Synthesis, solution dynamics and chemical vapour deposition of heteroleptic zinc complexes via ethyl and amide zinc thioureides
Bhide, Malavika; Mears, Kristian Luke; Carmalt, Claire J.; Knapp, Caroline E.; Chemical Science  (2021) –; doi:10.1039/D1SC01846A

data_1562837
_publ_section_title
;
 Synthesis, solution dynamics and chemical vapour deposition of
 heteroleptic zinc complexes via ethyl and amide zinc thioureides
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC01846A
_journal_year                    2021
_chemical_formula_moiety         'C11 H16 N2 S Zn'
_chemical_formula_sum            'C11 H16 N2 S Zn'
_chemical_formula_weight         273.69
_chemical_name_systematic        xstr1205
_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_date             2021-02-16
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2021-03-19 deposited with the CCDC.	2021-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.349(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5467(2)
_cell_length_b                   9.6250(2)
_cell_length_c                   15.3938(4)
_cell_measurement_reflns_used    11012
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.5030
_cell_measurement_theta_min      4.5530
_cell_volume                     1221.16(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -112.00 -24.00   1.00    1.00    --  -42.62 -38.00 120.00   88
  2  \w   -113.00 -15.00   1.00    1.00    --  -42.62 -57.00   0.00   98
  3  \w    -71.00  37.00   1.00    1.00    --  -42.62  19.00-180.00  108
  4  \w    -68.00 -14.00   1.00    1.00    --  -42.62 -57.00 -90.00   54
  5  \w   -107.00 -27.00   1.00    1.00    --  -42.62 -57.00-150.00   80
  6  \w    -94.00 -19.00   1.00    1.00    --  -42.62 -57.00  90.00   75
  7  \w    -66.00  31.00   1.00    1.00    --  -42.62  57.00 -90.00   97
  8  \w     13.00  41.00   1.00    1.00    --   42.62  72.00 135.07   28
  9  \w     10.00  35.00   1.00    1.00    --   42.62  75.00  46.97   25
 10  \w      9.00  34.00   1.00    1.00    --   42.62  82.00-111.07   25
 11  \w      7.00  84.00   1.00    1.00    --   42.62 -99.00   0.00   77
 12  \w     47.00  75.00   1.00    1.00    --   42.62-125.00-180.00   28
 13  \w      9.00  35.00   1.00    1.00    --   42.62  82.00-166.88   26
 14  \w     92.00 117.00   1.00    1.00    --   42.62  72.00 135.07   25
 15  \w      9.00  34.00   1.00    1.00    --   42.62  82.00 -59.05   25
 16  \w     74.00 101.00   1.00    1.00    --  104.49  67.00-124.68   27
 17  \w     73.00  99.00   1.00    1.00    --  104.49  71.00 168.63   26
 18  \w     74.00 176.00   1.00    1.00    --  104.49  67.00-161.34  102
 19  \w    136.00 177.00   1.00    1.00    --  104.49  69.00-149.71   41
 20  \w     75.00 102.00   1.00    1.00    --  104.49  61.00 -60.00   27
 21  \w     75.00 100.00   1.00    1.00    --  104.49  69.00-149.71   25
 22  \w     73.00 106.00   1.00    1.00    --  104.49 -94.00 -90.00   33
 23  \w     80.00 105.00   1.00    1.00    --  104.49  45.00 150.00   25
 24  \w    110.00 171.00   1.00    1.00    --  104.49  70.00  98.19   61
 25  \w     22.00 104.00   1.00    1.00    --  104.49 -94.00-180.00   82
 26  \w     30.00 106.00   1.00    1.00    --  104.49 -94.00 120.00   76
 27  \w     31.00 101.00   1.00    1.00    --  104.49-125.00  30.00   70
 28  \w     76.00 104.00   1.00    1.00    --  104.49  61.00   0.00   28
 29  \w     75.00 140.00   1.00    1.00    --  104.49  61.00 -30.00   65
 30  \w     84.00 175.00   1.00    1.00    --  104.49  45.00  30.00   91
 31  \w     74.00 102.00   1.00    1.00    --  104.49  70.00  98.19   28
 32  \w     47.00 108.00   1.00    1.00    --  104.49-103.00  50.21   61
 33  \w     78.00 112.00   1.00    1.00    --  104.49  59.00-104.00   34
 34  \w     75.00 156.00   1.00    1.00    --  104.49  70.00  67.51   81
 35  \w     75.00 164.00   1.00    1.00    --  104.49  65.00 -20.07   89
 36  \w     35.00 134.00   1.00    1.00    --  104.49 -61.00-180.00   99
 37  \w     80.00 128.00   1.00    1.00    --  104.49  45.00 -30.00   48
 38  \w     75.00 102.00   1.00    1.00    --  104.49  61.00  60.00   27
 39  \w     75.00 102.00   1.00    1.00    --  104.49  61.00 120.00   27
 40  \w    144.00 169.00   1.00    1.00    --  104.49  68.00  35.57   25
 41  \w     79.00 106.00   1.00    1.00    --  104.49  45.00 120.00   27
 42  \w     75.00 177.00   1.00    1.00    --  104.49  61.00 -90.00  102
 43  \w     76.00 102.00   1.00    1.00    --  104.49  61.00  30.00   26
 44  \w     75.00 114.00   1.00    1.00    --  104.49  61.00 150.00   39
 45  \w     74.00 101.00   1.00    1.00    --  104.49  68.00  35.57   27
 46  \w     74.00 176.00   1.00    1.00    --  104.49  70.00 154.57  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0139160000
_diffrn_orient_matrix_UB_12      0.1069507000
_diffrn_orient_matrix_UB_13      0.0720741000
_diffrn_orient_matrix_UB_21      -0.1585051000
_diffrn_orient_matrix_UB_22      -0.0693125000
_diffrn_orient_matrix_UB_23      0.0072589000
_diffrn_orient_matrix_UB_31      0.0978761000
_diffrn_orient_matrix_UB_32      -0.0968802000
_diffrn_orient_matrix_UB_33      0.0743541000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17213
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.578
_diffrn_reflns_theta_min         5.406
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.129
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_preparation       'ZnEt2 + HL1*'
_exptl_crystal_recrystallization_method
'Crystallised from a deuterated benzene solution'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0400P)^2^+0.6492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2326
_reflns_number_total             2403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01846a2.cif
_cod_data_source_block           xstr1205
_cod_database_code               1562837
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C44 H64 N8 S4 Zn4 '
_shelx_estimated_absorpt_t_max   0.683
_shelx_estimated_absorpt_t_min   0.492
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C7(H7), C10(H10), C8(H8), C9(H9)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              11674
_shelx_hkl_checksum              94555
_olex2_date_sample_data_collection 2020-06-23
_olex2_exptl_crystal_mounting_method 'Nylon loop'
_olex2_submission_original_sample_id xstr1205
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.084
_oxdiff_exptl_absorpt_empirical_full_min 0.704