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#$Date: 2024-08-05 21:57:44 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293843 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/63/7716376.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7716376
loop_
_publ_author_name
'Robson, Max E.'
'Johnson, Andrew L.'
_publ_section_title
;
 Zinc and cadmium thioamidate complexes: rational design of single-source
 precursors for the AACVD of ZnS.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11380
_journal_page_last               11392
_journal_paper_doi               10.1039/d4dt01278j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C40 H48 N4 S4 Zn2'
_chemical_formula_sum            'C40 H48 N4 S4 Zn2'
_chemical_formula_weight         843.80
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-04-25 deposited with the CCDC.	2024-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.491(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9334(4)
_cell_length_b                   17.3065(5)
_cell_length_c                   12.9808(5)
_cell_measurement_reflns_used    6977
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.3740
_cell_measurement_theta_min      3.2610
_cell_volume                     2076.41(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
 SHELXL-2018/3 (Sheldrick, 2018)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_structure_solution
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17282
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.776
_diffrn_reflns_theta_min         3.225
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.389
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       plate
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         5273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0216P)²+0.9615P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4355
_reflns_number_total             5273
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01278j2.cif
_cod_data_source_block           e21alj18
_cod_depositor_comments
'Adding full bibliography for 7716374--7716379.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7716376
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.443
_shelx_estimated_absorpt_t_max   0.874
_oxdiff_exptl_absorpt_empirical_full_min 0.753
_oxdiff_exptl_absorpt_empirical_full_max 1.292
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
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'
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 0.07124(2) 0.59282(2) 0.47656(2) 0.02035(6) Uani 1 1 d . . . . .
S1 S -0.04973(5) 0.71120(3) 0.45624(4) 0.02578(10) Uani 1 1 d . . . . .
S2 S -0.15998(5) 0.48574(3) 0.36521(4) 0.02365(10) Uani 1 1 d . . . . .
N1 N 0.22292(15) 0.68695(8) 0.50628(11) 0.0190(3) Uani 1 1 d . . . . .
N2 N 0.08472(15) 0.52705(8) 0.35152(11) 0.0190(3) Uani 1 1 d . . . . .
C1 C 0.12999(18) 0.74173(10) 0.49863(13) 0.0203(3) Uani 1 1 d . . . . .
C2 C 0.1681(2) 0.82589(10) 0.52666(15) 0.0266(4) Uani 1 1 d . . . . .
H2 H 0.269126 0.834491 0.530002 0.032 Uiso 1 1 calc R U . . .
C3 C 0.1639(3) 0.84344(12) 0.64123(18) 0.0424(5) Uani 1 1 d . . . . .
H3A H 0.066099 0.834196 0.640205 0.064 Uiso 1 1 calc R U . . .
H3B H 0.190455 0.897570 0.660248 0.064 Uiso 1 1 calc R U . . .
H3C H 0.232545 0.809764 0.696472 0.064 Uiso 1 1 calc R U . . .
C4 C 0.0676(3) 0.88081(12) 0.4396(2) 0.0477(6) Uani 1 1 d . . . . .
H4A H 0.072965 0.869464 0.367213 0.072 Uiso 1 1 calc R U . . .
H4B H 0.097685 0.934326 0.460232 0.072 Uiso 1 1 calc R U . . .
H4C H -0.032056 0.873730 0.435622 0.072 Uiso 1 1 calc R U . . .
C5 C -0.02129(18) 0.47883(10) 0.31167(13) 0.0200(3) Uani 1 1 d . . . . .
C6 C -0.0346(2) 0.42290(11) 0.21905(15) 0.0287(4) Uani 1 1 d . . . . .
H6 H 0.064038 0.415084 0.216885 0.034 Uiso 1 1 calc R U . . .
C7 C -0.1307(3) 0.45863(15) 0.10830(17) 0.0521(7) Uani 1 1 d . . . . .
H7A H -0.228541 0.466397 0.108124 0.078 Uiso 1 1 calc R U . . .
H7B H -0.134791 0.423849 0.047660 0.078 Uiso 1 1 calc R U . . .
H7C H -0.090231 0.508476 0.098391 0.078 Uiso 1 1 calc R U . . .
C8 C -0.0932(2) 0.34383(12) 0.23484(17) 0.0362(5) Uani 1 1 d . . . . .
H8A H -0.034050 0.323099 0.307636 0.054 Uiso 1 1 calc R U . . .
H8B H -0.089659 0.308469 0.176934 0.054 Uiso 1 1 calc R U . . .
H8C H -0.193559 0.349289 0.230050 0.054 Uiso 1 1 calc R U . . .
C11 C 0.37557(18) 0.70080(9) 0.54338(14) 0.0201(3) Uani 1 1 d . . . . .
C12 C 0.4565(2) 0.71748(11) 0.65340(16) 0.0287(4) Uani 1 1 d . . . . .
H12 H 0.410336 0.722163 0.705538 0.034 Uiso 1 1 calc R U . . .
C13 C 0.6051(2) 0.72729(12) 0.68692(18) 0.0385(5) Uani 1 1 d . . . . .
H13 H 0.660197 0.738920 0.762172 0.046 Uiso 1 1 calc R U . . .
C14 C 0.6738(2) 0.72033(12) 0.6122(2) 0.0388(5) Uani 1 1 d . . . . .
H14 H 0.775319 0.728011 0.635575 0.047 Uiso 1 1 calc R U . . .
C15 C 0.5941(2) 0.70217(11) 0.50346(19) 0.0340(5) Uani 1 1 d . . . . .
H15 H 0.641229 0.696795 0.452029 0.041 Uiso 1 1 calc R U . . .
C16 C 0.44502(19) 0.69162(11) 0.46839(16) 0.0266(4) Uani 1 1 d . . . . .
H16 H 0.390898 0.678218 0.393616 0.032 Uiso 1 1 calc R U . . .
C21 C 0.20471(18) 0.52854(10) 0.31454(14) 0.0194(3) Uani 1 1 d . . . . .
C22 C 0.2010(2) 0.57558(11) 0.22720(14) 0.0261(4) Uani 1 1 d . . . . .
H22 H 0.116793 0.604826 0.188074 0.031 Uiso 1 1 calc R U . . .
C23 C 0.3217(2) 0.57959(12) 0.19736(15) 0.0304(4) Uani 1 1 d . . . . .
H23 H 0.320016 0.611855 0.137698 0.036 Uiso 1 1 calc R U . . .
C24 C 0.4440(2) 0.53691(11) 0.25399(16) 0.0297(4) Uani 1 1 d . . . . .
H24 H 0.525852 0.539537 0.232836 0.036 Uiso 1 1 calc R U . . .
C25 C 0.4473(2) 0.49030(11) 0.34159(17) 0.0303(4) Uani 1 1 d . . . . .
H25 H 0.531480 0.460950 0.380462 0.036 Uiso 1 1 calc R U . . .
C26 C 0.32802(19) 0.48641(10) 0.37264(15) 0.0250(4) Uani 1 1 d . . . . .
H26 H 0.330703 0.455033 0.433413 0.030 Uiso 1 1 calc R U . . .
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'
S S 0.1246 0.1234 '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'
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
N2 Zn1 N1 108.71(5) . . ?
N2 Zn1 S1 125.67(4) . . ?
N1 Zn1 S1 69.82(4) . . ?
N2 Zn1 S2 105.16(4) . 3_566 ?
N1 Zn1 S2 105.49(4) . 3_566 ?
S1 Zn1 S2 128.161(18) . 3_566 ?
C1 S1 Zn1 78.81(6) . . ?
C5 S2 Zn1 102.04(6) . 3_566 ?
C1 N1 C11 122.51(14) . . ?
C1 N1 Zn1 96.15(10) . . ?
C11 N1 Zn1 140.42(11) . . ?
C5 N2 C21 122.04(14) . . ?
C5 N2 Zn1 113.55(11) . . ?
C21 N2 Zn1 124.26(11) . . ?
N1 C1 C2 125.05(15) . . ?
N1 C1 S1 114.73(13) . . ?
C2 C1 S1 120.19(13) . . ?
C1 C2 C4 112.40(16) . . ?
C1 C2 C3 109.28(15) . . ?
C4 C2 C3 110.54(17) . . ?
C1 C2 H2 108.2 . . ?
C4 C2 H2 108.2 . . ?
C3 C2 H2 108.2 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 123.55(15) . . ?
N2 C5 S2 116.01(13) . . ?
C6 C5 S2 120.31(13) . . ?
C5 C6 C8 113.15(15) . . ?
C5 C6 C7 109.29(17) . . ?
C8 C6 C7 110.44(17) . . ?
C5 C6 H6 107.9 . . ?
C8 C6 H6 107.9 . . ?
C7 C6 H6 107.9 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C12 C11 C16 119.61(16) . . ?
C12 C11 N1 121.54(15) . . ?
C16 C11 N1 118.68(16) . . ?
C13 C12 C11 119.77(18) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 C12 120.8(2) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C15 C14 C13 119.55(18) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 120.52(19) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C15 C16 C11 119.74(18) . . ?
C15 C16 H16 120.1 . . ?
C11 C16 H16 120.1 . . ?
C22 C21 C26 120.49(15) . . ?
C22 C21 N2 120.44(15) . . ?
C26 C21 N2 118.92(15) . . ?
C21 C22 C23 119.36(17) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C24 C23 C22 120.35(17) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 120.03(16) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C26 120.09(18) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C21 119.68(17) . . ?
C25 C26 H26 120.2 . . ?
C21 C26 H26 120.2 . . ?
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 N2 2.0266(13) . ?
Zn1 N1 2.1557(14) . ?
Zn1 S1 2.3407(5) . ?
Zn1 S2 2.3489(5) 3_566 ?
S1 C1 1.7462(18) . ?
S2 C5 1.7598(17) . ?
N1 C1 1.301(2) . ?
N1 C11 1.433(2) . ?
N2 C5 1.294(2) . ?
N2 C21 1.439(2) . ?
C1 C2 1.515(2) . ?
C2 C4 1.533(3) . ?
C2 C3 1.533(3) . ?
C2 H2 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.511(2) . ?
C6 C8 1.530(3) . ?
C6 C7 1.535(3) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C11 C12 1.388(2) . ?
C11 C16 1.393(2) . ?
C12 C13 1.388(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.378(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.393(2) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.385(2) . ?
C21 C26 1.387(2) . ?
C22 C23 1.390(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.385(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.386(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 N1 C1 C2 0.2(3) . . . . ?
Zn1 N1 C1 C2 171.24(15) . . . . ?
C11 N1 C1 S1 -177.86(12) . . . . ?
Zn1 N1 C1 S1 -6.80(12) . . . . ?
Zn1 S1 C1 N1 6.34(12) . . . . ?
Zn1 S1 C1 C2 -171.80(14) . . . . ?
N1 C1 C2 C4 135.61(19) . . . . ?
S1 C1 C2 C4 -46.5(2) . . . . ?
N1 C1 C2 C3 -101.3(2) . . . . ?
S1 C1 C2 C3 76.67(18) . . . . ?
C21 N2 C5 C6 -3.5(3) . . . . ?
Zn1 N2 C5 C6 -179.21(13) . . . . ?
C21 N2 C5 S2 -179.31(12) . . . . ?
Zn1 N2 C5 S2 5.02(16) . . . . ?
Zn1 S2 C5 N2 -86.25(13) 3_566 . . . ?
Zn1 S2 C5 C6 97.83(14) 3_566 . . . ?
N2 C5 C6 C8 141.54(18) . . . . ?
S2 C5 C6 C8 -42.9(2) . . . . ?
N2 C5 C6 C7 -94.9(2) . . . . ?
S2 C5 C6 C7 80.65(18) . . . . ?
C1 N1 C11 C12 71.6(2) . . . . ?
Zn1 N1 C11 C12 -94.4(2) . . . . ?
C1 N1 C11 C16 -113.15(19) . . . . ?
Zn1 N1 C11 C16 80.9(2) . . . . ?
C16 C11 C12 C13 2.1(3) . . . . ?
N1 C11 C12 C13 177.26(17) . . . . ?
C11 C12 C13 C14 -0.3(3) . . . . ?
C12 C13 C14 C15 -1.1(3) . . . . ?
C13 C14 C15 C16 0.7(3) . . . . ?
C14 C15 C16 C11 1.1(3) . . . . ?
C12 C11 C16 C15 -2.5(3) . . . . ?
N1 C11 C16 C15 -177.80(16) . . . . ?
C5 N2 C21 C22 90.7(2) . . . . ?
Zn1 N2 C21 C22 -94.06(18) . . . . ?
C5 N2 C21 C26 -93.8(2) . . . . ?
Zn1 N2 C21 C26 81.40(18) . . . . ?
C26 C21 C22 C23 0.7(3) . . . . ?
N2 C21 C22 C23 176.10(16) . . . . ?
C21 C22 C23 C24 0.2(3) . . . . ?
C22 C23 C24 C25 -0.5(3) . . . . ?
C23 C24 C25 C26 0.0(3) . . . . ?
C24 C25 C26 C21 0.9(3) . . . . ?
C22 C21 C26 C25 -1.3(3) . . . . ?
N2 C21 C26 C25 -176.73(16) . . . . ?
