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_7059069
_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         'C32 H30 Br4 N6 Se2 Zn2, C6 H6'
_chemical_formula_sum            'C38 H36 Br4 N6 Se2 Zn2'
_chemical_formula_weight         1185.07
_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     iterative
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2019-11-13 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                70.474(8)
_cell_angle_beta                 77.488(7)
_cell_angle_gamma                76.996(7)
_cell_formula_units_Z            1
_cell_length_a                   7.5364(5)
_cell_length_b                   12.0785(11)
_cell_length_c                   13.2048(12)
_cell_measurement_reflns_used    2606
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.0042
_cell_measurement_theta_min      2.9927
_cell_volume                     1090.66(17)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
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(compiled Oct 27 2011,15:02:11)
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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)'
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_diffrn_ambient_temperature      293.0
_diffrn_detector_area_resol_mean 16.1293
_diffrn_measured_fraction_theta_full 0.9987
_diffrn_measured_fraction_theta_max 0.8464
_diffrn_measurement_details
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  1 omega    0.00   46.00   1.0000    3.3200
omega____ theta____ kappa____ phi______ frames
    -      -17.7643   57.0000   60.0000 46

  2 omega  -38.00   -6.00   1.0000    3.3200
omega____ theta____ kappa____ phi______ frames
    -      -17.7643   57.0000 -120.0000 32

  3 omega  -63.00  -32.00   1.0000    3.3200
omega____ theta____ kappa____ phi______ frames
    -      -17.7643  105.0000   86.0000 31

  4 omega   -9.00   90.00   1.0000    3.3200
omega____ theta____ kappa____ phi______ frames
    -       19.6393   77.0000    0.0000 99

  5 omega  -49.00   41.00   1.0000    3.3200
omega____ theta____ kappa____ phi______ frames
    -       19.6393  -57.0000  120.0000 90

  6 omega  -10.00   16.00   1.0000    3.3200
omega____ theta____ kappa____ phi______ frames
    -       19.6393 -105.0000  -13.0000 26

  7 omega   -2.00   88.00   1.0000    3.3200
omega____ theta____ kappa____ phi______ frames
    -       19.6393   57.0000  -90.0000 90
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_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
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_diffrn_orient_matrix_UB_32      0.0135345000
_diffrn_orient_matrix_UB_33      0.0152038000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8943
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         29.07
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.465
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39460
_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.
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_exptl_crystal_colour            'metallic brownish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.8041
_exptl_crystal_description       prism
_exptl_crystal_F_000             573.6335
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_exptl_crystal_size_min          0.3
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_refine_ls_matrix_type           full
_refine_ls_number_constraints    33
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0106
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_refine_ls_R_factor_gt           0.0467
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0341P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                3258
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_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9nj04440j2.cif
_cod_data_source_block           5
_cod_depositor_comments
;Adding full bibliography for 7059065--7059073.cif.

 Adding full bibliography for 7059065--7059073.cif.
;
_cod_original_cell_volume        1090.67(17)
_cod_database_code               7059069
_chemical_oxdiff_formula         'C20 H20 N4 Se Zn Br'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C12(H12), C6(H6), C9(H9), C8(H8), C7(H7), C15(H15), C13(H13),
 C14(H14), C5(H5), C18(H18), C17(H17), C19(H19)
2.c Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c)
;
_olex2_submission_special_instructions 'No special instructions were received'