Role of C, S, Se and P donor ligands in copper(i) mediated C‒N and C‒Si bond formation reactions
Srinivas, Katam; Prabusankar, Ganesan; RSC Advances 8 (2018) 32269–; doi:10.1039/C8RA06057F

data_7237110
_publ_section_title
;
 Role of C, S, Se and P donor ligands in copper(i) mediated C--N and C--Si
 bond formation reactions
;
_journal_issue                   56
_journal_name_full               'RSC Advances'
_journal_page_first              32269
_journal_paper_doi               10.1039/C8RA06057F
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C72 H60 Cu4 I4 P4, 2(C2 N)'
_chemical_formula_sum            'C76 H60 Cu4 I4 N2 P4'
_chemical_formula_weight         1887.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     direct
_audit_creation_date             2017-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
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_audit_update_record
;
2018-07-11 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.048(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.6333(12)
_cell_length_b                   16.1396(6)
_cell_length_c                   18.2784(8)
_cell_measurement_reflns_used    5713
_cell_measurement_temperature    298
_cell_measurement_theta_max      71.4321
_cell_measurement_theta_min      3.2559
_cell_volume                     7380.9(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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      298
_diffrn_detector_area_resol_mean 16.1293
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_details
;
  1 omega   28.00   55.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 27

  2 omega  -43.00    6.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  115.0000  168.0000 49

  3 omega  -47.00  -21.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -57.0000  -60.0000 26

  4 omega  -27.00   25.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000    0.0000 52

  5 omega  -22.00   28.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000  120.0000 50

  6 omega -106.00  -80.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -57.0000  -60.0000 26

  7 omega -104.00  -48.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000 -168.0000  -65.0000 56

  8 omega  -13.00   85.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       55.1511  -77.0000 -180.0000 98

  9 omega   47.00  133.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.3022  -77.0000  -60.0000 86

 10 omega   82.00  178.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.3022   77.0000   30.0000 96

 11 omega   44.00   78.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.3022  -25.0000  120.0000 34

 12 omega  101.00  151.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.3022  115.0000  -11.0000 50

 13 omega   58.00   83.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.3022  -25.0000  -60.0000 25

 14 omega   88.00  174.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.3022   63.0000   90.0000 86

 15 omega  109.00  150.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.3022  178.0000   30.0000 41

 16 omega   80.00  177.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      110.3022   77.0000   60.0000 97
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0344327000
_diffrn_orient_matrix_UB_12      0.0681044000
_diffrn_orient_matrix_UB_13      0.0529719000
_diffrn_orient_matrix_UB_21      -0.0501048000
_diffrn_orient_matrix_UB_22      0.0349965000
_diffrn_orient_matrix_UB_23      0.0129432000
_diffrn_orient_matrix_UB_31      0.0101800000
_diffrn_orient_matrix_UB_32      -0.0570095000
_diffrn_orient_matrix_UB_33      0.0711575000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13446
_diffrn_reflns_theta_full        71.5742
_diffrn_reflns_theta_max         71.57
_diffrn_reflns_theta_min         3.26
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.579
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13326
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.6980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3650.2058
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.5340
_refine_diff_density_min         -3.1965
_refine_diff_density_rms         0.2671
_refine_ls_d_res_high            0.8126
_refine_ls_d_res_low             13.5625
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0268
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    60
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0268
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0790
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1672P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2104
_refine_ls_wR_factor_ref         0.2419
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              30
_reflns_limit_h_min              -32
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                5546
_reflns_number_total             7046
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8ra06057f2.cif
_cod_data_source_block           12
_cod_database_code               7237110
_chemical_oxdiff_formula         'C21 H24 N2 Se P Cu I'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C2aa(H2aa), C3(H3), C3aa(H3aa), C4(H4), C5(H5), C6(H6), C8(H8),
 C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C32(H32), C35(H35), C36(H36)
;
_olex2_submission_special_instructions 'No special instructions were received'