Group 11 metal complexes of a dinucleating triazole appended bisphosphine, 1,4-bis(5-(diisopropylphosphaneyl)-1-phenyl-1H-1,2,3-triazol-4-yl)benzene
Kote, Basvaraj S.; Kunchur, Harish S.; Radhakrishna, Latchupatula; Pandey, Madhusudan Kumar; Balakrishna, Maravanji Shivaramaiah; Dalton Transactions  (2021) –; doi:10.1039/D1DT02803K

data_7708658
_publ_section_title
;
 Group 11 metal complexes of a dinucleating triazole appended
 bisphosphine,
 1,4-bis(5-(diisopropylphosphaneyl)-1-phenyl-1H-1,2,3-triazol-4-yl)benzene
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02803K
_journal_year                    2021
_chemical_formula_moiety         'C34 H42 Au2 Cl2 N6 P2, C H2 Cl2'
_chemical_formula_sum            'C35 H44 Au2 Cl4 N6 P2'
_chemical_formula_weight         1146.43
_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             2021-10-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2021-10-26 deposited with the CCDC.	2021-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.888(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2017(2)
_cell_length_b                   32.7903(6)
_cell_length_c                   13.2599(3)
_cell_measurement_reflns_used    17616
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      23.2660
_cell_measurement_theta_min      1.6660
_cell_volume                     3952.82(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -108.63  15.87   0.50    3.00    --  -12.98 -59.25  20.08  249
  2  \w   -108.63  15.87   0.50    3.00    --  -12.98 -59.25 173.08  249
  3  \f    -30.17 153.33   0.50    3.00  77.88 -12.98  31.50    --   367
  4  \f   -116.21 115.79   0.50    3.00  16.12 -12.98 -59.25    --   464
  5  \w   -108.63  15.87   0.50    3.00    --  -12.98 -59.25  71.08  249
  6  \f   -126.01 105.99   0.50    3.00   9.41 -12.98 -31.50    --   464
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0043377000
_diffrn_orient_matrix_UB_12      -0.0195775000
_diffrn_orient_matrix_UB_13      0.0220659000
_diffrn_orient_matrix_UB_21      -0.0105744000
_diffrn_orient_matrix_UB_22      0.0091887000
_diffrn_orient_matrix_UB_23      0.0467284000
_diffrn_orient_matrix_UB_31      -0.0772166000
_diffrn_orient_matrix_UB_32      -0.0001627000
_diffrn_orient_matrix_UB_33      -0.0161048000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            119124
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         1.674
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.800
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.065
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.601
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         8615
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+17.5726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6734
_reflns_number_total             8615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02803k2.cif
_cod_data_source_block           Compound-10
_cod_database_code               7708658
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.631
_shelx_estimated_absorpt_t_min   0.544
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl3-C35 \\sim Cl3-C35A
 with sigma of 0.02
 Cl3-Cl4 \\sim Cl3-Cl4A
 with sigma of 0.04
 Cl4-C35 \\sim Cl4A-C35A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C35A) \\sim Ueq, Uanis(Cl4A) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(Cl4)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 Cl4A, C35A, C35, Cl4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: Cl4(0.92) C35(0.92) H35A(0.92) H35B(0.92) C35A(0.08) H35C(0.08)
 H35D(0.08) Cl4A(0.08)
6.a Ternary CH refined with riding coordinates:
 C6(H6), C23(H23), C26(H26), C9(H9)
6.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C35A(H35C,H35D)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C34(H34), C18(H18), C19(H19), C13(H13), C30(H30), C17(H17),
 C31(H31), C14(H14), C32(H32), C33(H33), C16(H16), C15(H15)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C25(H25A,H25B,H25C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C),
 C11(H11A,H11B,H11C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C)
;
_shelx_res_checksum              6684
_shelx_hkl_checksum              88850
_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 1.815
_oxdiff_exptl_absorpt_empirical_full_min 0.580