Highly active mesoionic chalcogenone zinc(ii) derivatives for C‒S cross-coupling reactions
Vaddamanu, Moulali; Velappan, Kavitha; Prabusankar, Ganesan; New Journal of Chemistry 44 (2020) 129–140; doi:10.1039/C9NJ04440J

data_7059073
_publ_section_title
;
 Highly active mesoionic chalcogenone zinc(ii) derivatives for C--S
 cross-coupling reactions
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              129
_journal_page_last               140
_journal_paper_doi               10.1039/C9NJ04440J
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C36 H38 Br4 N6 Se2 Zn2'
_chemical_formula_sum            'C36 H38 Br4 N6 Se2 Zn2'
_chemical_formula_weight         1163.02
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2019-10-20
_audit_creation_method
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Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
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_audit_update_record
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2019-10-25 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.367(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0434(3)
_cell_length_b                   13.9747(4)
_cell_length_c                   15.7202(5)
_cell_measurement_reflns_used    2451
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9908
_cell_measurement_theta_min      2.9924
_cell_volume                     2155.19(12)
_computing_cell_refinement
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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_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)
;
_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)
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_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293.0
_diffrn_detector_area_resol_mean 16.1293
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.8632
_diffrn_measurement_details
;
  1 omega  -22.00    3.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1894  -57.0000 -180.0000 25

  2 omega  -69.00  -28.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1894  121.0000  150.0000 41

  3 omega  -47.00   40.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2206  -57.0000  -90.0000 87

  4 omega   35.00   92.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2206  178.0000   90.0000 57

  5 omega    5.00   66.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2206   77.0000   90.0000 61
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0204555000
_diffrn_orient_matrix_UB_12      -0.0466317000
_diffrn_orient_matrix_UB_13      -0.0151793000
_diffrn_orient_matrix_UB_21      -0.0175035000
_diffrn_orient_matrix_UB_22      0.0175201000
_diffrn_orient_matrix_UB_23      -0.0433251000
_diffrn_orient_matrix_UB_31      0.0670992000
_diffrn_orient_matrix_UB_32      -0.0096369000
_diffrn_orient_matrix_UB_33      -0.0052711000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10913
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         29.05
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.542
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89835
_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            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.7921
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1127.2659
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.2257
_refine_diff_density_min         -1.5456
_refine_diff_density_rms         0.2303
_refine_ls_d_res_high            0.7317
_refine_ls_d_res_low             6.7935
_refine_ls_goodness_of_fit_ref   1.0394
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     229
_refine_ls_number_reflns         4978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0394
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.1774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1318
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                2963
_reflns_number_total             4978
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9nj04440j2.cif
_cod_data_source_block           2
_cod_depositor_comments
;Adding full bibliography for 7059065--7059073.cif.

 Adding full bibliography for 7059065--7059073.cif.
;
_cod_original_cell_volume        2155.19(11)
_cod_database_code               7059073
_chemical_oxdiff_formula         'C26 H20 N4 Se Zn Br2'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 Aromatic/amide H refined with riding coordinates:
 C14(H14), C8(H8), C9(H9), C12(H12), C7(H7), C6(H6), C5(H5)
2.b Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C3(H3a,H3b,H3c), C16(H16a,H16b,H16c)
;
_olex2_submission_special_instructions 'No special instructions were received'