N,N′-Substituted thioureas and their metal complexes: syntheses, structures and electronic properties
Al-Riyahee, Ali A. A.; Horton, Peter N.; Coles, Simon J.; Berry, Colin; Horrocks, Paul D.; Pope, Simon J. A.; Amoroso, Angelo J.; Dalton Transactions  (2022) –; doi:10.1039/D1DT04091J

data_7709468
_publ_section_title
;
 &#x000D; N,N&#x2032;-Substituted thioureas and their metal complexes:
 syntheses, structures and electronic properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04091J
_journal_year                    2022
_chemical_formula_moiety         'C26 H24 Cu N8 O2 S2, Cl O4'
_chemical_formula_sum            'C26 H24 Cl Cu N8 O6 S2'
_chemical_formula_weight         707.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2021-05-07 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.4260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4870(7)
_cell_length_b                   17.9141(13)
_cell_length_c                   15.3930(11)
_cell_measurement_reflns_used    33946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_cell_volume                     2773.8(3)
_computing_cell_refinement
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
scan:
	Number of images: 137
	           Slice: -107.0000 - 30.0000
	     Image width: 1.0000
	        Exp time: 80.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -18.0000
	             Phi: -30.0000
	             XTD: 44.8344
	          2theta: -17.1095
scan:
	Number of images: 99
	           Slice: -77.0000 - 22.0000
	     Image width: 1.0000
	        Exp time: 80.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -72.0000
	             Phi: -90.0000
	             XTD: 44.8344
	          2theta: -17.1095
scan:
	Number of images: 66
	           Slice: -31.0000 - 35.0000
	     Image width: 1.0000
	        Exp time: 80.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 54.0000
	             Phi: 150.0000
	             XTD: 44.8344
	          2theta: -17.1095
scan:
	Number of images: 75
	           Slice: -53.0000 - 22.0000
	     Image width: 1.0000
	        Exp time: 80.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -72.0000
	             Phi: 60.0000
	             XTD: 44.8344
	          2theta: -17.1095
scan:
	Number of images: 56
	           Slice: -31.0000 - 25.0000
	     Image width: 1.0000
	        Exp time: 80.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 72.0000
	             Phi: -180.0000
	             XTD: 44.8344
	          2theta: -17.1095
scan:
	Number of images: 126
	           Slice: -56.0000 - 70.0000
	     Image width: 1.0000
	        Exp time: 80.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 72.0000
	             Phi: 150.0000
	             XTD: 44.8344
	          2theta: -17.1095
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       d*Trek
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_diffrn_orient_matrix_UB_12      0.049066
_diffrn_orient_matrix_UB_13      0.083094
_diffrn_orient_matrix_UB_21      -0.033113
_diffrn_orient_matrix_UB_22      -0.042217
_diffrn_orient_matrix_UB_23      0.015406
_diffrn_orient_matrix_UB_31      0.045312
_diffrn_orient_matrix_UB_32      -0.018448
_diffrn_orient_matrix_UB_33      0.046837
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36950
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.925
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_exptl_crystal_colour            'Dark Orange'
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       Blade
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.334
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_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^)+(0.0583P)^2^+1.5115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5291
_reflns_number_total             6352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04091j2.cif
_cod_data_source_block           6_2014ncs0429
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7709468
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.871
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N4-H4A = N24-H24A
 0.88 with sigma of 0.02
 C22-C23 \\sim C22-C223
 with sigma of 0.02
3. Others
 Sof(C223)=Sof(C224)=Sof(H224)=Sof(C225)=Sof(H225)=Sof(C226)=Sof(H226)=
 Sof(C227)=Sof(H227)=Sof(C228)=Sof(H228)=1-FVAR(1)
 Sof(C23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=
 Sof(H27)=Sof(C28)=Sof(H28)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
  C224(H224), C225(H225), C226(H226), C227(H227), C228(H228)
4.b Fitted hexagon refined as free rotating group:
 C23(C24,C25,C26,C27,C28), C223(C224,C225,C226,C227,C228)
;
_shelx_res_checksum              7892
_shelx_hkl_checksum              28126
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'