Synthesis and structural studies of Cu(i) methylthiosalicylate complexes and their catalytic application in thiol-yne click reaction
Kumar, Krishna; Tiwari, Priyanka; Kant, Rajni; Bhattacharya, Subrato; New Journal of Chemistry 46 (2022) 17854–17864; doi:10.1039/D2NJ02722D

data_7061764
_publ_section_title
;
 Synthesis and structural studies of Cu(i) methylthiosalicylate complexes
 and their catalytic application in thiol-yne click reaction
;
_journal_issue                   37
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17854
_journal_page_last               17864
_journal_paper_doi               10.1039/D2NJ02722D
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C42 H35 Cu Fe O2 P2 S'
_chemical_formula_sum            'C42 H35 Cu Fe O2 P2 S'
_chemical_formula_weight         785.09
_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
_audit_block_doi                 10.5517/ccdc.csd.cc23wyvt
_audit_creation_date             2022-07-23
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.06.10 svn.r3fa896fb for OlexSys, GUI svn.r6535)
;
_audit_update_record
;
2022-08-22 deposited with the CCDC.	2022-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.992(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.521(7)
_cell_length_b                   19.574(11)
_cell_length_c                   16.525(8)
_cell_measurement_reflns_used    9205
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.14
_cell_volume                     3564(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1099
_diffrn_reflns_av_unetI/netI     0.0990
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12775
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        21.202
_diffrn_reflns_theta_max         21.202
_diffrn_reflns_theta_min         2.081
_exptl_absorpt_coefficient_mu    1.189
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-yellow
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       Rod-shape
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.2421
_refine_diff_density_max         1.290
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         3892
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0761
_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^)+(0.0332P)^2^+26.8927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2674
_reflns_number_total             3892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj02722d2.cif
_cod_data_source_block           kk26
_cod_depositor_comments
'Adding full bibliography for 7061763--7061765.cif.'
_cod_database_code               7061764
_shelx_shelxl_version_number     2018/3
_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. Uiso/Uaniso restraints and constraints
Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C7(H7), C6(H6), C10(H10)
3.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C15(H15), C14(H14), C13(H13), C12(H12), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C24(H24), C28(H28), C27(H27), C26(H26), C25(H25),
  C34(H34), C30(H30), C31(H31), C32(H32), C33(H33), C36(H36), C37(H37),
 C38(H38), C39(H39)
3.c Fitted pentagon refined as free rotating group:
 C5(C1,C2,C3,C4), C9(C8,C7,C6,C10)
3.d Fitted hexagon refined as free rotating group:
 C16(C15,C14,C13,C12,C11), C17(C18,C19,C20,C21,C22), C24(C23,C28,C27,C26,C25),
 C34(C29,C30,C31,C32,C33), C35(C36,C37,C38,C39,C40)
3.e Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C)
;
_shelx_res_checksum              97078
_olex2_submission_special_instructions 'No special instructions were received'