Dicationic Copper(I) Complexes Bearing ENE (E = S, Se) Pincer Ligands; Catalytic Applications in Regioselective Cyclization of 1,6-diynes
Das, Bhagyashree Ms; Sahoo, Amiya Kumar; Banjare, Shyam Kumar; Panda, Subhra Jyoti; Purohit, Chandra Shekhar; Doddi, Adinarayana; Dalton Transactions  (2023) –; doi:10.1039/D3DT01989F

data_7713743
_publ_section_title
;
 Dicationic Copper(I) Complexes Bearing ENE (E = S, Se) Pincer Ligands;
 Catalytic Applications in Regioselective Cyclization of 1,6-diynes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01989F
_journal_year                    2023
_chemical_formula_moiety         'C58 H46 Cu2 N2 P4 S4, 2(B F4), 0.34(H2 O)'
_chemical_formula_sum            'C58 H46.68 B2 Cu2 F8 N2 O0.34 P4 S4'
_chemical_formula_weight         1329.91
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-04-19 deposited with the CCDC.	2023-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.917(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.6320(8)
_cell_length_b                   13.0574(4)
_cell_length_c                   17.0639(4)
_cell_measurement_reflns_used    22284
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.3540
_cell_measurement_theta_min      3.6260
_cell_volume                     5902.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9964
_diffrn_measured_fraction_theta_max 0.8027
_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    -16.00  11.00   0.50    3.50    --    3.51 -89.00-119.00   54
  2  \w    -30.00  23.00   0.50    3.50    --   -4.14 -89.00-119.00  106
  3  \w    -15.00  31.00   0.50    3.50    --    3.51 -99.00  30.00   92
  4  \w    -67.00  -3.00   0.50    3.50    --   -4.14 -37.00  30.00  128
  5  \w    -18.00  21.00   0.50    3.50    --   -4.14  77.00 120.00   78
  6  \w    -15.00  16.00   0.50    3.50    --   -4.14 -99.00 -30.00   62
  7  \w    -14.00  19.00   0.50    3.50    --   -4.14  77.00-150.00   66
  8  \w    -22.00   4.00   0.50    3.50    --   -4.14  77.00   0.00   52
  9  \w     -6.00  25.00   0.50    3.50    --   -4.14 -99.00  90.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0241975000
_diffrn_orient_matrix_UB_12      -0.0231876000
_diffrn_orient_matrix_UB_13      0.0049607000
_diffrn_orient_matrix_UB_21      0.0104810000
_diffrn_orient_matrix_UB_22      0.0435537000
_diffrn_orient_matrix_UB_23      -0.0170665000
_diffrn_orient_matrix_UB_31      0.0046131000
_diffrn_orient_matrix_UB_32      0.0227165000
_diffrn_orient_matrix_UB_33      0.0378355000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.803
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            63264
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.803
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.569
_diffrn_reflns_theta_min         3.365
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.037
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       block
_exptl_crystal_F_000             2702
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow vapour diffusion'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.200
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         14558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+10.8289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1393
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10694
_reflns_number_total             14558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01989f2.cif
_cod_data_source_block           sjp-bd-211
_cod_database_code               7713743
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C236 H198 B8 Cl8 Cu8 F40 N8 O4 P16 S16 '
_chemical_oxdiff_usercomment     'DARK ORANGE BLOCK'
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.760
_diffrn_oxdiff_digest_frames
;
01ac92a0e07a65e65c6046f66947cbdfcc007003094
;
_diffrn_oxdiff_digest_hkl
;
01fbc0ae48d81f759c248828b9a9bf0ccb7320
;
_reflns_odcompleteness_completeness 99.64
_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 O(H,H) groups
2. Others
 Fixed Sof: F7(0.5) F11(0.5) F9(0.5) F5(0.5) F10(0.5) F4(0.5) F12(0.5) F8(0.5)
 O1(0.34) H1A(0.34) H1B(0.34)
3.a Free rotating group:
 O1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C45(H45), C31(H31), C14(H14), C43(H43), C16(H16), C35(H35),
 C25(H25), C38(H38), C28(H28), C44(H44), C48(H48), C33(H33), C26(H26), C37(H37),
  C15(H15), C58(H58), C32(H32), C34(H34), C6(H6), C23(H23), C11(H11), C12(H12),
 C27(H27), C22(H22), C39(H39), C2(H2), C52(H52), C5(H5), C3(H3), C49(H49),
 C57(H57), C21(H21), C10(H10), C4(H4), C19(H19), C51(H51), C50(H50), C8(H8),
 C41(H41), C54(H54), C40(H40), C9(H9), C56(H56), C20(H20), C55(H55)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25614
_shelx_fab_checksum              55047
_olex2_exptl_crystal_mounting_method 'Mounted on the loop'
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.175
_oxdiff_exptl_absorpt_empirical_full_min 0.823