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_7713742
_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 Se4, C H2 Cl2, 2(B F4)'
_chemical_formula_sum            'C59 H48 B2 Cl2 Cu2 F8 N2 P4 Se4'
_chemical_formula_weight         1596.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 100.231(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4083(4)
_cell_length_b                   24.9105(8)
_cell_length_c                   17.3957(6)
_cell_measurement_reflns_used    16689
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.4250
_cell_measurement_theta_min      3.5330
_cell_volume                     6144.4(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 2014/5 (Sheldrick, 2014)'
_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 0.9963
_diffrn_measured_fraction_theta_max 0.7987
_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     -2.00  39.00   0.50    4.20    --    3.51 -99.00-170.00   82
  2  \w    -15.00  31.00   0.50    4.20    --   -4.14 -99.00-170.00   92
  3  \w    -13.00  33.00   0.50    4.20    --    3.51 -99.00 150.00   92
  4  \w    -13.00  31.00   0.50    4.20    --    3.51 -99.00   0.00   88
  5  \w      0.00  70.00   0.50    4.20    --    3.51  37.00  30.00  140
  6  \w      2.00  31.00   0.50    4.20    --   -4.14 -99.00 -90.00   58
  7  \w    -15.00  23.00   0.50    4.20    --   -4.14 -99.00  60.00   76
  8  \w    -25.00  20.00   0.50    4.20    --   -4.14  77.00  30.00   90
;
_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      -0.0318180000
_diffrn_orient_matrix_UB_12      0.0126791000
_diffrn_orient_matrix_UB_13      -0.0304062000
_diffrn_orient_matrix_UB_21      0.0024880000
_diffrn_orient_matrix_UB_22      0.0238829000
_diffrn_orient_matrix_UB_23      0.0224073000
_diffrn_orient_matrix_UB_31      0.0385370000
_diffrn_orient_matrix_UB_32      0.0089246000
_diffrn_orient_matrix_UB_33      -0.0170028000
_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  0.0685
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.799
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            69099
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.595
_diffrn_reflns_theta_min         3.306
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.318
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66212
_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 reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_description       block
_exptl_crystal_F_000             3144
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Vapour diffusion'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.480
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         15100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+10.9959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11160
_reflns_number_total             15100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01989f2.cif
_cod_data_source_block           sjp-bd-210
_cod_database_code               7713742
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C232 H196 B8 Cl8 Cu8 F36 N12 P16 Se16 '
_chemical_oxdiff_usercomment     'DARAK ORANGE RED CRYSTAL'
_shelx_estimated_absorpt_t_max   0.479
_shelx_estimated_absorpt_t_min   0.436
_diffrn_oxdiff_digest_frames
;
010b11238a9d4057698ed2170a245bcafa00718562c
;
_diffrn_oxdiff_digest_hkl
;
018b9802a5932402945a1b8b9620013b58c844
;
_reflns_odcompleteness_completeness 99.63
_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
2. Others
 Fixed Sof: Se1(0.94) Se2(0.06) Cl3(0.615) Cl2(0.385) F7(0.5) F9(0.37)
 F11(0.67) F6(0.5) F8(0.63) F10(0.33)
3.a Secondary CH2 refined with riding coordinates:
 C59(H59a,H59b)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31),
 C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40),
  C41(H41), C43(H43), C44(H44), C45(H45), C48(H48), C49(H49), C50(H50),
 C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58)
;
_shelx_res_checksum              45632
_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 1.604
_oxdiff_exptl_absorpt_empirical_full_min 0.662