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_7708659
_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         'C68 H84 Ag4 Br4 N12 P4, 3(C H2 Cl2)'
_chemical_formula_sum            'C71 H90 Ag4 Br4 Cl6 N12 P4'
_chemical_formula_weight         2199.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-07-20
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_audit_update_record
;
2021-10-12 deposited with the CCDC.	2021-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                83.651(3)
_cell_angle_beta                 74.880(3)
_cell_angle_gamma                70.200(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3674(4)
_cell_length_b                   17.7306(8)
_cell_length_c                   20.2898(6)
_cell_measurement_reflns_used    15968
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.9370
_cell_measurement_theta_min      1.7930
_cell_volume                     4366.7(3)
_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-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_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  \f    -10.27 349.73   1.00   10.00  77.88 -12.98  31.50    --   360
  2  \w    -69.79  -9.79   1.00   10.00    --  -13.03 107.85-157.07   60
  3  \w    -51.94  33.06   1.00   10.00    --  -13.03  75.18  70.14   85
  4  \w    -59.89   6.11   1.00   10.00    --  -13.03  89.79 -69.09   66
  5  \w   -108.63  15.37   1.00   10.00    --  -12.98 -59.25 -84.92  124
  6  \f   -349.73  10.27   1.00   10.00   9.41 -12.98 -31.50    --   360
  7  \w   -108.63  15.37   1.00   10.00    --  -12.98 -59.25 122.08  124
  8  \f   -339.92  20.08   1.00   10.00  16.12 -12.98 -59.25    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker D8 venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1353
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            168363
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.719
_exptl_absorpt_coefficient_mu    3.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45857
_exptl_absorpt_correction_type   numerical
_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    1.673
_exptl_crystal_description       needle
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.012
_refine_diff_density_max         4.827
_refine_diff_density_min         -1.424
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         15366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1193P)^2^+20.7385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2249
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10664
_reflns_number_total             15366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02803k2.cif
_cod_data_source_block           compound-7
_cod_database_code               7708659
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.708
_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.a Ternary CH refined with riding coordinates:
 C40(H40), C60(H60), C26(H26), C57(H57), C43(H43), C9(H9), C23(H23), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C30(H30), C68(H68), C17(H17), C14(H14), C47(H47), C64(H64),
 C51(H51), C16(H16), C15(H15), C53(H53), C67(H67), C19(H19), C1(H1), C2(H2),
 C31(H31), C34(H34), C66(H66), C48(H48), C35(H35), C36(H36), C65(H65), C32(H32),
  C18(H18), C52(H52), C50(H50), C49(H49), C33(H33)
2.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C11(H11A,H11B,H11C), C42(H42A,H42B,
 H42C), C41(H41A,H41B,H41C), C62(H62A,H62B,H62C), C8(H8A,H8B,H8C), C61(H61A,
 H61B,H61C), C10(H10A,H10B,H10C), C24(H24A,H24B,H24C), C58(H58A,H58B,H58C),
 C45(H45A,H45B,H45C), C25(H25A,H25B,H25C), C7(H7A,H7B,H7C), C44(H44A,H44B,H44C),
  C59(H59A,H59B,H59C)
;
_shelx_res_checksum              12121
_shelx_hkl_checksum              87440
_shelx_fab_checksum              83248
_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
;