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_7713940
_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 Cl2 Cu2 P2 Si2'
_chemical_formula_sum            'C42 H46 Cl2 Cu2 P2 Si2'
_chemical_formula_weight         866.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-23
_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                 115.546(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3025(2)
_cell_length_b                   16.1615(2)
_cell_length_c                   17.2690(3)
_cell_measurement_reflns_used    27714
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      77.7480
_cell_measurement_theta_min      3.9360
_cell_volume                     4105.11(12)
_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      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9734
_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    -80.00   7.00   0.50    0.20    --  -38.50 109.00 -22.00  174
  2  \w     14.00  91.00   0.50    0.20    --   49.56-109.00-118.00  154
  3  \w     38.00 108.00   0.50    0.30    --  107.46-109.00-118.00  140
  4  \w    103.00 177.00   0.50    0.30    --  107.46 109.00 -22.00  148
  5  \w    -42.00  28.00   0.50    0.20    --  -38.50  37.00-120.00  140
  6  \w   -105.00 -35.00   0.50    0.20    --  -38.50 -37.00 -90.00  140
  7  \w     38.00 113.00   0.50    0.20    --   49.56  57.00  60.00  150
  8  \w     46.00 116.00   0.50    0.20    --   49.56  37.00-150.00  140
  9  \w     97.00 172.00   0.50    0.30    --  107.46 125.00 -60.00  150
 10  \w     39.00 107.00   0.50    0.30    --  107.46 -94.00 -90.00  136
 11  \w     39.00 111.00   0.50    0.30    --  107.46 -30.00-180.00  144
 12  \w    111.00 157.00   0.50    0.30    --  107.46  45.00 120.00   92
 13  \w    113.00 172.00   0.50    0.30    --  107.46  45.00 150.00  118
 14  \w     46.00  72.00   0.50    0.30    --  107.46-125.00  60.00   52
 15  \w     49.00 103.00   0.50    0.30    --  107.46 -94.00 -60.00  108
 16  \w     43.00  81.00   0.50    0.30    --  107.46 -77.00 -60.00   76
 17  \w     83.00 126.00   0.50    0.30    --  107.46 -77.00 -60.00   86
 18  \w     51.00 112.00   0.50    0.30    --  107.46 -45.00  60.00  122
 19  \w    100.00 156.00   0.50    0.30    --  107.46 125.00-180.00  112
 20  \w    131.00 156.00   0.50    0.30    --  107.46  77.00-180.00   50
 21  \w     43.00  98.00   0.50    0.30    --  107.46 -45.00  30.00  110
;
_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      -0.0600527000
_diffrn_orient_matrix_UB_12      -0.0292867000
_diffrn_orient_matrix_UB_13      0.0432842000
_diffrn_orient_matrix_UB_21      0.0012850000
_diffrn_orient_matrix_UB_22      0.0880470000
_diffrn_orient_matrix_UB_23      0.0346307000
_diffrn_orient_matrix_UB_31      -0.0858085000
_diffrn_orient_matrix_UB_32      0.0217609000
_diffrn_orient_matrix_UB_33      -0.0819342000
_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  0.0375
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33570
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.055
_diffrn_reflns_theta_min         3.941
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.988
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59058
_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            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         8580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0432P)^2^+2.8021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8135
_reflns_number_total             8580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01692g2.cif
_cod_data_source_block           ska-ad-ak-111_auto
_cod_database_code               7713940
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H P Cl Cu Si'
_chemical_oxdiff_usercomment     'colourless block'
_shelx_estimated_absorpt_t_max   0.488
_shelx_estimated_absorpt_t_min   0.381
_diffrn_oxdiff_digest_frames
;
01c0c9d650dcb10e99cd660a77a112fb900254265ec
;
_diffrn_oxdiff_digest_hkl
;
01ec757db3f4b99f712189ab9e5ec6eb2619e2
;
_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:
 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), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36)
2.b Idealised Me refined as rotating group:
 C37(H37a,H37b,H37c), C38(H38a,H38b,H38c), C39(H39a,H39b,H39c), C40(H40a,H40b,
 H40c), C41(H41a,H41b,H41c), C42(H42a,H42b,H42c)
;
_shelx_res_checksum              10893
_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 1.565
_oxdiff_exptl_absorpt_empirical_full_min 0.697