Homoleptic and heteroleptic Zn(ii) selone catalysts for thioetherification of aryl halides without scrubbing oxygen
Vaddamanu, Moulali; Velappan, Kavitha; Prabusankar, Ganesan; New Journal of Chemistry 44 (2020) 3574–3583; doi:10.1039/C9NJ05818D

data_7059364
_publ_section_title
;
 Homoleptic and heteroleptic Zn(ii) selone catalysts for
 thioetherification of aryl halides without scrubbing oxygen
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3574
_journal_page_last               3583
_journal_paper_doi               10.1039/C9NJ05818D
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C28 H48 N8 Se4 Zn, 2(Cl O4)'
_chemical_formula_sum            'C28 H48 Cl2 N8 O8 Se4 Zn'
_chemical_formula_weight         1076.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     direct
_audit_creation_date             2019-11-14
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Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
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_audit_update_record
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2019-11-22 deposited with the CCDC.	2020-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                67.891(7)
_cell_angle_beta                 68.825(7)
_cell_angle_gamma                89.725(6)
_cell_formula_units_Z            2
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_cell_length_b                   12.6356(9)
_cell_length_c                   15.6832(12)
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_cell_measurement_temperature    293
_cell_measurement_theta_max      71.5371
_cell_measurement_theta_min      3.2973
_cell_volume                     2135.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 16.1293
_diffrn_measured_fraction_theta_full 0.7362
_diffrn_measured_fraction_theta_max 0.7362
_diffrn_measurement_details
;
  1 omega  -15.00   20.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -180.0000 35

  2 omega  -61.00  -35.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -180.0000 26

  3 omega  -37.00   24.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000  150.0000 61

  4 omega  -21.00   22.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   63.0000 -180.0000 43

  5 omega  -94.00  -22.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -57.0000 -120.0000 72

  6 omega -118.00  -90.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000 -180.0000 28

  7 omega  -87.00  -40.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  111.0000   30.0000 47

  8 omega -110.00  -63.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -63.0000 -150.0000 47

  9 omega   39.00   94.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -25.0000  -30.0000 55

 10 omega   56.00  109.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.2786 -111.0000   60.0000 53

 11 omega   38.00  115.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.2786 -111.0000 -150.0000 77

 12 omega   63.00   91.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -25.0000 -180.0000 28

 13 omega  100.00  171.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  111.0000 -120.0000 71

 14 omega   69.00  125.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -63.0000  150.0000 56

 15 omega  101.00  127.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  111.0000  150.0000 26

 16 omega   39.00   88.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -38.0000 -120.0000 49

 17 omega   47.00   94.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -25.0000 -120.0000 47

 18 omega   41.00   93.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -38.0000  -60.0000 52
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0891673000
_diffrn_orient_matrix_UB_12      -0.0833427000
_diffrn_orient_matrix_UB_13      -0.0069796000
_diffrn_orient_matrix_UB_21      0.0963991000
_diffrn_orient_matrix_UB_22      0.0995067000
_diffrn_orient_matrix_UB_23      -0.0351110000
_diffrn_orient_matrix_UB_31      -0.0174193000
_diffrn_orient_matrix_UB_32      -0.0296487000
_diffrn_orient_matrix_UB_33      0.1093223000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8035
_diffrn_reflns_theta_full        71.6305
_diffrn_reflns_theta_max         71.63
_diffrn_reflns_theta_min         3.30
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.289
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic whiteish white'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.6749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1066.3007
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.3878
_refine_diff_density_min         -0.9413
_refine_diff_density_rms         0.1626
_refine_ls_d_res_high            0.8123
_refine_ls_d_res_low             13.3921
_refine_ls_goodness_of_fit_ref   1.0564
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    72
_refine_ls_number_parameters     472
_refine_ls_number_reflns         6141
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0564
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.5499
_refine_ls_shift/su_mean         0.1160
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1444P)^2^+0.3325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2058
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_reflns_limit_h_min              -13
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_reflns_limit_k_min              -14
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                4377
_reflns_number_total             6141
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9nj05818d2.cif
_cod_data_source_block           4-CCDC1861565
_cod_depositor_comments
'Adding full bibliography for 7059363--7059367.cif.'
_cod_database_code               7059364
_chemical_oxdiff_formula         'C10 H10 N2 Zn Cl O4'
_reflns_odcompleteness_completeness 76.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Ternary CH refined with riding coordinates:
 C12(H12), C5(H5), C26(H26), C20(H20)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C2(H2), C10(H10), C9(H9), C3(H3), C23(H23), C24(H24), C16(H16)
2.c Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C4(H4a,H4b,H4c), C28(H28a,H28b,H28c), C11(H11a,H11b,
 H11c), C14(H14a,H14b,H14c), C25(H25a,H25b,H25c), C27(H27a,H27b,H27c), C21(H21a,
 H21b,H21c), C18(H18a,H18b,H18c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C19(H19a,
 H19b,H19c)
;
_olex2_submission_special_instructions 'No special instructions were received'