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_1562835
_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         'C9 H12 N2 S'
_chemical_formula_sum            'C9 H12 N2 S'
_chemical_formula_weight         180.27
_chemical_name_systematic        xstr1192
_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   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                 100.114(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.63230(10)
_cell_length_b                   13.4731(2)
_cell_length_c                   12.4161(3)
_cell_measurement_reflns_used    9412
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.3440
_cell_measurement_theta_min      4.8410
_cell_volume                     927.55(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.993
_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    -45.00  -6.00   1.00    1.00    --  -42.75 125.00  60.00   39
  2  \w    -81.00  -8.00   1.00    1.00    --  -42.75 125.00 150.00   73
  3  \w   -100.00 -15.00   1.00    1.00    --  -42.75 -57.00-150.00   85
  4  \w   -113.00 -16.00   1.00    1.00    --  -42.75 -57.00 -60.00   97
  5  \w    -49.00 -15.00   1.00    1.00    --  -42.75 -57.00  90.00   34
  6  \w   -101.00 -18.00   1.00    1.00    --  -42.75 -38.00   0.00   83
  7  \w   -109.00 -53.00   1.00    1.00    --  -42.75 -57.00-180.00   56
  8  \w    -78.00 -51.00   1.00    1.00    --  -42.75 -57.00  90.00   27
  9  \w    -57.00  31.00   1.00    1.00    --  -42.75  38.00 -30.00   88
 10  \w    -86.00 -10.00   1.00    1.00    --  -42.75 125.00 -30.00   76
 11  \w     11.00  42.00   1.00    1.00    --   42.75  79.00 -32.47   31
 12  \w     10.00  41.00   1.00    1.00    --   42.75  76.00-109.07   31
 13  \w     13.00  41.00   1.00    1.00    --   42.75  79.00 167.10   28
 14  \w      9.00  36.00   1.00    1.00    --   42.75  82.00  55.66   27
 15  \w      9.00  35.00   1.00    1.00    --   42.75  82.00 135.34   26
 16  \w    108.00 137.00   1.00    1.00    --  104.49 -77.00  90.00   29
 17  \w     29.00  88.00   1.00    1.00    --  104.49 -77.00  90.00   59
 18  \w     76.00 102.00   1.00    1.00    --  104.49  58.00-128.50   26
 19  \w     75.00 102.00   1.00    1.00    --  104.49  61.00 120.00   27
 20  \w     31.00 113.00   1.00    1.00    --  104.49-125.00  90.00   82
 21  \w     32.00  99.00   1.00    1.00    --  104.49-125.00  30.00   67
 22  \w     75.00 101.00   1.00    1.00    --  104.49  63.00 -68.00   26
 23  \w    113.00 175.00   1.00    1.00    --  104.49  61.00 -30.00   62
 24  \w     75.00 175.00   1.00    1.00    --  104.49  61.00 -90.00  100
 25  \w     75.00 108.00   1.00    1.00    --  104.49  61.00 -30.00   33
 26  \w     31.00 113.00   1.00    1.00    --  104.49-125.00 -60.00   82
 27  \w     31.00 110.00   1.00    1.00    --  104.49-125.00-150.00   79
 28  \w    115.00 162.00   1.00    1.00    --  104.49 125.00  60.00   47
 29  \w     75.00 156.00   1.00    1.00    --  104.49  61.00-120.00   81
 30  \w     75.00 105.00   1.00    1.00    --  104.49  61.00-180.00   30
 31  \w     77.00 106.00   1.00    1.00    --  104.49  61.00   6.04   29
 32  \w     80.00 162.00   1.00    1.00    --  104.49  37.00  49.96   82
 33  \w     76.00 106.00   1.00    1.00    --  104.49  63.00-170.62   30
 34  \w     75.00 102.00   1.00    1.00    --  104.49  61.00  30.00   27
 35  \w     75.00 173.00   1.00    1.00    --  104.49  61.00  90.00   98
 36  \w     74.00 101.00   1.00    1.00    --  104.49  66.00  45.91   27
 37  \w     75.00 101.00   1.00    1.00    --  104.49  61.00   0.00   26
 38  \w    135.00 177.00   1.00    1.00    --  104.49  61.00   0.00   42
 39  \w     79.00 106.00   1.00    1.00    --  104.49  45.00   0.00   27
 40  \w     83.00 109.00   1.00    1.00    --  104.49  45.00  90.00   26
 41  \w     86.00 117.00   1.00    1.00    --  104.49  45.00 150.00   31
 42  \w     76.00 173.00   1.00    1.00    --  104.49  61.00 150.00   97
 43  \w     80.00 107.00   1.00    1.00    --  104.49  45.00 -30.00   27
 44  \w     78.00 105.00   1.00    1.00    --  104.49  61.00  60.00   27
 45  \w     76.00 137.00   1.00    1.00    --  104.49  61.00-150.00   61
 46  \w    145.00 172.00   1.00    1.00    --  104.49  58.00-128.50   27
;
_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      -0.0766084000
_diffrn_orient_matrix_UB_12      0.1071817000
_diffrn_orient_matrix_UB_13      0.0203136000
_diffrn_orient_matrix_UB_21      -0.2601412000
_diffrn_orient_matrix_UB_22      -0.0242275000
_diffrn_orient_matrix_UB_23      -0.0554986000
_diffrn_orient_matrix_UB_31      -0.0604341000
_diffrn_orient_matrix_UB_32      -0.0316292000
_diffrn_orient_matrix_UB_33      0.1113205000
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12975
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.694
_diffrn_reflns_theta_min         4.885
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.645
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65998
_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    1.291
_exptl_crystal_description       plate
_exptl_crystal_F_000             384
_exptl_crystal_preparation       'PhSCN + HNMe2'
_exptl_crystal_recrystallization_method
'Crystallised from a toluene/THF solution'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0512P)^2^+0.4834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1736
_reflns_number_total             1823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01846a2.cif
_cod_data_source_block           xstr1192
_cod_database_code               1562835
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C9 H12 N2 S '
_chemical_oxdiff_usercomment     'CEK MAB'
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.620
_reflns_odcompleteness_completeness 99.77
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C5(H5), C9(H9), C6(H6), C7(H7), C8(H8)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              5478
_shelx_hkl_checksum              77716
_olex2_date_sample_data_collection 2020-03-10
_olex2_exptl_crystal_mounting_method 'Nylon loop'
_olex2_submission_original_sample_id xstr1192
_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 3.022
_oxdiff_exptl_absorpt_empirical_full_min 0.735