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_7708662
_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
'C38 H48 Ag2 N6 O4 P2, 0.662(C1 H1 Cl3), 2.338(C1 H2 Cl2)'
_chemical_formula_sum            'C41 H53.338 Ag2 Cl6.662 N6 O4 P2'
_chemical_formula_weight         1208.056
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2021-10-24
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.10.14 svn.r9718050b for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-10-26 deposited with the CCDC.	2021-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                67.733(2)
_cell_angle_beta                 85.412(2)
_cell_angle_gamma                75.516(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6903(3)
_cell_length_b                   13.7105(3)
_cell_length_c                   16.3337(4)
_cell_measurement_reflns_used    17631
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.3970
_cell_measurement_theta_min      1.7640
_cell_volume                     2546.05(11)
_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-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9996
_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    5.00  77.88 -12.98  31.50    --   360
  2  \w    -67.90  -7.91   1.00    5.00    --  -13.03 104.46-153.44   60
  3  \w    -52.82  30.18   1.00    5.00    --  -13.03  76.79  78.78   83
  4  \w    -58.70  19.30   1.00    5.00    --  -13.03  87.54 -54.33   78
  5  \w   -108.63  15.37   1.00    5.00    --  -12.98 -59.25 122.08  124
  6  \f   -349.73  10.27   1.00    5.00   9.41 -12.98 -31.50    --   360
  7  \w   -108.63  15.37   1.00    5.00    --  -12.98 -59.25 -84.92  124
  8  \f   -339.92  20.08   1.00    5.00  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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1213
_diffrn_reflns_av_unetI/netI     0.1121
_diffrn_reflns_Laue_measured_fraction_full 0.9996
_diffrn_reflns_Laue_measured_fraction_max 0.9996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            142218
_diffrn_reflns_point_group_measured_fraction_full 0.9996
_diffrn_reflns_point_group_measured_fraction_max 0.9996
_diffrn_reflns_theta_full        24.9996
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67296
_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    1.576
_exptl_crystal_description       needle
_exptl_crystal_F_000             1220.385
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.1928
_refine_diff_density_min         -0.8650
_refine_diff_density_rms         0.1143
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             9.9685
_refine_ls_goodness_of_fit_ref   1.0461
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    90
_refine_ls_number_parameters     607
_refine_ls_number_reflns         8975
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.0432
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          -0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+3.8447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1223
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -14
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                7298
_reflns_number_total             8975
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1dt02803k2.cif
_cod_data_source_block           Compound-9
_cod_database_code               7708662
_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
 Cl1-C39 \\sim Cl1A-C39A
 with sigma of 0.02
 Cl2-H39a \\sim Cl2A-H39c
 with sigma of 0.04
 Cl2-C39 \\sim Cl2A-C39A
 with sigma of 0.02
 Cl2-H39b \\sim Cl2A-H39d
 with sigma of 0.04
 C39-H39a \\sim C39A-H39c
 with sigma of 0.02
 C39-H39b \\sim C39A-H39d
 with sigma of 0.02
 H39a-H39b \\sim H39c-H39d
 with sigma of 0.04
 Cl1-Cl2 \\sim Cl1A-Cl2A
 with sigma of 0.04
 Cl1-H39a \\sim Cl1A-H39c
 with sigma of 0.04
 Cl1-H39b \\sim Cl1A-H39d
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C41 \\sim C41A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(Cl6A) \\sim Ueq, Uanis(C41A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C41A, Cl6A, Cl7A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C41A)=Sof(H41a)=Sof(H41b)=Sof(Cl6A)=Sof(Cl7A)=1-FVAR(1)
 Sof(Cl6)=Sof(Cl5)=Sof(C41)=Sof(H41)=Sof(Cl7)=FVAR(1)
 Sof(Cl1A)=Sof(C39A)=Sof(H39c)=Sof(H39d)=Sof(Cl2A)=1-FVAR(2)
 Sof(Cl1)=Sof(Cl2)=Sof(C39)=Sof(H39a)=Sof(H39b)=FVAR(2)
 Fixed Uiso: Cl1A(0.14) C39A(0.14) H39c(0.14) H39d(0.14) Cl2A(0.14)
6.a Ternary CH refined with riding coordinates:
 C26(H26), C9(H9), C7(H7), C23(H23), C41(H41)
6.b Secondary CH2 refined with riding coordinates:
 C39(H39a,H39b), C40(H40a,H40b), C41A(H41a,H41b), C39A(H39c,H39d)
6.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C30(H30), C1(H1), C2(H2), C19(H19), C13(H13), C14(H14),
 C31(H31), C15(H15), C16(H16), C34(H34), C32(H32), C33(H33)
6.d Idealised Me refined as rotating group:
 C28(H28a,H28b,H28c), C6(H6a,H6b,H6c), C8(H8a,H8b,H8c), C10(H10a,H10b,H10c),
 C24(H24a,H24b,H24c), C11(H11a,H11b,H11c), C27(H27a,H27b,H27c), C25(H25a,H25b,
 H25c), C38(H38a,H38b,H38c), C36(H36a,H36b,H36c)
;
_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
;