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_1562836
_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         'C13 H29 N3 O S Zn, C3.5'
_chemical_formula_sum            'C16.5 H29 N3 O S Zn'
_chemical_formula_weight         382.86
_chemical_name_systematic        xstr1294
_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             2021-02-15
_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                 104.1930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.72190(10)
_cell_length_b                   10.99980(10)
_cell_length_c                   17.8205(2)
_cell_measurement_reflns_used    25113
_cell_measurement_temperature    151(1)
_cell_measurement_theta_max      73.1800
_cell_measurement_theta_min      5.4440
_cell_volume                     2037.57(4)
_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      151(1)
_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 0.994
_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   -113.00 -17.00   1.00    1.40    --  -43.29 -57.00 -90.00   96
  2  \w    -87.00  -6.00   1.00    1.40    --  -43.29 125.00 120.00   81
  3  \w    -70.00  26.00   1.00    1.40    --  -43.29  57.00  60.00   96
  4  \w    -96.00 -18.00   1.00    1.40    --  -43.29 -57.00  60.00   78
  5  \w    -64.00 -21.00   1.00    1.40    --  -43.29 -38.00-180.00   43
  6  \w   -112.00 -21.00   1.00    1.40    --  -43.29 -57.00 150.00   91
  7  \w   -108.00 -22.00   1.00    1.40    --  -43.29 -38.00 -30.00   86
  8  \w    -63.00  27.00   1.00    1.40    --  -43.29  57.00 -60.00   90
  9  \w     12.00  39.00   1.00    1.40    --   43.29  76.00 -39.85   27
 10  \w     11.00  36.00   1.00    1.40    --   43.29  79.00  18.05   25
 11  \w     12.00  42.00   1.00    1.40    --   43.29  77.00  55.17   30
 12  \w     13.00  40.00   1.00    1.40    --   43.29  77.00 175.32   27
 13  \w     13.00  40.00   1.00    1.40    --   43.29  79.00-103.69   27
 14  \w     13.00  38.00   1.00    1.40    --   43.29  78.00 124.52   25
 15  \w     75.00 132.00   1.00    5.61    --  105.52  72.00  67.19   57
 16  \w     76.00 175.00   1.00    5.61    --  105.52  71.00 -79.11   99
 17  \w     75.00 173.00   1.00    5.61    --  105.52  72.00  93.74   98
 18  \w     76.00 102.00   1.00    5.61    --  105.52  71.00  -4.02   26
 19  \w     79.00 110.00   1.00    5.61    --  105.52  56.00 -43.61   31
 20  \w     79.00 104.00   1.00    5.61    --  105.52  62.00-162.73   25
 21  \w     78.00 105.00   1.00    5.61    --  105.52  61.00  60.00   27
 22  \w     74.00 104.00   1.00    5.61    --  105.52 -94.00  30.00   30
 23  \w     78.00 106.00   1.00    5.61    --  105.52  60.00 160.20   28
 24  \w     82.00 145.00   1.00    5.61    --  105.52  45.00 -90.00   63
 25  \w     79.00 104.00   1.00    5.61    --  105.52  61.00-150.00   25
 26  \w     24.00 106.00   1.00    5.61    --  105.52 -94.00 120.00   82
 27  \w     25.00 106.00   1.00    5.61    --  105.52 -94.00 -60.00   81
 28  \w    108.00 157.00   1.00    5.61    --  105.52  62.00-137.25   49
 29  \w     77.00 103.00   1.00    5.61    --  105.52  67.00 -98.17   26
 30  \w     78.00 155.00   1.00    5.61    --  105.52  61.00-120.00   77
 31  \w     75.00 106.00   1.00    5.61    --  105.52 -94.00-150.00   31
 32  \w     48.00 133.00   1.00    5.61    --  105.52 -61.00 120.00   85
 33  \w     78.00 111.00   1.00    5.61    --  105.52  61.00  23.91   33
 34  \w     78.00 105.00   1.00    5.61    --  105.52  62.00-137.25   27
 35  \w    124.00 174.00   1.00    5.61    --  105.52  61.00 120.00   50
 36  \w     78.00 118.00   1.00    5.61    --  105.52  61.00 -30.00   40
 37  \w    121.00 170.00   1.00    5.61    --  105.52  61.00 -30.00   49
 38  \w     78.00 104.00   1.00    5.61    --  105.52  61.00   0.00   26
 39  \w     78.00 105.00   1.00    5.61    --  105.52  61.00 120.00   27
 40  \w     75.00 178.00   1.00    5.61    --  105.52  74.00  26.00  103
 41  \w     35.00 121.00   1.00    5.61    --  105.52 -61.00 -30.00   86
 42  \w     81.00 138.00   1.00    5.61    --  105.52  61.00  90.00   57
 43  \w     79.00 169.00   1.00    5.61    --  105.52  57.00  -2.71   90
 44  \w     79.00 104.00   1.00    5.61    --  105.52  61.00-180.00   25
 45  \w     77.00 103.00   1.00    5.61    --  105.52  67.00-177.25   26
 46  \w     78.00 104.00   1.00    5.61    --  105.52  61.00 150.00   26
 47  \w     78.00 176.00   1.00    5.61    --  105.52  63.00 171.25   98
 48  \w     79.00 116.00   1.00    5.61    --  105.52  54.00 143.33   37
;
_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      0.1386964000
_diffrn_orient_matrix_UB_12      -0.0215062000
_diffrn_orient_matrix_UB_13      0.0478722000
_diffrn_orient_matrix_UB_21      -0.0203246000
_diffrn_orient_matrix_UB_22      0.0938551000
_diffrn_orient_matrix_UB_23      0.0600682000
_diffrn_orient_matrix_UB_31      -0.0479601000
_diffrn_orient_matrix_UB_32      -0.1017633000
_diffrn_orient_matrix_UB_33      0.0453210000
_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  0.0307
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32620
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.453
_diffrn_reflns_theta_min         5.960
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84888
_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    1.248
_exptl_crystal_description       plate
_exptl_crystal_F_000             812
_exptl_crystal_preparation       '[L1ZnEt] + HL4'
_exptl_crystal_recrystallization_method 'Crystallised from a toluene solution'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         4076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0696P)^2^+3.0488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3930
_reflns_number_total             4076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01846a2.cif
_cod_data_source_block           xstr1294
_cod_original_formula_sum        'C16.50 H29 N3 O S Zn'
_cod_database_code               1562836
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn O S N3 C13 H29'
_chemical_oxdiff_usercomment     'CEK MAB'
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.776
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C18(0.5) C17(0.5) C15(0.5)
3.a Ternary CH refined with riding coordinates:
 C9(H9)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C6(H6A,H6B), C4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1)
3.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              95937
_shelx_hkl_checksum              82177
_olex2_date_sample_data_collection 2021-01-18
_olex2_exptl_crystal_mounting_method 'Nylon loop'
_olex2_submission_original_sample_id xstr1294
_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 1.672
_oxdiff_exptl_absorpt_empirical_full_min 0.766