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_7713942
_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         'C42 H46 Ag N O3 P2 Si2, H2 O'
_chemical_formula_sum            'C42 H48 Ag N O4 P2 Si2'
_chemical_formula_weight         856.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-05-23 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.6194(3)
_cell_length_b                   22.2002(4)
_cell_length_c                   23.7789(4)
_cell_measurement_reflns_used    27039
_cell_measurement_temperature    99.98
_cell_measurement_theta_max      77.8060
_cell_measurement_theta_min      3.3940
_cell_volume                     8245.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9976
_diffrn_measured_fraction_theta_max 0.9719
_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    -67.00  -8.00   0.50    1.00    --  -38.50 127.00  -1.00  118
  2  \w    -92.00 -16.00   0.50    1.00    --  -38.50 143.00 167.00  152
  3  \w     41.00  66.00   0.50    1.00    --   49.31-127.00 -77.00   50
  4  \w     44.00 100.00   0.50    2.00    --  107.46-127.00 -77.00  112
  5  \w     88.00 149.00   0.50    2.00    --  107.46 143.00 167.00  122
  6  \w    -28.00  -1.00   0.50    1.00    --  -38.50  37.00 120.00   54
  7  \w    -67.00 -40.00   0.50    1.00    --  -38.50 -57.00 -60.00   54
  8  \w    -17.00  52.00   0.50    1.00    --   49.31 -37.00 -90.00  138
  9  \w    104.00 151.00   0.50    2.00    --  107.46  77.00  60.00   94
 10  \w    145.00 170.00   0.50    2.00    --  107.46 125.00  90.00   50
 11  \w     39.00  72.00   0.50    2.00    --  107.46 -94.00  90.00   66
 12  \w     40.00 102.00   0.50    2.00    --  107.46 -30.00-150.00  124
 13  \w     97.00 132.00   0.50    2.00    --  107.46 125.00  90.00   70
 14  \w     55.00 111.00   0.50    2.00    --  107.46 -61.00  60.00  112
 15  \w    103.00 171.00   0.50    2.00    --  107.46  45.00 -90.00  136
;
_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      0.0422128000
_diffrn_orient_matrix_UB_12      0.0333150000
_diffrn_orient_matrix_UB_13      -0.0495505000
_diffrn_orient_matrix_UB_21      0.0422523000
_diffrn_orient_matrix_UB_22      0.0442456000
_diffrn_orient_matrix_UB_23      0.0414990000
_diffrn_orient_matrix_UB_31      0.0785324000
_diffrn_orient_matrix_UB_32      -0.0417817000
_diffrn_orient_matrix_UB_33      0.0043770000
_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  0.0570
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35343
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.067
_diffrn_reflns_theta_min         3.718
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.540
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             3552
_exptl_crystal_preparation       'As per the preparation scheme'
_exptl_crystal_recrystallization_method 'Slow vapour diffusion'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.941
_refine_diff_density_min         -1.999
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         8639
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0603
_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^)+(0.1090P)^2^+25.1356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8241
_reflns_number_total             8639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01692g2.cif
_cod_data_source_block           sjp-as-240
_cod_database_code               7713942
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H N O Ag  Si'
_chemical_oxdiff_usercomment     'COLOURLESS BLOCK'
_shelx_estimated_absorpt_t_max   0.327
_shelx_estimated_absorpt_t_min   0.262
_diffrn_oxdiff_ac3_digest_hkl    01144f4aacc4f98856600d383046dea2754417
_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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3.a Free rotating group:
 O4(H4a,H4b)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24),
  C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
3.c 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)
;
_shelx_res_checksum              54998
_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 3.203
_oxdiff_exptl_absorpt_empirical_full_min 0.626