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_7237105
_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         'C54 H72 Cu N4 Se2, F6 P'
_chemical_formula_sum            'C54 H72 Cu F6 N4 P Se2'
_chemical_formula_weight         1143.63
_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)
;
_audit_update_record
;
2018-07-11 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.637(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5751(8)
_cell_length_b                   16.3426(4)
_cell_length_c                   20.4314(10)
_cell_measurement_reflns_used    4398
_cell_measurement_temperature    298
_cell_measurement_theta_max      71.6238
_cell_measurement_theta_min      3.6562
_cell_volume                     5987.8(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
_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  -56.00  -29.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  124.0000   -5.0000 27

  2 omega  -15.00   11.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 26

  3 omega  -48.00   23.00   1.0000    2.9000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000 -180.0000 71

  4 omega  -80.00  -23.00   1.0000    2.9000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -57.0000 -120.0000 57

  5 omega -115.00  -59.00   1.0000    2.9000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000 -120.0000 56

  6 omega  -84.00   29.00   1.0000    2.9000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   19.0000  -60.0000 113

  7 omega   50.00   86.00   1.0000    2.9000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -25.0000  120.0000 36

  8 omega   41.00  114.00   1.0000    2.9000
omega____ theta____ kappa____ phi______ frames
    -      110.2786 -111.0000  120.0000 73

  9 omega   43.00  107.00   1.0000    2.9000
omega____ theta____ kappa____ phi______ frames
    -      110.2786 -111.0000   30.0000 64

 10 omega   39.00   86.00   1.0000    2.9000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -38.0000 -180.0000 47

 11 omega   39.00   83.00   1.0000    2.9000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -38.0000   60.0000 44

 12 omega   80.00  116.00   1.0000    2.9000
omega____ theta____ kappa____ phi______ frames
    -      110.2786 -111.0000 -150.0000 36

 13 omega   42.00   68.00   1.0000    2.9000
omega____ theta____ kappa____ phi______ frames
    -      110.2786 -111.0000 -150.0000 26

 14 omega   96.00  178.00   1.0000    2.9000
omega____ theta____ kappa____ phi______ frames
    -      110.2786   25.0000 -120.0000 82

 15 omega   39.00   82.00   1.0000    2.9000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -25.0000   90.0000 43

 16 omega  120.00  161.00   1.0000    2.9000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  111.0000   90.0000 41
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0302178000
_diffrn_orient_matrix_UB_12      0.0081720000
_diffrn_orient_matrix_UB_13      0.0586446000
_diffrn_orient_matrix_UB_21      0.0782119000
_diffrn_orient_matrix_UB_22      -0.0189954000
_diffrn_orient_matrix_UB_23      0.0573840000
_diffrn_orient_matrix_UB_31      0.0188276000
_diffrn_orient_matrix_UB_32      0.0919558000
_diffrn_orient_matrix_UB_33      0.0066642000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10607
_diffrn_reflns_theta_full        71.7674
_diffrn_reflns_theta_max         71.77
_diffrn_reflns_theta_min         3.66
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.601
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76929
_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    1.2685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2353.1034
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.9039
_refine_diff_density_min         -1.0294
_refine_diff_density_rms         0.0865
_refine_ls_d_res_high            0.8117
_refine_ls_d_res_low             12.0791
_refine_ls_goodness_of_fit_ref   1.0450
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    56
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0450
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1036P)^2^+3.2468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1697
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              21
_reflns_limit_h_min              -24
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                4504
_reflns_number_total             5722
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8ra06057f2.cif
_cod_data_source_block           11
_cod_database_code               7237105
_chemical_oxdiff_formula         'C21 H24 N2 Se Cu P'
_reflns_odcompleteness_completeness 99.95
_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 Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20)
2.c Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C14(H14a,H14b,H14c), C15(H15a,H15b,
 H15c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C26(H26a,H26b,H26c), C27(H27a,
 H27b,H27c)
;
_olex2_submission_special_instructions 'No special instructions were received'