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_7709462
_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         'C28 H26 Cu N6 O2 S2, Cl O4, C2 H3 N'
_chemical_formula_sum            'C30 H29 Cl Cu N7 O6 S2'
_chemical_formula_weight         746.71
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-05-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-07 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.196(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4602(11)
_cell_length_b                   9.7669(7)
_cell_length_c                   21.9107(15)
_cell_measurement_reflns_used    17705
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     3124.5(4)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (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 0.996
_diffrn_measurement_details
;
scan:
	Number of images: 151
	           Slice: -78.0000 - 73.0000
	     Image width: 1.0000
	        Exp time: 6.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 18.0000
	             Phi: -30.0000
	             XTD: 45.0378
	          2theta: -17.3203
scan:
	Number of images: 91
	           Slice: -80.0000 - 11.0000
	     Image width: 1.0000
	        Exp time: 6.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -72.0000
	             Phi: -180.0000
	             XTD: 45.0378
	          2theta: -17.3203
scan:
	Number of images: 53
	           Slice: -107.0000 - -54.0000
	     Image width: 1.0000
	        Exp time: 6.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -18.0000
	             Phi: 150.0000
	             XTD: 45.0378
	          2theta: -17.3203
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF 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
_diffrn_orient_matrix_UB_11      0.005028
_diffrn_orient_matrix_UB_12      -0.007466
_diffrn_orient_matrix_UB_13      0.067896
_diffrn_orient_matrix_UB_21      0.097372
_diffrn_orient_matrix_UB_22      0.031427
_diffrn_orient_matrix_UB_23      -0.003755
_diffrn_orient_matrix_UB_31      -0.012539
_diffrn_orient_matrix_UB_32      0.041419
_diffrn_orient_matrix_UB_33      0.021512
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20514
_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         27.485
_diffrn_reflns_theta_min         2.509
_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    0.975
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0536P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5054
_reflns_number_total             7140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04091j2.cif
_cod_data_source_block           1_2014ncs0359
_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               7709462
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.779
_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:
 C3(H3), C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C23(H23), C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C27(H27A,H27B,H27C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              67026
_shelx_hkl_checksum              60929
_olex2_submission_special_instructions 'No special instructions were received'