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_7713943
_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         'C26 H21 Cl N4 O'
_chemical_formula_sum            'C26 H21 Cl N4 O'
_chemical_formula_weight         440.92
_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   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                 99.623(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7468(4)
_cell_length_b                   5.53310(10)
_cell_length_c                   33.9191(15)
_cell_measurement_reflns_used    10435
_cell_measurement_temperature    100.05
_cell_measurement_theta_max      77.6820
_cell_measurement_theta_min      3.8220
_cell_volume                     2173.59(13)
_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      100.05
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9870
_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    -95.00 -13.00   0.50    1.50    --  -38.50 137.00   4.00  164
  2  \w    -92.00  -9.00   0.50    1.50    --  -38.50 132.00-172.00  166
  3  \w     34.00 107.00   0.50    1.50    --   49.06-137.00 -59.00  146
  4  \w     91.00 171.00   0.50    2.40    --  107.46 137.00   4.00  160
  5  \w     45.00 118.00   0.50    2.40    --  107.46-132.00 118.00  146
  6  \w     94.00 170.00   0.50    2.40    --  107.46 132.00-172.00  152
  7  \w     45.00 121.00   0.50    2.40    --  107.46-137.00 -59.00  152
  8  \w   -102.00 -21.00   0.50    1.50    --  -38.50 -70.00 119.34  162
  9  \w    -42.00  28.00   0.50    1.50    --  -38.50  37.00  60.00  140
 10  \w    -42.00  28.00   0.50    1.50    --  -38.50  37.00 -90.00  140
 11  \w   -108.00 -33.00   0.50    1.50    --  -38.50 -19.00 120.00  150
 12  \w    -42.00  28.00   0.50    1.50    --  -38.50  37.00 -30.00  140
 13  \w     30.00 104.00   0.50    1.50    --   49.06-132.00 118.00  148
 14  \w     38.00 112.00   0.50    1.50    --   49.06  57.00 -90.00  148
 15  \w     45.00 121.00   0.50    2.40    --  107.46 -61.00-150.00  152
 16  \w     45.00 121.00   0.50    2.40    --  107.46 -61.00  60.00  152
 17  \w     39.00 111.00   0.50    2.40    --  107.46 -30.00  90.00  144
 18  \w     45.00 113.00   0.50    2.40    --  107.46-125.00   0.00  136
 19  \w     39.00 107.00   0.50    2.40    --  107.46 -94.00 150.00  136
 20  \w    103.00 172.00   0.50    2.40    --  107.46  45.00  90.00  138
 21  \w     39.00 107.00   0.50    2.40    --  107.46 -94.00-120.00  136
 22  \w     39.00 116.00   0.50    2.40    --  107.46 -15.00 120.00  154
 23  \w     96.00 170.00   0.50    2.40    --  107.46  58.00-155.34  148
 24  \w     89.00 171.00   0.50    2.40    --  107.46  71.00-112.27  164
 25  \w     43.00 131.00   0.50    2.40    --  107.46 -77.00 120.00  176
 26  \w    105.00 162.00   0.50    2.40    --  107.46  30.00 150.00  114
 27  \w     57.00 108.00   0.50    2.40    --  107.46-109.00   5.71  102
 28  \w    102.00 160.00   0.50    2.40    --  107.46 125.00-120.00  116
 29  \w     68.00 107.00   0.50    2.40    --  107.46 -94.00  90.00   78
 30  \w     48.00 112.00   0.50    2.40    --  107.46 -45.00-180.00  128
 31  \w    128.00 172.00   0.50    2.40    --  107.46  77.00 150.00   88
 32  \w     53.00  82.00   0.50    2.40    --  107.46-125.00-150.00   58
 33  \w    102.00 165.00   0.50    2.40    --  107.46  54.00 108.21  126
 34  \w     66.00 107.00   0.50    2.40    --  107.46 -94.00  30.00   82
 35  \w     47.00 104.00   0.50    2.40    --  107.46-125.00  90.00  114
 36  \w     39.00 108.00   0.50    2.40    --  107.46 -30.00 -60.00  138
 37  \w     62.00 110.00   0.50    2.40    --  107.46 -45.00 -90.00   96
 38  \w    146.00 172.00   0.50    2.40    --  107.46  45.00 116.89   52
;
_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      -0.0735930000
_diffrn_orient_matrix_UB_12      -0.0632363000
_diffrn_orient_matrix_UB_13      -0.0407140000
_diffrn_orient_matrix_UB_21      -0.0927254000
_diffrn_orient_matrix_UB_22      -0.1114773000
_diffrn_orient_matrix_UB_23      0.0215935000
_diffrn_orient_matrix_UB_31      -0.0606340000
_diffrn_orient_matrix_UB_32      0.2471156000
_diffrn_orient_matrix_UB_33      -0.0006252000
_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  0.0837
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            33818
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.457
_diffrn_reflns_theta_min         3.817
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39130
_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    1.347
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_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          0.2
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0857
_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^)+(0.1126P)^2^+4.4903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2315
_refine_ls_wR_factor_ref         0.2372
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4029
_reflns_number_total             4594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01692g2.cif
_cod_data_source_block           sjp-cat-cu-55
_cod_database_code               7713943
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H N O Cl'
_chemical_oxdiff_usercomment     'COLOURLESS PLATES'
_shelx_estimated_absorpt_t_max   0.754
_shelx_estimated_absorpt_t_min   0.657
_diffrn_oxdiff_ac3_digest_hkl    019b0dfa1f677533ebc4cc2feee1bf2712a5c3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C10(H10a,H10b), C13(H13a,H13b), C14(H14a,H14b)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C16(H16), C17(H17), C18(H18),
 C19(H19), C23(H23), C24(H24), C25(H25), C26(H26)
;
_shelx_res_checksum              91199
_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 1.695
_oxdiff_exptl_absorpt_empirical_full_min 0.603