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_7237106
_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         'C21 H24 Cu I N2 S'
_chemical_formula_sum            'C21 H24 Cu I N2 S'
_chemical_formula_weight         526.95
_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'
_symmetry_Int_Tables_number      14
_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)
;
_audit_update_record
;
2018-07-11 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.632(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5024(12)
_cell_length_b                   15.4127(14)
_cell_length_c                   13.6155(16)
_cell_measurement_reflns_used    2859
_cell_measurement_temperature    298.0
_cell_measurement_theta_max      71.1585
_cell_measurement_theta_min      3.5141
_cell_volume                     2227.9(5)
_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      298.0
_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   29.00   54.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  -30.0000 25

  2 omega  -37.00   30.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   38.0000  120.0000 67

  3 omega  -70.00  -39.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000   90.0000 31

  4 omega  -98.00  -72.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000 -150.0000 26

  5 omega   35.00  121.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000   30.0000 86

  6 omega   23.00  107.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000 -120.0000 84

  7 omega  -14.00   73.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   60.0000 87

  8 omega   75.00  101.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 26

  9 omega   58.00   93.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   30.0000 35

 10 omega   36.00   88.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   90.0000 52

 11 omega  134.00  169.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 35

 12 omega   40.00   89.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -60.0000 49

 13 omega   44.00   93.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -120.0000 49

 14 omega   50.00   90.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -180.0000 40

 15 omega   40.00  136.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -120.0000 96

 16 omega   44.00  169.00   1.0000    3.4200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -12.0000 -150.0000 125
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1136665000
_diffrn_orient_matrix_UB_12      0.0587482000
_diffrn_orient_matrix_UB_13      0.0142124000
_diffrn_orient_matrix_UB_21      0.0898607000
_diffrn_orient_matrix_UB_22      -0.0765279000
_diffrn_orient_matrix_UB_23      0.0483404000
_diffrn_orient_matrix_UB_31      -0.0076977000
_diffrn_orient_matrix_UB_32      -0.0256859000
_diffrn_orient_matrix_UB_33      -0.1118211000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8950
_diffrn_reflns_theta_full        71.2983
_diffrn_reflns_theta_max         71.30
_diffrn_reflns_theta_min         4.16
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.179
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32807
_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    1.5709
_exptl_crystal_description       needle
_exptl_crystal_F_000             1042.9361
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.8092
_refine_diff_density_min         -2.8690
_refine_diff_density_rms         0.1881
_refine_ls_d_res_high            0.8139
_refine_ls_d_res_low             10.6167
_refine_ls_goodness_of_fit_ref   1.0724
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    36
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0724
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0851
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2421
_refine_ls_wR_factor_ref         0.3220
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2630
_reflns_number_total             4192
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8ra06057f2.cif
_cod_data_source_block           4
_cod_database_code               7237106
_chemical_oxdiff_formula         'C21 H28 N2 S Cu I'
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C15(H15), C17(H17)
2.b Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C19(H19a,H19b,
 H19c), C20(H20a,H20b,H20c), C21(H21a,H21b,H21c)
;
_olex2_submission_special_instructions 'No special instructions were received'