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_7713941
_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         'F6 Sb, C42 H46 Ag P2 Si2'
_chemical_formula_sum            'C42 H46 Ag F6 P2 Sb Si2'
_chemical_formula_weight         1012.53
_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             2023-01-28
_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                98.729(2)
_cell_angle_beta                 91.481(2)
_cell_angle_gamma                101.102(2)
_cell_formula_units_Z            1
_cell_length_a                   8.2983(2)
_cell_length_b                   10.5547(3)
_cell_length_c                   12.5094(3)
_cell_measurement_reflns_used    12765
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.3310
_cell_measurement_theta_min      3.6330
_cell_volume                     1060.98(5)
_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      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.7116
_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    -74.00  16.00   0.50    0.10    --  -38.50  98.00  57.00  180
  2  \w      5.00  84.00   0.50    0.10    --   49.06 -98.00 -49.00  158
  3  \w    104.00 176.00   0.50    0.30    --  107.46  98.00  57.00  144
  4  \w     39.00 107.00   0.50    0.30    --  107.46 -98.00 -49.00  136
  5  \w    -42.00  28.00   0.50    0.10    --  -38.50  37.00 -90.00  140
  6  \w   -101.00 -26.00   0.50    0.10    --  -38.50 -59.00-178.15  150
  7  \w   -105.00 -35.00   0.50    0.10    --  -38.50 -37.00  90.00  140
  8  \w   -101.00 -27.00   0.50    0.10    --  -38.50 -57.00 -90.00  148
  9  \w    -86.00  -6.00   0.50    0.10    --  -38.50 125.00 -90.00  160
 10  \w    -20.00  55.00   0.50    0.10    --   49.06 -19.00 120.00  150
 11  \w     28.00 100.00   0.50    0.10    --   49.06-125.00 -90.00  144
 12  \w    -17.00  52.00   0.50    0.10    --   49.06 -37.00  60.00  138
 13  \w     45.00 121.00   0.50    0.30    --  107.46 -61.00 150.00  152
 14  \w    103.00 172.00   0.50    0.30    --  107.46  45.00 -60.00  138
 15  \w     39.00 107.00   0.50    0.30    --  107.46 -94.00-180.00  136
 16  \w     39.00 107.00   0.50    0.30    --  107.46 -94.00-150.00  136
 17  \w     39.00 107.00   0.50    0.30    --  107.46 -94.00 120.00  136
 18  \w    103.00 172.00   0.50    0.30    --  107.46  45.00  30.00  138
 19  \w    104.00 176.00   0.50    0.30    --  107.46  30.00   0.00  144
 20  \w     43.00 112.00   0.50    0.30    --  107.46 -45.00 -90.00  138
 21  \w     39.00 116.00   0.50    0.30    --  107.46 -15.00-180.00  154
 22  \w     43.00 113.00   0.50    0.30    --  107.46-125.00  90.00  140
 23  \w     45.00 121.00   0.50    0.30    --  107.46 -61.00  60.00  152
 24  \w     43.00 113.00   0.50    0.30    --  107.46-125.00 -90.00  140
 25  \w     43.00 112.00   0.50    0.30    --  107.46 -45.00-180.00  138
 26  \w     43.00 112.00   0.50    0.30    --  107.46 -45.00   0.00  138
 27  \w     43.00 112.00   0.50    0.30    --  107.46 -45.00  60.00  138
 28  \w     43.00 131.00   0.50    0.30    --  107.46 -77.00 -60.00  176
 29  \w     43.00 131.00   0.50    0.30    --  107.46 -77.00 -90.00  176
 30  \w     39.00 111.00   0.50    0.30    --  107.46 -30.00  30.00  144
 31  \w     96.00 170.00   0.50    0.30    --  107.46  57.00-153.77  148
 32  \w     99.00 171.00   0.50    0.30    --  107.46  54.00 -35.61  144
 33  \w   -101.00 -21.00   0.50    0.10    --  -38.50 -68.00  -2.46  160
 34  \w     31.00  96.00   0.50    0.10    --   49.06  69.00  73.91  130
 35  \w     38.00 112.00   0.50    0.10    --   49.06  57.00-180.00  148
;
_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      -0.0253971000
_diffrn_orient_matrix_UB_12      0.0591380000
_diffrn_orient_matrix_UB_13      0.1172286000
_diffrn_orient_matrix_UB_21      0.1738849000
_diffrn_orient_matrix_UB_22      0.0857002000
_diffrn_orient_matrix_UB_23      0.0076763000
_diffrn_orient_matrix_UB_31      -0.0709016000
_diffrn_orient_matrix_UB_32      0.1089157000
_diffrn_orient_matrix_UB_33      -0.0421051000
_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  0.0815
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16610
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.824
_diffrn_reflns_theta_min         3.580
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.480
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26182
_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    1.585
_exptl_crystal_description       plate
_exptl_crystal_F_000             508
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow vapour diffusion'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.383
_refine_diff_density_min         -1.738
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+0.1803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4122
_reflns_number_total             4411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01692g2.cif
_cod_data_source_block           sjp-as-211_auto
_cod_database_code               7713941
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H N P Si Ag Sb F'
_chemical_oxdiff_usercomment     'COLOURLESS PLATES'
_shelx_estimated_absorpt_t_max   0.228
_shelx_estimated_absorpt_t_min   0.129
_diffrn_oxdiff_digest_frames
;
015b6754dd3a80a8fd90ca86d19342d8d800041b2b0
;
_diffrn_oxdiff_digest_hkl
;
0137af9fc2d240470341d5795d7b4016ad0d47
;
_reflns_odcompleteness_completeness 99.90
_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:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17)
2.b Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C21(H21a,H21b,H21c)
;
_shelx_res_checksum              118
_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 2.647
_oxdiff_exptl_absorpt_empirical_full_min 0.503