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_7713937
_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         'C21 H23 P Si'
_chemical_formula_sum            'C21 H23 P Si'
_chemical_formula_weight         334.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-21
_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                90
_cell_angle_beta                 95.628(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.05060(10)
_cell_length_b                   24.7054(4)
_cell_length_c                   19.7244(3)
_cell_measurement_reflns_used    15537
_cell_measurement_temperature    288(3)
_cell_measurement_theta_max      77.2250
_cell_measurement_theta_min      3.5640
_cell_volume                     3904.14(10)
_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      288(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9727
_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    -65.00  28.00   0.50    1.00    --  -38.50  83.00-123.00  186
  2  \w    -12.00  76.00   0.50    1.00    --   49.56 -83.00 115.00  176
  3  \w    100.00 174.00   0.50    2.00    --  107.46  83.00-123.00  148
  4  \w     41.00 134.00   0.50    2.00    --  107.46 -83.00 115.00  186
  5  \w    -42.00  28.00   0.50    1.00    --  -38.50  37.00 -30.00  140
  6  \w    -42.00  28.00   0.50    1.00    --  -38.50  37.00-120.00  140
  7  \w     38.00 113.00   0.50    1.00    --   49.56  57.00 -30.00  150
  8  \w     46.00 116.00   0.50    1.00    --   49.56  37.00 -60.00  140
  9  \w     43.00 112.00   0.50    2.00    --  107.46 -45.00 -60.00  138
 10  \w     43.00 112.00   0.50    2.00    --  107.46 -45.00-150.00  138
 11  \w    104.00 176.00   0.50    2.00    --  107.46  30.00-180.00  144
 12  \w     43.00 113.00   0.50    2.00    --  107.46-125.00 120.00  140
 13  \w     39.00 107.00   0.50    2.00    --  107.46 -94.00 -90.00  136
 14  \w     98.00 150.00   0.50    2.00    --  107.46 125.00 -60.00  104
 15  \w     44.00  89.00   0.50    2.00    --  107.46-125.00  60.00   90
 16  \w    122.00 169.00   0.50    2.00    --  107.46  77.00  30.00   94
 17  \w     52.00 103.00   0.50    2.00    --  107.46 -94.00  60.00  102
 18  \w     54.00 112.00   0.50    2.00    --  107.46 -15.00 120.00  116
 19  \w    105.00 149.00   0.50    2.00    --  107.46 125.00-180.00   88
;
_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      -0.0240390000
_diffrn_orient_matrix_UB_12      -0.0546525000
_diffrn_orient_matrix_UB_13      0.0353786000
_diffrn_orient_matrix_UB_21      -0.1871526000
_diffrn_orient_matrix_UB_22      0.0011103000
_diffrn_orient_matrix_UB_23      -0.0253518000
_diffrn_orient_matrix_UB_31      0.0369313000
_diffrn_orient_matrix_UB_32      -0.0300037000
_diffrn_orient_matrix_UB_33      -0.0653199000
_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  0.0366
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31560
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.937
_diffrn_reflns_theta_min         3.578
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84034
_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    1.138
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow vapour diffuion'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.716
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         8060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0806
_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^)+(0.1641P)^2^+0.7723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2217
_refine_ls_wR_factor_ref         0.2325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6709
_reflns_number_total             8060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01692g2.cif
_cod_data_source_block           ska-ad-ak-181_auto
_cod_database_code               7713937
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H P Si'
_chemical_oxdiff_usercomment     'white block'
_shelx_estimated_absorpt_t_max   0.653
_shelx_estimated_absorpt_t_min   0.598
_diffrn_oxdiff_digest_frames
;
014850074dd31907f54cfbd409e1f40419000287c2a
;
_diffrn_oxdiff_digest_hkl
;
01b9ba6f6793ac3ed972bf297072f97188b988
;
_reflns_odcompleteness_completeness 99.92
_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), 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)
;
_shelx_res_checksum              49496
_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 1.258
_oxdiff_exptl_absorpt_empirical_full_min 0.792