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_7059366
_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(B F5)'
_chemical_formula_sum            'C28 H48 B2 F10 N8 Se4 Zn'
_chemical_formula_weight         1089.61
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_symmetry_Int_Tables_number      88
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-22 deposited with the CCDC.	2020-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4234(2)
_cell_length_b                   12.4234(2)
_cell_length_c                   27.7432(11)
_cell_measurement_reflns_used    1659
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.5810
_cell_measurement_theta_min      3.1832
_cell_volume                     4281.9(2)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.0
_diffrn_detector_area_resol_mean 16.1293
_diffrn_measured_fraction_theta_full 0.9946
_diffrn_measured_fraction_theta_max 0.9769
_diffrn_measurement_details
;
  1 omega  -57.00  -30.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   30.0000 27

  2 omega  -14.00   14.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   30.0000 28

  3 omega   36.00  117.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -30.0000 81

  4 omega   15.00   69.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000 -180.0000 54

  5 omega   39.00   97.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -60.0000 58

  6 omega   39.00   99.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   90.0000 60

  7 omega   39.00   71.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -120.0000 32

  8 omega   37.00   79.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -90.0000 42

  9 omega   38.00   89.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -180.0000 51

 10 omega   43.00   68.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -30.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0795398000
_diffrn_orient_matrix_UB_12      -0.0952308000
_diffrn_orient_matrix_UB_13      0.0001985000
_diffrn_orient_matrix_UB_21      -0.0929302000
_diffrn_orient_matrix_UB_22      -0.0777184000
_diffrn_orient_matrix_UB_23      -0.0119449000
_diffrn_orient_matrix_UB_31      0.0206524000
_diffrn_orient_matrix_UB_32      0.0168598000
_diffrn_orient_matrix_UB_33      -0.0541770000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            4375
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         70.72
_diffrn_reflns_theta_min         3.90
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.351
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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    1.6901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2138.9865
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.3203
_refine_diff_density_min         -0.6658
_refine_diff_density_rms         0.1168
_refine_ls_d_res_high            0.8167
_refine_ls_d_res_low             11.3385
_refine_ls_goodness_of_fit_ref   1.0413
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0413
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1067P)^2^+0.6380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1735
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                1450
_reflns_number_total             2026
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9nj05818d2.cif
_cod_data_source_block           3-CCDC1861564
_cod_depositor_comments
'Adding full bibliography for 7059363--7059367.cif.'
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7059366
_chemical_oxdiff_formula         'C20 H16 N4 Se2 Zn B F4'
_reflns_odcompleteness_completeness 99.90
_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:
 C5(H5)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2)
2.c Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C4(H4a,H4b,H4c), C6(H6a,H6b,H6c)
;
_olex2_submission_special_instructions 'No special instructions were received'