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_7237103
_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_absolute_configuration unk
_chemical_formula_moiety         'C21 H33 Cu N6 Se3, B F4'
_chemical_formula_sum            'C21 H33 B Cu F4 N6 Se3'
_chemical_formula_weight         756.78
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_Int_Tables_number      92
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.4174(2)
_cell_length_b                   16.4174(2)
_cell_length_c                   22.1831(4)
_cell_measurement_reflns_used    4920
_cell_measurement_temperature    298
_cell_measurement_theta_max      71.3255
_cell_measurement_theta_min      3.3463
_cell_volume                     5979.03(15)
_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   -2.00   40.00   1.0000    2.8000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -30.0000 42

  2 omega  -37.00   23.00   1.0000   11.2100
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000  150.0000 60

  3 omega  -20.00   24.00   1.0000   11.2100
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000    0.0000 44

  4 omega  -20.00   25.00   1.0000   11.2100
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000  -90.0000 45

  5 omega   98.00  157.00   1.0000   11.2100
omega____ theta____ kappa____ phi______ frames
    -      110.2786   77.0000   90.0000 59

  6 omega   41.00   86.00   1.0000   11.2100
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -38.0000 -180.0000 45

  7 omega   46.00   81.00   1.0000   11.2100
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -38.0000   30.0000 35

  8 omega   44.00   96.00   1.0000   11.2100
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -50.0000 -120.0000 52

  9 omega   38.00  114.00   1.0000   11.2100
omega____ theta____ kappa____ phi______ frames
    -      110.2786 -111.0000 -180.0000 76

 10 omega   40.00   66.00   1.0000   11.2100
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -38.0000  120.0000 26
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0442655000
_diffrn_orient_matrix_UB_12      -0.0594867000
_diffrn_orient_matrix_UB_13      0.0425447000
_diffrn_orient_matrix_UB_21      0.0827586000
_diffrn_orient_matrix_UB_22      0.0300796000
_diffrn_orient_matrix_UB_23      -0.0240328000
_diffrn_orient_matrix_UB_31      0.0021519000
_diffrn_orient_matrix_UB_32      0.0659902000
_diffrn_orient_matrix_UB_33      0.0493472000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12308
_diffrn_reflns_theta_full        71.4667
_diffrn_reflns_theta_max         71.47
_diffrn_reflns_theta_min         3.35
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67767
_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    1.6813
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2955.9276
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.3487
_refine_diff_density_min         -0.4325
_refine_diff_density_rms         0.0625
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_d_res_high            0.8131
_refine_ls_d_res_low             13.1964
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0445
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    51
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0445
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+2.2142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.938
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              14
_reflns_limit_k_min              -13
_reflns_limit_l_max              26
_reflns_limit_l_min              -26
_reflns_number_gt                4859
_reflns_number_total             5646
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8ra06057f2.cif
_cod_data_source_block           14
_cod_original_cell_volume        5979.02(16)
_cod_original_sg_symbol_Hall     ' P 4abw 2nw'
_cod_database_code               7237103
_chemical_oxdiff_formula         'C21 H24 N2 S Cu O F Cl B'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4), C11(H11), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C14(H14a,H14b), C21(H21a,H21b)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C3(H3), C2(H2), C10(H10), C16(H16), C17(H17)
2.d Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C6(H6a,H6b,H6c), C5(H5a,H5b,H5c), C12(H12a,H12b,H12c),
 C20(H20a,H20b,H20c), C19(H19a,H19b,H19c)
;
_olex2_submission_special_instructions 'No special instructions were received'