0.044(2) 0.0323(18) 0.0025(15) -0.0081(13) -0.0101(14)
O27 0.0161(10) 0.0396(14) 0.0226(11) -0.0074(10) 0.0007(8) 0.0006(9)
O28 0.0379(15) 0.0298(14) 0.0273(13) 0.0004(11) 0.0057(11) 0.0101(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
Cd01 N1 2.376(3) . ?
Cd01 N13 2.289(2) 9_766 ?
Cd01 N14 2.276(2) . ?
Cd01 O23 2.360(2) . ?
Cd01 O24 2.376(2) . ?
Cd01 C25 2.703(3) . ?
Cd01 O27 2.326(2) . ?
N1 C2 1.337(4) . ?
N1 C6 1.351(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.389(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.377(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.391(4) . ?
C6 C7 1.479(4) . ?
C7 C8 1.495(4) . ?
C7 N14 1.292(3) . ?
C8 C9 1.388(4) . ?
C8 N13 1.352(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.397(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.378(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.379(4) . ?
C12 H12 0.9500 . ?
C12 N13 1.341(3) . ?
N14 N15 1.362(3) . ?
N15 C16 1.352(4) . ?
C16 C17 1.486(4) . ?
C16 O23 1.261(3) . ?
C17 C18 1.402(4) . ?
C17 C22 1.395(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.390(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.394(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.388(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.387(5) . ?
C22 H22 0.9500 . ?
O24 C25 1.244(4) . ?
C25 C26 1.505(4) . ?
C25 O27 1.271(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
O28 H28A 0.86(5) . ?
O28 H28B 0.83(6) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd01 O24 107.48(9) . . ?
N1 Cd01 C25 102.01(9) . . ?
N13 Cd01 N1 114.53(8) 9_766 . ?
N13 Cd01 O23 88.20(8) 9_766 . ?
N13 Cd01 O24 125.32(8) 9_766 . ?
N13 Cd01 C25 107.93(8) 9_766 . ?
N13 Cd01 O27 88.91(8) 9_766 . ?
N14 Cd01 N1 70.10(8) . . ?
N14 Cd01 N13 123.83(8) . 9_766 ?
N14 Cd01 O23 68.39(8) . . ?
N14 Cd01 O24 102.07(8) . . ?
N14 Cd01 C25 126.42(8) . . ?
N14 Cd01 O27 146.72(8) . . ?
O23 Cd01 N1 138.48(8) . . ?
O23 Cd01 O24 82.32(8) . . ?
O23 Cd01 C25 103.08(9) . . ?
O24 Cd01 C25 27.40(8) . . ?
O27 Cd01 N1 92.20(9) . . ?
O27 Cd01 O23 124.01(8) . . ?
O27 Cd01 O24 55.40(8) . . ?
O27 Cd01 C25 28.03(9) . . ?
C2 N1 Cd01 125.9(2) . . ?
C2 N1 C6 118.6(3) . . ?
C6 N1 Cd01 115.50(18) . . ?
N1 C2 H2 118.6 . . ?
N1 C2 C3 122.9(3) . . ?
C3 C2 H2 118.6 . . ?
C2 C3 H3 120.7 . . ?
C4 C3 C2 118.6(3) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.1(3) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 H5 120.4 . . ?
C4 C5 C6 119.2(3) . . ?
C6 C5 H5 120.4 . . ?
N1 C6 C5 121.6(3) . . ?
N1 C6 C7 116.2(2) . . ?
C5 C6 C7 122.1(3) . . ?
C6 C7 C8 121.8(2) . . ?
N14 C7 C6 117.4(2) . . ?
N14 C7 C8 120.7(2) . . ?
C9 C8 C7 121.3(2) . . ?
N13 C8 C7 116.5(2) . . ?
N13 C8 C9 122.1(3) . . ?
C8 C9 H9 120.7 . . ?
C8 C9 C10 118.7(3) . . ?
C10 C9 H9 120.7 . . ?
C9 C10 H10 120.5 . . ?
C11 C10 C9 119.1(3) . . ?
C11 C10 H10 120.5 . . ?
C10 C11 H11 120.6 . . ?
C10 C11 C12 118.8(3) . . ?
C12 C11 H11 120.6 . . ?
C11 C12 H12 118.4 . . ?
N13 C12 C11 123.2(3) . . ?
N13 C12 H12 118.4 . . ?
C8 N13 Cd01 121.88(17) . 9_766 ?
C12 N13 Cd01 119.72(18) . 9_766 ?
C12 N13 C8 118.1(2) . . ?
C7 N14 Cd01 120.54(19) . . ?
C7 N14 N15 118.9(2) . . ?
N15 N14 Cd01 120.53(17) . . ?
C16 N15 N14 110.7(2) . . ?
N15 C16 C17 113.6(2) . . ?
O23 C16 N15 126.7(3) . . ?
O23 C16 C17 119.7(3) . . ?
C18 C17 C16 121.6(3) . . ?
C22 C17 C16 119.7(3) . . ?
C22 C17 C18 118.6(3) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 C17 120.7(3) . . ?
C19 C18 H18 119.6 . . ?
C18 C19 H19 120.1 . . ?
C18 C19 C20 119.9(3) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 120.1 . . ?
C21 C20 C19 119.7(3) . . ?
C21 C20 H20 120.1 . . ?
C20 C21 H21 119.8 . . ?
C22 C21 C20 120.4(3) . . ?
C22 C21 H21 119.8 . . ?
C17 C22 H22 119.7 . . ?
C21 C22 C17 120.7(3) . . ?
C21 C22 H22 119.7 . . ?
C16 O23 Cd01 112.81(18) . . ?
C25 O24 Cd01 91.07(19) . . ?
O24 C25 Cd01 61.53(16) . . ?
O24 C25 C26 119.7(3) . . ?
O24 C25 O27 120.7(3) . . ?
C26 C25 Cd01 175.5(2) . . ?
O27 C25 Cd01 59.30(15) . . ?
O27 C25 C26 119.6(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 O27 Cd01 92.67(18) . . ?
H28A O28 H28B 106(5) . . ?
_iucr_refine_instructions_details
;
TITL mo_DT_CdOAcL2_1_1_0m_a.res in I4(1)/a
mo_dt_cdoacl2_1_1_0m_a.res
created by SHELXL-2017/1 at 12:10:34 on 31-Jul-2019
REM Old TITL mo_DT_CdOAcL2_1_1_0m in I4(1)/a
REM SHELXT solution in I4(1)/a
REM R1 0.084, Rweak 0.017, Alpha 0.061, Orientation as input
REM Formula found by SHELXT: C20 Cd N4 O4
CELL 0.71073 29.6301 29.6301 8.9973 90 90 90
ZERR 8 0.0024 0.0024 0.0007 0 0 0
LATT 2
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.75-Y,0.25+X,0.25+Z
SYMM 0.75+Y,0.75-X,0.75+Z
SFAC C H Cd N O
UNIT 320 288 16 64 64
L.S. 10
PLAN 20
SIZE 0.18 0.24 0.38
TEMP -123.17
BOND $H
LIST 6
fmap 2
acta
REM
REM
REM
WGHT 0.031000 48.524002
FVAR 0.12836
CD01 3 0.923198 0.474412 0.483155 11.00000 0.01052 0.01972 =
0.01097 0.00215 0.00125 -0.00035
N1 4 0.921820 0.550341 0.398463 11.00000 0.01136 0.02079 =
0.01535 -0.00014 -0.00073 0.00163
C2 1 0.889875 0.580836 0.428763 11.00000 0.01322 0.02703 =
0.02257 0.00011 0.00083 0.00404
AFIX 43
H2 2 0.865870 0.572470 0.493109 11.00000 -1.20000
AFIX 0
H28A 2 0.777939 0.510674 0.722431 11.00000 0.02988
C3 1 0.890236 0.624235 0.370274 11.00000 0.01754 0.02286 =
0.03034 -0.00193 -0.00290 0.00757
AFIX 43
H3 2 0.867031 0.645107 0.394439 11.00000 -1.20000
AFIX 0
C4 1 0.924922 0.636377 0.276556 11.00000 0.02718 0.01796 =
0.02879 0.00371 0.00034 0.00370
AFIX 43
H4 2 0.925577 0.665543 0.232754 11.00000 -1.20000
AFIX 0
C5 1 0.958943 0.605389 0.246950 11.00000 0.02141 0.01936 =
0.02073 0.00364 0.00233 0.00050
AFIX 43
H5 2 0.983589 0.613365 0.184734 11.00000 -1.20000
AFIX 0
C6 1 0.956463 0.562544 0.309544 11.00000 0.01241 0.01733 =
0.01215 -0.00022 -0.00182 0.00017
H28B 2 0.801045 0.509204 0.593622 11.00000 0.05817
C7 1 0.991243 0.527745 0.282074 11.00000 0.01092 0.01759 =
0.00963 0.00160 -0.00082 0.00016
C8 1 1.032640 0.537460 0.192722 11.00000 0.01264 0.01282 =
0.01236 -0.00077 0.00075 -0.00074
C9 1 1.029987 0.547655 0.042410 11.00000 0.01607 0.01961 =
0.01221 0.00101 0.00011 -0.00242
AFIX 43
H9 2 1.001524 0.550825 -0.005066 11.00000 -1.20000
AFIX 0
C10 1 1.070010 0.553166 -0.037703 11.00000 0.02139 0.02012 =
0.00961 0.00049 0.00274 -0.00317
AFIX 43
H10 2 1.069188 0.560214 -0.140672 11.00000 -1.20000
AFIX 0
C11 1 1.110687 0.548235 0.034728 11.00000 0.01739 0.02293 =
0.01442 -0.00122 0.00542 -0.00387
AFIX 43
H11 2 1.138338 0.551519 -0.017615 11.00000 -1.20000
AFIX 0
C12 1 1.110534 0.538445 0.184570 11.00000 0.01207 0.01809 =
0.01694 -0.00159 0.00279 -0.00023
AFIX 43
H12 2 1.138690 0.535119 0.233878 11.00000 -1.20000
AFIX 0
N13 4 1.072603 0.533392 0.264065 11.00000 0.01202 0.01494 =
0.01174 -0.00077 0.00035 -0.00042
N14 4 0.983968 0.487877 0.334936 11.00000 0.01050 0.01697 =
0.01059 0.00006 -0.00074 -0.00001
N15 4 1.013322 0.454040 0.300851 11.00000 0.01173 0.01689 =
0.01329 0.00096 0.00073 0.00152
C16 1 1.000831 0.415072 0.367444 11.00000 0.01223 0.01586 =
0.01229 -0.00121 -0.00239 -0.00069
C17 1 1.028012 0.375434 0.320316 11.00000 0.01187 0.01873 =
0.01735 -0.00269 -0.00323 0.00199
C18 1 1.059597 0.378364 0.204692 11.00000 0.01916 0.02691 =
0.02061 -0.00043 0.00048 0.00491
AFIX 43
H18 2 1.065245 0.406691 0.158862 11.00000 -1.20000
AFIX 0
C19 1 1.082737 0.340297 0.156368 11.00000 0.02473 0.03771 =
0.02848 -0.00568 0.00371 0.01196
AFIX 43
H19 2 1.103833 0.342601 0.077219 11.00000 -1.20000
AFIX 0
C20 1 1.074942 0.298725 0.224233 11.00000 0.02693 0.02472 =
0.04378 -0.01016 -0.00337 0.00823
AFIX 43
H20 2 1.090557 0.272590 0.191125 11.00000 -1.20000
AFIX 0
C21 1 1.044272 0.295690 0.340357 11.00000 0.02965 0.01891 =
0.05281 -0.00248 0.00024 0.00315
AFIX 43
H21 2 1.039283 0.267480 0.387774 11.00000 -1.20000
AFIX 0
C22 1 1.020850 0.333613 0.387622 11.00000 0.01966 0.01765 =
0.03586 0.00090 0.00201 -0.00109
AFIX 43
H22 2 0.999723 0.331082 0.466606 11.00000 -1.20000
AFIX 0
O23 5 0.969668 0.410074 0.461539 11.00000 0.01949 0.01798 =
0.01986 0.00431 0.00600 0.00120
O24 5 0.875607 0.431717 0.323736 11.00000 0.01839 0.04150 =
0.02114 -0.00551 0.00342 -0.00289
C25 1 0.841611 0.443774 0.394513 11.00000 0.01379 0.02624 =
0.01506 0.00601 -0.00222 -0.00341
C26 1 0.796212 0.424298 0.355765 11.00000 0.01778 0.04367 =
0.03226 0.00253 -0.00806 -0.01008
AFIX 137
H26A 2 0.790346 0.428709 0.249560 11.00000 -1.50000
H26B 2 0.772765 0.439541 0.413914 11.00000 -1.50000
H26C 2 0.795958 0.391959 0.378585 11.00000 -1.50000
AFIX 0
O27 5 0.844922 0.471670 0.501306 11.00000 0.01609 0.03961 =
0.02263 -0.00735 0.00066 0.00058
O28 5 0.783014 0.524989 0.641184 11.00000 0.03790 0.02977 =
0.02734 0.00036 0.00565 0.01013
HKLF 4
REM mo_DT_CdOAcL2_1_1_0m_a.res in I4(1)/a
REM R1 = 0.0355 for 4772 Fo > 4sig(Fo) and 0.0449 for all 5572 data
REM 271 parameters refined using 0 restraints
END
WGHT 0.0310 48.5011
REM Highest difference peak 0.706, deepest hole -1.055, 1-sigma level 0.113
Q1 1 0.9499 0.4486 0.4886 11.00000 0.05 0.71
Q2 1 0.8973 0.4492 0.4734 11.00000 0.05 0.70
Q3 1 0.8910 0.5081 0.4439 11.00000 0.05 0.60
Q4 1 1.1089 0.5209 -0.0734 11.00000 0.05 0.59
Q5 1 0.9221 0.4767 0.4001 11.00000 0.05 0.56
Q6 1 0.7831 0.4199 0.4734 11.00000 0.05 0.56
Q7 1 1.0313 0.5417 0.1186 11.00000 0.05 0.56
Q8 1 1.0438 0.5197 -0.0719 11.00000 0.05 0.52
Q9 1 0.9614 0.2994 0.4556 11.00000 0.05 0.51
Q10 1 1.0509 0.5211 -0.0140 11.00000 0.05 0.51
Q11 1 1.1121 0.5423 0.1060 11.00000 0.05 0.50
Q12 1 0.8898 0.5032 0.5097 11.00000 0.05 0.46
Q13 1 1.0799 0.4878 -0.0656 11.00000 0.05 0.45
Q14 1 1.0126 0.5321 0.2469 11.00000 0.05 0.43
Q15 1 0.9512 0.5086 0.4421 11.00000 0.05 0.43
Q16 1 1.0725 0.5491 -0.0954 11.00000 0.05 0.43
Q17 1 1.0496 0.5368 0.0054 11.00000 0.05 0.42
Q18 1 0.8189 0.4302 0.3730 11.00000 0.05 0.42
Q19 1 1.0408 0.4617 0.2730 11.00000 0.05 0.41
Q20 1 0.9674 0.3316 0.5208 11.00000 0.05 0.41
REM The information below was added by Olex2.
REM
REM R1 = 0.0355 for 4772 Fo > 4sig(Fo) and 0.0449 for all 122190 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.71, deepest hole -1.06
REM Mean Shift 0, Max Shift 0.004.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0449
REM R1_gt = 0.0355
REM wR_ref = 0.0888
REM GOOF = 1.095
REM Shift_max = 0.004
REM Shift_mean = 0
REM Reflections_all = 122190
REM Reflections_gt = 4772
REM Parameters = n/a
REM Hole = -1.06
REM Peak = 0.71
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_Complex_5
_database_code_depnum_ccdc_archive 'CCDC 1993508'
loop_
_audit_author_name
_audit_author_address
'Krishna K. Damodaran'
;University of Iceland
Iceland
;
_audit_update_record
;
2020-03-29 deposited with the CCDC. 2020-12-09 downloaded from the CCDC.
;
_audit_creation_date 2019-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H30 N10 O2 Zn, 2(N O3)'
_chemical_formula_sum 'C36 H30 N12 O8 Zn'
_chemical_formula_weight 824.09
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 13.4129(8)
_cell_length_b 18.8966(12)
_cell_length_c 15.1602(9)
_cell_angle_alpha 90
_cell_angle_beta 113.177(2)
_cell_angle_gamma 90
_cell_volume 3532.4(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9899
_cell_measurement_temperature 121(2)
_cell_measurement_theta_max 28.87
_cell_measurement_theta_min 2.94
_shelx_estimated_absorpt_T_max 0.900
_shelx_estimated_absorpt_T_min 0.861
_exptl_absorpt_coefficient_mu 0.769
_exptl_absorpt_correction_T_max 0.7458
_exptl_absorpt_correction_T_min 0.7025
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0582 before and 0.0491 after correction. The Ratio of minimum to maximum transmission is 0.9419. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.550
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 1696
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.185
_exptl_crystal_size_min 0.14
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0744
_diffrn_reflns_av_unetI/netI 0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 105076
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.903
_diffrn_reflns_theta_min 2.939
_diffrn_ambient_temperature 120.78
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7355
_reflns_number_total 9280
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT V8.38A (?, 2016)'
_computing_data_collection 'SAINT V8.38A (?, 2016)'
_computing_data_reduction 'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max 0.690
_refine_diff_density_min -0.485
_refine_diff_density_rms 0.058
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.018
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 514
_refine_ls_number_reflns 9280
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0533
_refine_ls_R_factor_gt 0.0338
_refine_ls_restrained_S_all 1.018
_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^)+(0.0372P)^2^+1.6351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0744
_refine_ls_wR_factor_ref 0.0794
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C12(H12), C11(H11), C10(H10),
N15(H15), N17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26),
C27(H27), C28(H28), C29(H29), C33(H33), C34(H34), C35(H35), C36(H36),
N39(H39), N41(H41), C45(H45), C44(H44), C43(H43), C46(H46), C47(H47)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.25106(2) 0.54618(2) 0.72899(2) 0.01262(5) Uani 1 1 d . . . . .
N1 N 0.25410(10) 0.65613(7) 0.75440(9) 0.0147(2) Uani 1 1 d . . . . .
C2 C 0.16740(13) 0.69822(9) 0.71581(12) 0.0191(3) Uani 1 1 d . . . . .
H2 H 0.104921 0.680264 0.665005 0.023 Uiso 1 1 calc R . . . .
C3 C 0.16505(14) 0.76707(9) 0.74700(13) 0.0256(4) Uani 1 1 d . . . . .
H3 H 0.103845 0.796604 0.716007 0.031 Uiso 1 1 calc R . . . .
C4 C 0.25410(14) 0.79153(9) 0.82435(13) 0.0252(4) Uani 1 1 d . . . . .
H4 H 0.254397 0.838133 0.847944 0.030 Uiso 1 1 calc R . . . .
C6 C 0.34244(12) 0.68071(8) 0.82885(10) 0.0143(3) Uani 1 1 d . . . . .
C5 C 0.34301(13) 0.74754(9) 0.86726(12) 0.0200(3) Uani 1 1 d . . . . .
H5 H 0.403425 0.762911 0.922130 0.024 Uiso 1 1 calc R . . . .
C7 C 0.43473(12) 0.63034(8) 0.86801(10) 0.0142(3) Uani 1 1 d . . . . .
C8 C 0.54793(12) 0.65349(8) 0.92541(10) 0.0159(3) Uani 1 1 d . . . . .
C9 C 0.58604(13) 0.72040(9) 0.91525(12) 0.0201(3) Uani 1 1 d . . . . .
H9 H 0.538907 0.754348 0.873030 0.024 Uiso 1 1 calc R . . . .
C12 C 0.71791(13) 0.61937(10) 1.03144(12) 0.0226(3) Uani 1 1 d . . . . .
H12 H 0.764624 0.583974 1.070872 0.027 Uiso 1 1 calc R . . . .
C11 C 0.76117(14) 0.68543(10) 1.02737(12) 0.0260(4) Uani 1 1 d . . . . .
H11 H 0.835384 0.695342 1.064658 0.031 Uiso 1 1 calc R . . . .
C10 C 0.69455(14) 0.73633(10) 0.96829(12) 0.0250(4) Uani 1 1 d . . . . .
H10 H 0.722389 0.781804 0.963796 0.030 Uiso 1 1 calc R . . . .
N13 N 0.61340(11) 0.60332(7) 0.98235(9) 0.0181(3) Uani 1 1 d . . . . .
C16 C 0.42521(12) 0.44539(8) 0.83339(10) 0.0143(3) Uani 1 1 d . . . . .
N15 N 0.47291(10) 0.50975(7) 0.87077(9) 0.0155(3) Uani 1 1 d . . . . .
H15 H 0.541760 0.513817 0.909153 0.019 Uiso 1 1 calc R . . . .
N14 N 0.40511(10) 0.56541(7) 0.84342(9) 0.0136(2) Uani 1 1 d . . . . .
N17 N 0.49284(10) 0.39008(7) 0.86360(9) 0.0148(2) Uani 1 1 d . . . . .
H17 H 0.559816 0.399580 0.903096 0.018 Uiso 1 1 calc R . . . .
C18 C 0.46825(12) 0.31815(8) 0.83888(10) 0.0150(3) Uani 1 1 d . . . . .
C19 C 0.55592(13) 0.27364(9) 0.85140(11) 0.0184(3) Uani 1 1 d . . . . .
H19 H 0.627311 0.292327 0.872768 0.022 Uiso 1 1 calc R . . . .
C20 C 0.53783(14) 0.20174(9) 0.83232(12) 0.0219(3) Uani 1 1 d . . . . .
H20 H 0.597299 0.171241 0.841081 0.026 Uiso 1 1 calc R . . . .
C21 C 0.43350(15) 0.17407(9) 0.80052(12) 0.0233(3) Uani 1 1 d . . . . .
H21 H 0.421571 0.124953 0.787172 0.028 Uiso 1 1 calc R . . . .
C22 C 0.34687(14) 0.21869(9) 0.78842(12) 0.0206(3) Uani 1 1 d . . . . .
H22 H 0.275510 0.199907 0.766703 0.025 Uiso 1 1 calc R . . . .
C23 C 0.36366(13) 0.29075(9) 0.80782(11) 0.0175(3) Uani 1 1 d . . . . .
H23 H 0.304161 0.320992 0.799914 0.021 Uiso 1 1 calc R . . . .
N25 N 0.12014(10) 0.52756(7) 0.77246(9) 0.0141(2) Uani 1 1 d . . . . .
O24 O 0.32908(9) 0.44276(6) 0.77585(8) 0.0166(2) Uani 1 1 d . . . . .
C26 C 0.10329(13) 0.55941(9) 0.84422(11) 0.0177(3) Uani 1 1 d . . . . .
H26 H 0.147932 0.598360 0.875628 0.021 Uiso 1 1 calc R . . . .
C27 C 0.02288(14) 0.53765(10) 0.87456(12) 0.0244(4) Uani 1 1 d . . . . .
H27 H 0.012762 0.561326 0.925699 0.029 Uiso 1 1 calc R . . . .
C28 C -0.04202(14) 0.48097(11) 0.82895(12) 0.0269(4) Uani 1 1 d . . . . .
H28 H -0.096108 0.464162 0.849519 0.032 Uiso 1 1 calc R . . . .
C29 C -0.02708(13) 0.44893(10) 0.75263(12) 0.0219(3) Uani 1 1 d . . . . .
H29 H -0.071775 0.410515 0.719394 0.026 Uiso 1 1 calc R . . . .
C30 C 0.05391(12) 0.47377(8) 0.72564(10) 0.0142(3) Uani 1 1 d . . . . .
C31 C 0.07282(12) 0.44372(8) 0.64301(10) 0.0130(3) Uani 1 1 d . . . . .
C32 C 0.02007(12) 0.37599(8) 0.59806(10) 0.0147(3) Uani 1 1 d . . . . .
C33 C 0.08164(15) 0.31505(9) 0.61380(12) 0.0237(3) Uani 1 1 d . . . . .
H33 H 0.158004 0.316613 0.648458 0.028 Uiso 1 1 calc R . . . .
C34 C 0.02958(17) 0.25154(10) 0.57793(13) 0.0301(4) Uani 1 1 d . . . . .
H34 H 0.069469 0.208607 0.588647 0.036 Uiso 1 1 calc R . . . .
C35 C -0.08118(16) 0.25188(10) 0.52640(12) 0.0286(4) Uani 1 1 d . . . . .
H35 H -0.119271 0.209284 0.500951 0.034 Uiso 1 1 calc R . . . .
C36 C -0.13526(15) 0.31585(10) 0.51277(13) 0.0264(4) Uani 1 1 d . . . . .
H36 H -0.211290 0.315909 0.476137 0.032 Uiso 1 1 calc R . . . .
N37 N -0.08746(11) 0.37767(8) 0.54784(10) 0.0206(3) Uani 1 1 d . . . . .
N38 N 0.14230(10) 0.47884(7) 0.62180(9) 0.0135(2) Uani 1 1 d . . . . .
N39 N 0.17290(10) 0.46172(7) 0.54980(9) 0.0147(2) Uani 1 1 d . . . . .
H39 H 0.145795 0.425735 0.510831 0.018 Uiso 1 1 calc R . . . .
C40 C 0.25161(12) 0.50673(8) 0.54351(10) 0.0134(3) Uani 1 1 d . . . . .
C42 C 0.34596(12) 0.53054(8) 0.43500(10) 0.0139(3) Uani 1 1 d . . . . .
N41 N 0.26987(10) 0.49634(7) 0.46339(9) 0.0147(2) Uani 1 1 d . . . . .
H41 H 0.229155 0.464093 0.423582 0.018 Uiso 1 1 calc R . . . .
C45 C 0.49570(13) 0.58901(9) 0.37004(12) 0.0204(3) Uani 1 1 d . . . . .
H45 H 0.547010 0.608745 0.348153 0.024 Uiso 1 1 calc R . . . .
C44 C 0.41357(14) 0.54533(9) 0.31066(11) 0.0208(3) Uani 1 1 d . . . . .
H44 H 0.408717 0.535258 0.247706 0.025 Uiso 1 1 calc R . . . .
C43 C 0.33854(13) 0.51621(9) 0.34209(11) 0.0180(3) Uani 1 1 d . . . . .
H43 H 0.282287 0.486635 0.300715 0.022 Uiso 1 1 calc R . . . .
C46 C 0.50197(13) 0.60356(8) 0.46212(12) 0.0180(3) Uani 1 1 d . . . . .
H46 H 0.557686 0.633687 0.503050 0.022 Uiso 1 1 calc R . . . .
N50 N 0.10720(11) 0.34594(8) 0.34655(10) 0.0211(3) Uani 1 1 d . . . . .
O49 O 0.07713(13) 0.35734(9) 0.41342(10) 0.0483(5) Uani 1 1 d . . . . .
O48 O 0.29855(8) 0.54987(6) 0.60842(7) 0.0145(2) Uani 1 1 d . . . . .
C47 C 0.42751(12) 0.57446(8) 0.49483(11) 0.0154(3) Uani 1 1 d . . . . .
H47 H 0.432457 0.584595 0.557799 0.018 Uiso 1 1 calc R . . . .
O51 O 0.07559(11) 0.29279(7) 0.29586(10) 0.0335(3) Uani 1 1 d . . . . .
O52 O 0.16906(13) 0.38884(8) 0.33210(11) 0.0425(4) Uani 1 1 d . . . . .
N54 N 0.75140(11) 0.44895(9) 0.93497(10) 0.0236(3) Uani 1 1 d . . . . .
O55 O 0.68796(10) 0.44560(8) 0.97943(9) 0.0296(3) Uani 1 1 d . . . . .
O56 O 0.79176(12) 0.39429(7) 0.91840(10) 0.0347(3) Uani 1 1 d . . . . .
O53 O 0.77236(14) 0.50745(8) 0.91005(11) 0.0419(4) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.01213(8) 0.01086(8) 0.01518(8) -0.00236(7) 0.00572(6) -0.00197(7)
N1 0.0156(6) 0.0126(6) 0.0176(6) -0.0014(5) 0.0084(5) -0.0015(5)
C2 0.0171(7) 0.0160(7) 0.0238(7) -0.0025(6) 0.0077(6) -0.0007(6)
C3 0.0219(8) 0.0168(8) 0.0349(9) -0.0018(7) 0.0078(7) 0.0046(7)
C4 0.0252(8) 0.0138(7) 0.0371(9) -0.0083(7) 0.0127(7) -0.0005(7)
C6 0.0147(7) 0.0127(7) 0.0171(7) -0.0007(6) 0.0079(6) -0.0014(5)
C5 0.0194(7) 0.0152(7) 0.0257(8) -0.0066(6) 0.0091(6) -0.0038(6)
C7 0.0152(7) 0.0141(7) 0.0152(6) -0.0018(5) 0.0081(5) -0.0019(6)
C8 0.0160(7) 0.0177(7) 0.0160(6) -0.0040(6) 0.0085(6) -0.0022(6)
C9 0.0201(8) 0.0174(7) 0.0226(7) -0.0031(6) 0.0083(6) -0.0042(6)
C12 0.0179(8) 0.0277(9) 0.0204(7) -0.0048(7) 0.0055(6) 0.0003(7)
C11 0.0153(7) 0.0344(10) 0.0259(8) -0.0105(8) 0.0056(6) -0.0073(7)
C10 0.0231(8) 0.0247(9) 0.0289(8) -0.0095(7) 0.0120(7) -0.0114(7)
N13 0.0161(6) 0.0212(7) 0.0166(6) -0.0042(5) 0.0059(5) -0.0010(5)
C16 0.0161(7) 0.0137(7) 0.0160(6) 0.0007(6) 0.0093(5) -0.0001(6)
N15 0.0136(6) 0.0125(6) 0.0189(6) -0.0001(5) 0.0048(5) 0.0000(5)
N14 0.0138(6) 0.0126(6) 0.0161(6) -0.0004(5) 0.0076(5) 0.0002(5)
N17 0.0128(6) 0.0129(6) 0.0183(6) 0.0002(5) 0.0055(5) 0.0008(5)
C18 0.0188(7) 0.0130(7) 0.0154(6) 0.0029(5) 0.0093(6) 0.0026(6)
C19 0.0187(7) 0.0181(7) 0.0207(7) 0.0044(6) 0.0103(6) 0.0043(6)
C20 0.0264(8) 0.0172(8) 0.0252(8) 0.0056(7) 0.0136(7) 0.0088(7)
C21 0.0339(9) 0.0132(7) 0.0243(8) 0.0018(6) 0.0133(7) 0.0026(7)
C22 0.0231(8) 0.0171(8) 0.0223(8) 0.0022(6) 0.0097(6) -0.0022(6)
C23 0.0173(7) 0.0164(7) 0.0200(7) 0.0018(6) 0.0087(6) 0.0030(6)
N25 0.0134(6) 0.0145(6) 0.0143(5) -0.0001(5) 0.0054(5) 0.0005(5)
O24 0.0148(5) 0.0122(5) 0.0207(5) 0.0003(4) 0.0045(4) 0.0005(4)
C26 0.0179(7) 0.0196(8) 0.0147(6) -0.0013(6) 0.0053(6) 0.0020(6)
C27 0.0231(8) 0.0350(10) 0.0181(7) -0.0028(7) 0.0114(6) 0.0023(7)
C28 0.0223(8) 0.0400(10) 0.0249(8) -0.0019(8) 0.0162(7) -0.0045(8)
C29 0.0190(7) 0.0270(9) 0.0220(7) -0.0030(7) 0.0106(6) -0.0077(7)
C30 0.0129(6) 0.0150(7) 0.0150(6) 0.0010(5) 0.0059(5) 0.0001(5)
C31 0.0119(6) 0.0131(7) 0.0139(6) -0.0002(5) 0.0048(5) -0.0006(5)
C32 0.0160(7) 0.0141(7) 0.0144(6) -0.0008(6) 0.0064(5) -0.0036(6)
C33 0.0243(8) 0.0179(8) 0.0232(8) -0.0014(7) 0.0033(7) 0.0010(7)
C34 0.0423(11) 0.0147(8) 0.0283(9) -0.0005(7) 0.0085(8) 0.0013(8)
C35 0.0411(11) 0.0185(8) 0.0244(8) -0.0051(7) 0.0111(8) -0.0146(8)
C36 0.0233(8) 0.0286(9) 0.0252(8) -0.0070(7) 0.0072(7) -0.0121(7)
N37 0.0158(6) 0.0215(7) 0.0224(6) -0.0040(6) 0.0051(5) -0.0042(5)
N38 0.0138(6) 0.0136(6) 0.0144(5) -0.0003(5) 0.0071(5) 0.0003(5)
N39 0.0178(6) 0.0137(6) 0.0157(6) -0.0044(5) 0.0099(5) -0.0046(5)
C40 0.0129(6) 0.0107(6) 0.0170(6) 0.0011(5) 0.0064(5) 0.0013(5)
C42 0.0151(7) 0.0120(7) 0.0174(7) 0.0040(5) 0.0092(6) 0.0036(5)
N41 0.0156(6) 0.0148(6) 0.0157(6) -0.0027(5) 0.0085(5) -0.0024(5)
C45 0.0214(8) 0.0192(8) 0.0254(8) 0.0073(7) 0.0145(7) 0.0019(6)
C44 0.0257(8) 0.0224(8) 0.0184(7) 0.0039(6) 0.0132(6) 0.0031(7)
C43 0.0182(7) 0.0200(7) 0.0170(7) 0.0009(6) 0.0082(6) 0.0010(6)
C46 0.0188(7) 0.0126(7) 0.0246(8) 0.0032(6) 0.0106(6) 0.0006(6)
N50 0.0187(6) 0.0209(7) 0.0204(6) -0.0031(6) 0.0042(5) -0.0012(6)
O49 0.0514(9) 0.0712(12) 0.0349(7) -0.0344(8) 0.0306(7) -0.0417(9)
O48 0.0160(5) 0.0128(5) 0.0162(5) -0.0023(4) 0.0080(4) -0.0027(4)
C47 0.0177(7) 0.0128(6) 0.0175(7) 0.0008(6) 0.0089(6) 0.0021(6)
O51 0.0345(7) 0.0275(7) 0.0356(7) -0.0159(6) 0.0106(6) -0.0109(6)
O52 0.0586(10) 0.0358(8) 0.0489(9) -0.0220(7) 0.0384(8) -0.0259(8)
N54 0.0172(6) 0.0331(8) 0.0198(6) -0.0016(6) 0.0064(5) 0.0005(6)
O55 0.0168(6) 0.0471(9) 0.0259(6) -0.0002(6) 0.0095(5) -0.0028(6)
O56 0.0417(8) 0.0241(7) 0.0420(8) 0.0025(6) 0.0206(7) 0.0094(6)
O53 0.0639(11) 0.0262(7) 0.0534(9) 0.0028(7) 0.0423(8) 0.0031(7)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N1 2.1105(13) . ?
Zn1 N14 2.1423(13) . ?
Zn1 N25 2.1336(13) . ?
Zn1 O24 2.1986(11) . ?
Zn1 N38 2.1265(13) . ?
Zn1 O48 2.1606(10) . ?
N1 C2 1.339(2) . ?
N1 C6 1.3569(19) . ?
C2 H2 0.9500 . ?
C2 C3 1.389(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.383(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.388(2) . ?
C6 C5 1.389(2) . ?
C6 C7 1.487(2) . ?
C5 H5 0.9500 . ?
C7 C8 1.488(2) . ?
C7 N14 1.2983(19) . ?
C8 C9 1.395(2) . ?
C8 N13 1.348(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.391(2) . ?
C12 H12 0.9500 . ?
C12 C11 1.388(2) . ?
C12 N13 1.338(2) . ?
C11 H11 0.9500 . ?
C11 C10 1.377(3) . ?
C10 H10 0.9500 . ?
C16 N15 1.3871(19) . ?
C16 N17 1.3408(19) . ?
C16 O24 1.2412(18) . ?
N15 H15 0.8800 . ?
N15 N14 1.3448(17) . ?
N17 H17 0.8800 . ?
N17 C18 1.4140(19) . ?
C18 C19 1.397(2) . ?
C18 C23 1.392(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.390(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.390(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.388(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.393(2) . ?
C23 H23 0.9500 . ?
N25 C26 1.3381(19) . ?
N25 C30 1.3526(19) . ?
C26 H26 0.9500 . ?
C26 C27 1.391(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.382(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.389(2) . ?
C29 H29 0.9500 . ?
C29 C30 1.385(2) . ?
C30 C31 1.485(2) . ?
C31 C32 1.491(2) . ?
C31 N38 1.2837(18) . ?
C32 C33 1.382(2) . ?
C32 N37 1.3403(19) . ?
C33 H33 0.9500 . ?
C33 C34 1.387(2) . ?
C34 H34 0.9500 . ?
C34 C35 1.380(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.383(3) . ?
C36 H36 0.9500 . ?
C36 N37 1.338(2) . ?
N38 N39 1.3481(16) . ?
N39 H39 0.8800 . ?
N39 C40 1.3878(18) . ?
C40 N41 1.3446(18) . ?
C40 O48 1.2417(17) . ?
C42 N41 1.4108(19) . ?
C42 C43 1.399(2) . ?
C42 C47 1.388(2) . ?
N41 H41 0.8800 . ?
C45 H45 0.9500 . ?
C45 C44 1.387(2) . ?
C45 C46 1.393(2) . ?
C44 H44 0.9500 . ?
C44 C43 1.386(2) . ?
C43 H43 0.9500 . ?
C46 H46 0.9500 . ?
C46 C47 1.391(2) . ?
N50 O49 1.2485(19) . ?
N50 O51 1.2339(18) . ?
N50 O52 1.2397(19) . ?
C47 H47 0.9500 . ?
N54 O55 1.2783(18) . ?
N54 O56 1.2368(19) . ?
N54 O53 1.236(2) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Zn1 N14 75.05(5) . . ?
N1 Zn1 N25 93.73(5) . . ?
N1 Zn1 O24 147.51(4) . . ?
N1 Zn1 N38 133.37(5) . . ?
N1 Zn1 O48 97.57(4) . . ?
N14 Zn1 O24 72.80(4) . . ?
N14 Zn1 O48 99.67(4) . . ?
N25 Zn1 N14 115.25(5) . . ?
N25 Zn1 O24 95.66(5) . . ?
N25 Zn1 O48 145.00(4) . . ?
N38 Zn1 N14 150.84(5) . . ?
N38 Zn1 N25 74.75(5) . . ?
N38 Zn1 O24 79.12(4) . . ?
N38 Zn1 O48 73.43(4) . . ?
O48 Zn1 O24 92.33(4) . . ?
C2 N1 Zn1 123.65(11) . . ?
C2 N1 C6 118.96(13) . . ?
C6 N1 Zn1 115.90(10) . . ?
N1 C2 H2 118.7 . . ?
N1 C2 C3 122.69(15) . . ?
C3 C2 H2 118.7 . . ?
C2 C3 H3 120.9 . . ?
C4 C3 C2 118.29(16) . . ?
C4 C3 H3 120.9 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.56(15) . . ?
C5 C4 H4 120.2 . . ?
N1 C6 C5 121.25(14) . . ?
N1 C6 C7 115.47(13) . . ?
C5 C6 C7 123.23(14) . . ?
C4 C5 C6 119.08(15) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C6 C7 C8 122.87(13) . . ?
N14 C7 C6 112.19(13) . . ?
N14 C7 C8 124.91(14) . . ?
C9 C8 C7 122.41(14) . . ?
N13 C8 C7 115.17(14) . . ?
N13 C8 C9 122.22(14) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 C8 118.56(16) . . ?
C10 C9 H9 120.7 . . ?
C11 C12 H12 118.5 . . ?
N13 C12 H12 118.5 . . ?
N13 C12 C11 122.96(16) . . ?
C12 C11 H11 120.6 . . ?
C10 C11 C12 118.78(15) . . ?
C10 C11 H11 120.6 . . ?
C9 C10 H10 120.4 . . ?
C11 C10 C9 119.24(16) . . ?
C11 C10 H10 120.4 . . ?
C12 N13 C8 118.20(15) . . ?
N17 C16 N15 113.75(13) . . ?
O24 C16 N15 120.44(14) . . ?
O24 C16 N17 125.79(14) . . ?
C16 N15 H15 122.8 . . ?
N14 N15 C16 114.37(12) . . ?
N14 N15 H15 122.8 . . ?
C7 N14 Zn1 118.78(10) . . ?
C7 N14 N15 123.87(13) . . ?
N15 N14 Zn1 115.89(9) . . ?
C16 N17 H17 116.5 . . ?
C16 N17 C18 127.08(13) . . ?
C18 N17 H17 116.5 . . ?
C19 C18 N17 116.54(14) . . ?
C23 C18 N17 123.10(14) . . ?
C23 C18 C19 120.29(15) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 C18 119.45(15) . . ?
C20 C19 H19 120.3 . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.59(15) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 120.2 . . ?
C22 C21 C20 119.56(16) . . ?
C22 C21 H21 120.2 . . ?
C21 C22 H22 119.7 . . ?
C21 C22 C23 120.58(16) . . ?
C23 C22 H22 119.7 . . ?
C18 C23 C22 119.52(15) . . ?
C18 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C26 N25 Zn1 126.86(11) . . ?
C26 N25 C30 118.58(14) . . ?
C30 N25 Zn1 114.35(10) . . ?
C16 O24 Zn1 114.98(10) . . ?
N25 C26 H26 118.8 . . ?
N25 C26 C27 122.48(15) . . ?
C27 C26 H26 118.8 . . ?
C26 C27 H27 120.6 . . ?
C28 C27 C26 118.79(15) . . ?
C28 C27 H27 120.6 . . ?
C27 C28 H28 120.5 . . ?
C27 C28 C29 119.06(16) . . ?
C29 C28 H28 120.5 . . ?
C28 C29 H29 120.5 . . ?
C30 C29 C28 119.05(16) . . ?
C30 C29 H29 120.5 . . ?
N25 C30 C29 121.96(14) . . ?
N25 C30 C31 115.78(13) . . ?
C29 C30 C31 122.26(14) . . ?
C30 C31 C32 120.38(13) . . ?
N38 C31 C30 113.29(13) . . ?
N38 C31 C32 126.15(13) . . ?
C33 C32 C31 119.50(14) . . ?
N37 C32 C31 116.76(14) . . ?
N37 C32 C33 123.65(15) . . ?
C32 C33 H33 120.7 . . ?
C32 C33 C34 118.61(16) . . ?
C34 C33 H33 120.7 . . ?
C33 C34 H34 120.6 . . ?
C35 C34 C33 118.79(17) . . ?
C35 C34 H34 120.6 . . ?
C34 C35 H35 120.9 . . ?
C34 C35 C36 118.24(16) . . ?
C36 C35 H35 120.9 . . ?
C35 C36 H36 117.9 . . ?
N37 C36 C35 124.24(17) . . ?
N37 C36 H36 117.9 . . ?
C36 N37 C32 116.45(15) . . ?
C31 N38 Zn1 117.72(10) . . ?
C31 N38 N39 124.13(13) . . ?
N39 N38 Zn1 115.24(9) . . ?
N38 N39 H39 123.5 . . ?
N38 N39 C40 113.00(12) . . ?
C40 N39 H39 123.5 . . ?
N41 C40 N39 112.73(13) . . ?
O48 C40 N39 120.68(13) . . ?
O48 C40 N41 126.58(14) . . ?
C43 C42 N41 116.43(14) . . ?
C47 C42 N41 123.58(13) . . ?
C47 C42 C43 119.95(14) . . ?
C40 N41 C42 128.29(13) . . ?
C40 N41 H41 115.9 . . ?
C42 N41 H41 115.9 . . ?
C44 C45 H45 120.4 . . ?
C44 C45 C46 119.16(15) . . ?
C46 C45 H45 120.4 . . ?
C45 C44 H44 119.6 . . ?
C43 C44 C45 120.79(15) . . ?
C43 C44 H44 119.6 . . ?
C42 C43 H43 120.1 . . ?
C44 C43 C42 119.72(15) . . ?
C44 C43 H43 120.1 . . ?
C45 C46 H46 119.6 . . ?
C47 C46 C45 120.71(15) . . ?
C47 C46 H46 119.6 . . ?
O51 N50 O49 120.30(15) . . ?
O51 N50 O52 120.80(15) . . ?
O52 N50 O49 118.90(14) . . ?
C40 O48 Zn1 115.02(9) . . ?
C42 C47 C46 119.67(14) . . ?
C42 C47 H47 120.2 . . ?
C46 C47 H47 120.2 . . ?
O56 N54 O55 120.07(16) . . ?
O53 N54 O55 118.96(16) . . ?
O53 N54 O56 120.96(15) . . ?
_iucr_refine_instructions_details
;
TITL DT_ZnNO3L1_1_0m_a.res in P2(1)/c
dt_znno3l1_1_0m_a.res
created by SHELXL-2017/1 at 16:13:43 on 01-Aug-2019
CELL 0.71073 13.4129 18.8966 15.1602 90 113.177 90
ZERR 4 0.0008 0.0012 0.0009 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O Zn
UNIT 144 120 48 32 4
L.S. 10
PLAN 20
SIZE 0.14 0.185 0.2
TEMP -152.37
BOND $H
LIST 6
fmap 2
acta
REM
REM
REM
WGHT 0.037200 1.635100
FVAR 0.25169
ZN1 5 0.251055 0.546181 0.728988 11.00000 0.01213 0.01086 =
0.01518 -0.00236 0.00572 -0.00197
N1 3 0.254097 0.656126 0.754403 11.00000 0.01556 0.01260 =
0.01759 -0.00138 0.00836 -0.00146
C2 1 0.167399 0.698218 0.715809 11.00000 0.01711 0.01597 =
0.02379 -0.00249 0.00774 -0.00075
AFIX 43
H2 2 0.104921 0.680264 0.665005 11.00000 -1.20000
AFIX 0
C3 1 0.165047 0.767071 0.747002 11.00000 0.02191 0.01681 =
0.03489 -0.00182 0.00781 0.00465
AFIX 43
H3 2 0.103845 0.796604 0.716007 11.00000 -1.20000
AFIX 0
C4 1 0.254098 0.791527 0.824347 11.00000 0.02524 0.01378 =
0.03708 -0.00833 0.01270 -0.00055
AFIX 43
H4 2 0.254397 0.838133 0.847944 11.00000 -1.20000
AFIX 0
C6 1 0.342439 0.680713 0.828852 11.00000 0.01466 0.01268 =
0.01706 -0.00071 0.00792 -0.00142
C5 1 0.343006 0.747542 0.867255 11.00000 0.01938 0.01521 =
0.02570 -0.00661 0.00912 -0.00378
AFIX 43
H5 2 0.403425 0.762911 0.922130 11.00000 -1.20000
AFIX 0
C7 1 0.434730 0.630339 0.868015 11.00000 0.01520 0.01406 =
0.01523 -0.00180 0.00813 -0.00192
C8 1 0.547925 0.653486 0.925411 11.00000 0.01599 0.01771 =
0.01596 -0.00398 0.00848 -0.00224
C9 1 0.586044 0.720397 0.915254 11.00000 0.02015 0.01744 =
0.02263 -0.00309 0.00833 -0.00422
AFIX 43
H9 2 0.538907 0.754348 0.873030 11.00000 -1.20000
AFIX 0
C12 1 0.717913 0.619374 1.031444 11.00000 0.01791 0.02773 =
0.02036 -0.00480 0.00552 0.00031
AFIX 43
H12 2 0.764624 0.583974 1.070872 11.00000 -1.20000
AFIX 0
C11 1 0.761174 0.685433 1.027367 11.00000 0.01528 0.03441 =
0.02593 -0.01049 0.00557 -0.00734
AFIX 43
H11 2 0.835384 0.695342 1.064658 11.00000 -1.20000
AFIX 0
C10 1 0.694554 0.736327 0.968286 11.00000 0.02309 0.02474 =
0.02893 -0.00952 0.01197 -0.01142
AFIX 43
H10 2 0.722389 0.781804 0.963796 11.00000 -1.20000
AFIX 0
N13 3 0.613403 0.603317 0.982350 11.00000 0.01612 0.02120 =
0.01660 -0.00424 0.00591 -0.00101
C16 1 0.425214 0.445390 0.833394 11.00000 0.01605 0.01368 =
0.01597 0.00067 0.00935 -0.00010
N15 3 0.472908 0.509751 0.870765 11.00000 0.01365 0.01252 =
0.01886 -0.00008 0.00485 -0.00001
AFIX 43
H15 2 0.541760 0.513817 0.909153 11.00000 -1.20000
AFIX 0
N14 3 0.405111 0.565413 0.843416 11.00000 0.01382 0.01262 =
0.01608 -0.00039 0.00764 0.00022
N17 3 0.492839 0.390080 0.863595 11.00000 0.01277 0.01285 =
0.01830 0.00024 0.00551 0.00077
AFIX 43
H17 2 0.559816 0.399580 0.903096 11.00000 -1.20000
AFIX 0
C18 1 0.468251 0.318151 0.838885 11.00000 0.01881 0.01298 =
0.01542 0.00293 0.00926 0.00262
C19 1 0.555917 0.273636 0.851397 11.00000 0.01871 0.01808 =
0.02067 0.00441 0.01033 0.00433
AFIX 43
H19 2 0.627311 0.292327 0.872768 11.00000 -1.20000
AFIX 0
C20 1 0.537832 0.201736 0.832316 11.00000 0.02643 0.01716 =
0.02524 0.00563 0.01359 0.00877
AFIX 43
H20 2 0.597299 0.171241 0.841081 11.00000 -1.20000
AFIX 0
C21 1 0.433496 0.174070 0.800522 11.00000 0.03394 0.01324 =
0.02428 0.00176 0.01327 0.00263
AFIX 43
H21 2 0.421571 0.124953 0.787172 11.00000 -1.20000
AFIX 0
C22 1 0.346872 0.218691 0.788416 11.00000 0.02312 0.01705 =
0.02227 0.00223 0.00974 -0.00217
AFIX 43
H22 2 0.275510 0.199907 0.766703 11.00000 -1.20000
AFIX 0
C23 1 0.363658 0.290750 0.807819 11.00000 0.01730 0.01636 =
0.02001 0.00185 0.00868 0.00296
AFIX 43
H23 2 0.304161 0.320992 0.799914 11.00000 -1.20000
AFIX 0
N25 3 0.120142 0.527559 0.772458 11.00000 0.01342 0.01447 =
0.01430 -0.00006 0.00536 0.00046
O24 4 0.329082 0.442762 0.775849 11.00000 0.01479 0.01219 =
0.02065 0.00029 0.00453 0.00053
C26 1 0.103289 0.559413 0.844219 11.00000 0.01786 0.01964 =
0.01473 -0.00134 0.00534 0.00198
AFIX 43
H26 2 0.147932 0.598360 0.875628 11.00000 -1.20000
AFIX 0
C27 1 0.022880 0.537654 0.874556 11.00000 0.02314 0.03504 =
0.01813 -0.00284 0.01136 0.00234
AFIX 43
H27 2 0.012762 0.561326 0.925699 11.00000 -1.20000
AFIX 0
C28 1 -0.042023 0.480973 0.828949 11.00000 0.02229 0.04004 =
0.02492 -0.00191 0.01619 -0.00448
AFIX 43
H28 2 -0.096108 0.464162 0.849519 11.00000 -1.20000
AFIX 0
C29 1 -0.027076 0.448931 0.752626 11.00000 0.01897 0.02705 =
0.02204 -0.00303 0.01057 -0.00774
AFIX 43
H29 2 -0.071775 0.410515 0.719394 11.00000 -1.20000
AFIX 0
C30 1 0.053914 0.473775 0.725644 11.00000 0.01291 0.01498 =
0.01505 0.00099 0.00591 0.00012
C31 1 0.072825 0.443724 0.643013 11.00000 0.01192 0.01307 =
0.01389 -0.00017 0.00483 -0.00059
C32 1 0.020068 0.375991 0.598058 11.00000 0.01604 0.01408 =
0.01438 -0.00076 0.00642 -0.00364
C33 1 0.081637 0.315048 0.613800 11.00000 0.02429 0.01788 =
0.02324 -0.00141 0.00331 0.00095
AFIX 43
H33 2 0.158004 0.316613 0.648458 11.00000 -1.20000
AFIX 0
C34 1 0.029583 0.251544 0.577928 11.00000 0.04229 0.01470 =
0.02828 -0.00050 0.00855 0.00129
AFIX 43
H34 2 0.069469 0.208607 0.588647 11.00000 -1.20000
AFIX 0
C35 1 -0.081176 0.251876 0.526397 11.00000 0.04115 0.01851 =
0.02438 -0.00508 0.01107 -0.01456
AFIX 43
H35 2 -0.119271 0.209284 0.500951 11.00000 -1.20000
AFIX 0
C36 1 -0.135264 0.315852 0.512772 11.00000 0.02328 0.02859 =
0.02517 -0.00699 0.00718 -0.01208
AFIX 43
H36 2 -0.211290 0.315909 0.476137 11.00000 -1.20000
AFIX 0
N37 3 -0.087461 0.377667 0.547839 11.00000 0.01581 0.02148 =
0.02242 -0.00400 0.00513 -0.00421
N38 3 0.142297 0.478841 0.621800 11.00000 0.01383 0.01358 =
0.01436 -0.00026 0.00705 0.00027
N39 3 0.172904 0.461717 0.549798 11.00000 0.01785 0.01372 =
0.01566 -0.00441 0.00987 -0.00460
AFIX 43
H39 2 0.145795 0.425735 0.510831 11.00000 -1.20000
AFIX 0
C40 1 0.251607 0.506729 0.543513 11.00000 0.01292 0.01071 =
0.01700 0.00114 0.00639 0.00127
C42 1 0.345959 0.530545 0.434998 11.00000 0.01507 0.01203 =
0.01738 0.00399 0.00924 0.00361
N41 3 0.269867 0.496343 0.463392 11.00000 0.01564 0.01481 =
0.01569 -0.00273 0.00847 -0.00236
AFIX 43
H41 2 0.229155 0.464093 0.423582 11.00000 -1.20000
AFIX 0
C45 1 0.495699 0.589011 0.370036 11.00000 0.02142 0.01923 =
0.02543 0.00728 0.01446 0.00192
AFIX 43
H45 2 0.547010 0.608745 0.348153 11.00000 -1.20000
AFIX 0
C44 1 0.413573 0.545329 0.310663 11.00000 0.02571 0.02245 =
0.01844 0.00394 0.01324 0.00307
AFIX 43
H44 2 0.408717 0.535258 0.247706 11.00000 -1.20000
AFIX 0
C43 1 0.338536 0.516210 0.342092 11.00000 0.01822 0.01998 =
0.01703 0.00095 0.00816 0.00103
AFIX 43
H43 2 0.282287 0.486635 0.300715 11.00000 -1.20000
AFIX 0
C46 1 0.501968 0.603563 0.462125 11.00000 0.01875 0.01262 =
0.02456 0.00321 0.01062 0.00061
AFIX 43
H46 2 0.557686 0.633687 0.503050 11.00000 -1.20000
AFIX 0
N50 3 0.107205 0.345938 0.346552 11.00000 0.01874 0.02087 =
0.02045 -0.00307 0.00420 -0.00122
O49 4 0.077129 0.357339 0.413418 11.00000 0.05136 0.07118 =
0.03492 -0.03437 0.03055 -0.04169
O48 4 0.298550 0.549872 0.608422 11.00000 0.01604 0.01283 =
0.01622 -0.00233 0.00795 -0.00266
C47 1 0.427514 0.574463 0.494831 11.00000 0.01768 0.01277 =
0.01752 0.00082 0.00893 0.00213
AFIX 43
H47 2 0.432457 0.584595 0.557799 11.00000 -1.20000
AFIX 0
O51 4 0.075590 0.292788 0.295859 11.00000 0.03454 0.02753 =
0.03557 -0.01589 0.01060 -0.01090
O52 4 0.169061 0.388843 0.332095 11.00000 0.05862 0.03584 =
0.04895 -0.02196 0.03836 -0.02588
N54 3 0.751402 0.448948 0.934971 11.00000 0.01716 0.03314 =
0.01977 -0.00157 0.00639 0.00046
O55 4 0.687961 0.445598 0.979434 11.00000 0.01678 0.04713 =
0.02587 -0.00018 0.00948 -0.00282
O56 4 0.791757 0.394293 0.918402 11.00000 0.04170 0.02412 =
0.04205 0.00255 0.02062 0.00936
O53 4 0.772356 0.507446 0.910052 11.00000 0.06389 0.02618 =
0.05338 0.00280 0.04227 0.00312
HKLF 4
REM DT_ZnNO3L1_1_0m_a.res in P2(1)/c
REM R1 = 0.0338 for 7355 Fo > 4sig(Fo) and 0.0533 for all 9280 data
REM 514 parameters refined using 0 restraints
END
WGHT 0.0371 1.6349
REM Highest difference peak 0.690, deepest hole -0.485, 1-sigma level 0.058
Q1 1 0.7088 0.3867 0.9859 11.00000 0.05 0.69
Q2 1 0.2006 0.3674 0.3812 11.00000 0.05 0.57
Q3 1 0.0509 0.3930 0.3876 11.00000 0.05 0.56
Q4 1 0.7072 0.4837 0.9047 11.00000 0.05 0.45
Q5 1 0.0651 0.4592 0.6880 11.00000 0.05 0.38
Q6 1 0.0506 0.4103 0.6227 11.00000 0.05 0.35
Q7 1 0.3888 0.6594 0.8481 11.00000 0.05 0.34
Q8 1 0.8148 0.5996 0.8647 11.00000 0.05 0.34
Q9 1 0.4468 0.5969 0.4701 11.00000 0.05 0.34
Q10 1 0.5072 0.2959 0.8345 11.00000 0.05 0.32
Q11 1 0.4885 0.6445 0.8962 11.00000 0.05 0.32
Q12 1 0.1289 0.4479 0.6450 11.00000 0.05 0.32
Q13 1 0.0597 0.5454 0.8545 11.00000 0.05 0.32
Q14 1 0.3960 0.2002 0.7887 11.00000 0.05 0.30
Q15 1 0.5390 0.2413 0.8271 11.00000 0.05 0.30
Q16 1 0.5009 0.5893 0.4153 11.00000 0.05 0.30
Q17 1 0.5684 0.6842 0.9110 11.00000 0.05 0.29
Q18 1 0.3472 0.5193 0.3936 11.00000 0.05 0.29
Q19 1 0.6473 0.7194 0.9397 11.00000 0.05 0.29
Q20 1 0.4497 0.5738 0.3411 11.00000 0.05 0.29
REM The information below was added by Olex2.
REM
REM R1 = 0.0338 for 7355 Fo > 4sig(Fo) and 0.0533 for all 107067 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.69, deepest hole -0.49
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0533
REM R1_gt = 0.0338
REM wR_ref = 0.0794
REM GOOF = 1.018
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 107067
REM Reflections_gt = 7355
REM Parameters = n/a
REM Hole = -0.49
REM Peak = 0.69
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'