New Cationic Coinage Metal Complexes Featuring Silyl Group Functionalized Phosphine; Syntheses, Structures and Catalytic Studies in Alkyne-Azide Cycloaddition Reactions
Sahoo, Amiya Kumar; Sahoo, Ashish Kumar; Das, Bhagyashree Ms; Panda, Subhra Jyoti; Purohit, Chandra Shekhar; Doddi, Adinarayana; Dalton Transactions  (2023) –; doi:10.1039/D3DT01692G

data_7713938
_publ_section_title
;
 New Cationic Coinage Metal Complexes Featuring Silyl Group Functionalized
 Phosphine; Syntheses, Structures and Catalytic Studies in Alkyne-Azide
 Cycloaddition Reactions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01692G
_journal_year                    2023
_chemical_formula_moiety         'C44 H49 Cu N P2 Si2, B F4'
_chemical_formula_sum            'C44 H49 B Cu F4 N P2 Si2'
_chemical_formula_weight         860.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-05-23 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                93.9050(10)
_cell_angle_beta                 105.2530(10)
_cell_angle_gamma                106.9030(10)
_cell_formula_units_Z            2
_cell_length_a                   13.13560(10)
_cell_length_b                   13.50820(10)
_cell_length_c                   13.79440(10)
_cell_measurement_reflns_used    24458
_cell_measurement_temperature    293(7)
_cell_measurement_theta_max      77.6110
_cell_measurement_theta_min      3.6760
_cell_volume                     2231.52(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9783
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -71.00  22.00   0.50    0.50    --  -38.50  93.00-139.00  186
  2  \w      0.00  82.00   0.50    0.50    --   49.56 -93.00 108.00  164
  3  \w    104.00 176.00   0.50    1.00    --  107.46  93.00-139.00  144
  4  \w     39.00 106.00   0.50    1.00    --  107.46 -93.00 108.00  134
  5  \w    -42.00  28.00   0.50    0.50    --  -38.50  37.00 -30.00  140
  6  \w   -101.00 -22.00   0.50    0.50    --  -38.50 -67.00 110.48  158
  7  \w   -108.00 -33.00   0.50    0.50    --  -38.50 -19.00  30.00  150
  8  \w   -105.00 -35.00   0.50    0.50    --  -38.50 -37.00 -30.00  140
  9  \w     28.00 101.00   0.50    0.50    --   49.56-125.00  60.00  146
 10  \w    -13.00  61.00   0.50    0.50    --   49.56 -57.00 -30.00  148
 11  \w    -17.00  53.00   0.50    0.50    --   49.56 -37.00-150.00  140
 12  \w     39.00 111.00   0.50    1.00    --  107.46 -30.00 150.00  144
 13  \w     95.00 170.00   0.50    1.00    --  107.46  61.00 -60.00  150
 14  \w     45.00 121.00   0.50    1.00    --  107.46 -61.00-180.00  152
 15  \w     43.00 113.00   0.50    1.00    --  107.46-125.00 -30.00  140
 16  \w     97.00 172.00   0.50    1.00    --  107.46 125.00  60.00  150
 17  \w    104.00 176.00   0.50    1.00    --  107.46  30.00-150.00  144
 18  \w     43.00 112.00   0.50    1.00    --  107.46 -45.00  60.00  138
 19  \w     45.00 121.00   0.50    1.00    --  107.46 -61.00 -30.00  152
 20  \w     39.00 107.00   0.50    1.00    --  107.46 -94.00   0.00  136
 21  \w     95.00 170.00   0.50    1.00    --  107.46  61.00 -30.00  150
 22  \w     99.00 176.00   0.50    1.00    --  107.46  15.00  90.00  154
 23  \w     39.00 107.00   0.50    1.00    --  107.46 -94.00-150.00  136
 24  \w     43.00 113.00   0.50    1.00    --  107.46-125.00 120.00  140
 25  \w     39.00 107.00   0.50    1.00    --  107.46 -94.00-180.00  136
 26  \w     44.00 120.00   0.50    1.00    --  107.46-135.00  98.02  152
 27  \w     45.00 121.00   0.50    1.00    --  107.46 -61.00 150.00  152
 28  \w    103.00 172.00   0.50    1.00    --  107.46  77.00  90.00  138
 29  \w     38.00 109.00   0.50    1.00    --  107.46-111.00 -21.01  142
 30  \w     43.00 112.00   0.50    1.00    --  107.46 -45.00 -60.00  138
 31  \w     39.00 107.00   0.50    1.00    --  107.46 -94.00 150.00  136
 32  \w    114.00 172.00   0.50    1.00    --  107.46  45.00-180.00  116
 33  \w     97.00 168.00   0.50    1.00    --  107.46  56.00 128.44  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0694311000
_diffrn_orient_matrix_UB_12      0.0113399000
_diffrn_orient_matrix_UB_13      -0.1051119000
_diffrn_orient_matrix_UB_21      0.0486766000
_diffrn_orient_matrix_UB_22      0.1201478000
_diffrn_orient_matrix_UB_23      0.0280078000
_diffrn_orient_matrix_UB_31      0.0963400000
_diffrn_orient_matrix_UB_32      -0.0009764000
_diffrn_orient_matrix_UB_33      -0.0436349000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35737
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.942
_diffrn_reflns_theta_min         3.362
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.273
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.52a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow vapour diffusion'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.00108(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         9320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0542P)^2^+0.4339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8507
_reflns_number_total             9320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01692g2.cif
_cod_data_source_block           ska-ad-as-208_auto
_cod_database_code               7713938
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H Cu N P Si'
_chemical_oxdiff_usercomment     'colourless block'
_shelx_estimated_absorpt_t_max   0.647
_shelx_estimated_absorpt_t_min   0.611
_diffrn_oxdiff_digest_frames
;
01737243b541f54b9e3024d60c553787ed00031cdef
;
_diffrn_oxdiff_digest_hkl
;
01730c1cfd3aa02b9f2970d500ac05baaea692
;
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25),
  C26(H26), C27(H27), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              65257
_olex2_exptl_crystal_mounting_method 'Mounted on the loop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.296
_oxdiff_exptl_absorpt_empirical_full_min 0.768