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_7713939
_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         'C63 H69 Cu1 P3 S3 Si3, B1 F4'
_chemical_formula_sum            'C63 H69 B Cu F4 P3 S3 Si3'
_chemical_formula_weight         1249.89
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_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                120
_cell_formula_units_Z            2
_cell_length_a                   15.64330(10)
_cell_length_b                   15.64330(10)
_cell_length_c                   16.00190(10)
_cell_measurement_reflns_used    14710
_cell_measurement_temperature    297.1(3)
_cell_measurement_theta_max      79.0100
_cell_measurement_theta_min      4.2660
_cell_volume                     3391.24(4)
_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      air
_diffrn_ambient_temperature      297.1(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.8556
_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   -101.00 -25.00   0.50    0.50    --  -38.50 -61.00  24.00  152
  2  \w    -40.00  23.00   0.50    0.50    --  -38.50  61.00 162.00  126
  3  \w     25.00  50.00   0.50    0.50    --   49.56 -61.00  24.00   50
  4  \w     74.00  99.00   0.50    0.50    --   49.56  61.00 162.00   50
  5  \w     48.00 113.00   0.50    1.00    --  111.00 -61.00  24.00  130
  6  \w    141.00 173.00   0.50    1.00    --  111.00  61.00 162.00   64
  7  \w    -16.00  53.00   0.50    0.50    --   49.56 -37.00  30.00  138
  8  \w     46.00 115.00   0.50    0.50    --   49.56  37.00 -90.00  138
  9  \w    139.00 172.00   0.50    1.00    --  111.00 111.00   0.00   66
 10  \w     45.00 113.00   0.50    1.00    --  111.00 -30.00-120.00  136
 11  \w    113.00 154.00   0.50    1.00    --  111.00  77.00 -90.00   82
 12  \w    104.00 177.00   0.50    1.00    --  111.00 111.00  30.00  146
 13  \w    142.00 176.00   0.50    1.00    --  111.00  45.00   0.00   68
 14  \w    108.00 137.00   0.50    1.00    --  111.00  45.00   0.00   58
 15  \w     48.00 109.00   0.50    1.00    --  111.00-111.00-150.00  122
 16  \w     44.00  93.00   0.50    1.00    --  111.00-111.00  60.00   98
 17  \w    104.00 136.00   0.50    1.00    --  111.00 111.00   0.00   64
 18  \w     43.00 102.00   0.50    1.00    --  111.00 -94.00-150.00  118
;
_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      0.1049265000
_diffrn_orient_matrix_UB_12      0.0146619000
_diffrn_orient_matrix_UB_13      -0.0037837000
_diffrn_orient_matrix_UB_21      0.0287781000
_diffrn_orient_matrix_UB_22      0.0814380000
_diffrn_orient_matrix_UB_23      -0.0661329000
_diffrn_orient_matrix_UB_31      0.0330372000
_diffrn_orient_matrix_UB_32      0.0779789000
_diffrn_orient_matrix_UB_33      0.0698501000
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18846
_diffrn_reflns_point_group_measured_fraction_full 0.884
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.287
_diffrn_reflns_theta_min         4.276
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.870
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29422
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow vapour diffusion'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.344
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.11(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         4234
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1416P)^2^+3.4947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2092
_refine_ls_wR_factor_ref         0.2097
_reflns_Friedel_coverage         0.722
_reflns_Friedel_fraction_full    0.767
_reflns_Friedel_fraction_max     0.723
_reflns_number_gt                4177
_reflns_number_total             4234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01692g2.cif
_cod_data_source_block           ska-ad-ak-144
_cod_original_cell_volume        3391.24(5)
_cod_database_code               7713939
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H Cu P S Si'
_chemical_oxdiff_usercomment     'colourless flacks'
_shelx_estimated_absorpt_t_max   0.571
_shelx_estimated_absorpt_t_min   0.522
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              85938
_shelx_fab_checksum              51650
_olex2_exptl_crystal_mounting_method 'Mounted on the nylon 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 2.202
_oxdiff_exptl_absorpt_empirical_full_min 0.573