Isomer Dependence in the Assembly and Lability of Silver(I) Trifluoromethanesulfonate Complexes of the Heteroditopic Ligands, 2-, 3-, and 4-[Di(1H-pyrazolyl)methyl]phenyl(di-p-tolyl)phosphine
Gardinier, James R.; Hewage, Jeewantha S.; Lindeman, Sergey V.; Inorganic Chemistry  (2014) 141106150122003–; doi:10.1021/ic5019357

data_4341448
_publ_section_title
;
 Isomer Dependence in the Assembly and Lability of Silver(I)
 Trifluoromethanesulfonate Complexes of the Heteroditopic Ligands, 2-, 3-,
 and 4-[Di(1H-pyrazolyl)methyl]phenyl(di-p-tolyl)phosphine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              141106150122003
_journal_paper_doi               10.1021/ic5019357
_journal_year                    2014
_chemical_formula_moiety         'C26 H22 Ag I2 N8, C F3 O3 S'
_chemical_formula_sum            'C27 H22 Ag F3 I2 N8 O3 S'
_chemical_formula_weight         957.26
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                70.706(2)
_cell_angle_beta                 86.720(2)
_cell_angle_gamma                85.857(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4676(3)
_cell_length_b                   11.6230(3)
_cell_length_c                   15.5967(4)
_cell_measurement_reflns_used    15970
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.7950
_cell_measurement_theta_min      3.4460
_cell_volume                     1614.65(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9013
_diffrn_measurement_details
;
  1 omega   13.00   53.00   1.0000    1.4500
omega____ theta____ kappa____ phi______ frames
    -       11.3624  -99.0000   30.0000 40

  2 omega  -87.00    6.00   1.0000    1.4500
omega____ theta____ kappa____ phi______ frames
    -      -11.7530  -37.0000   60.0000 93

  3 omega  -24.00   69.00   1.0000    1.4500
omega____ theta____ kappa____ phi______ frames
    -      -11.7530   19.0000  -30.0000 93

  4 omega  -91.00    9.00   1.0000    1.4500
omega____ theta____ kappa____ phi______ frames
    -      -11.7530  -19.0000  150.0000 100

  5 omega  -18.00   30.00   1.0000    1.4500
omega____ theta____ kappa____ phi______ frames
    -      -11.7530  -99.0000 -150.0000 48

  6 omega  -38.00   64.00   1.0000    1.4500
omega____ theta____ kappa____ phi______ frames
    -      -11.7530   37.0000  150.0000 102

  7 omega  -20.00   30.00   1.0000    1.4500
omega____ theta____ kappa____ phi______ frames
    -      -11.7530  -99.0000    0.0000 50

  8 omega -100.00  -55.00   1.0000    1.4500
omega____ theta____ kappa____ phi______ frames
    -      -11.7530  178.0000 -150.0000 45

  9 omega  -93.00   34.00   1.0000    1.4500
omega____ theta____ kappa____ phi______ frames
    -      -11.7530  -19.0000  150.0000 127

 10 omega  -89.00  -49.00   1.0000    1.4500
omega____ theta____ kappa____ phi______ frames
    -      -11.7530  154.0000 -175.5724 40

 11 omega  -38.00   64.00   1.0000    1.4500
omega____ theta____ kappa____ phi______ frames
    -      -11.7530   37.0000 -150.0000 102
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0221022000
_diffrn_orient_matrix_UB_12      -0.0215356000
_diffrn_orient_matrix_UB_13      0.0455512000
_diffrn_orient_matrix_UB_21      0.0641184000
_diffrn_orient_matrix_UB_22      0.0300060000
_diffrn_orient_matrix_UB_23      -0.0140883000
_diffrn_orient_matrix_UB_31      -0.0323992000
_diffrn_orient_matrix_UB_32      0.0531958000
_diffrn_orient_matrix_UB_33      0.0071548000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36367
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.52
_diffrn_reflns_theta_min         2.78
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.661
_exptl_absorpt_correction_T_max  0.723
_exptl_absorpt_correction_T_min  0.523
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.2423
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.484
_refine_diff_density_min         -1.527
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+2.4455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                6725
_reflns_number_total             8114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5019357_si_002.cif
_cod_data_source_block           Ag_bispz2CHC6H4I_II
_cod_database_code               4341448
_chemical_oxdiff_formula         'Ag C26 H22 N8 I2 S O3 C F3'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H11(0.032) H12(0.032) H13(0.025) H21(0.034) H22(0.04) H23(0.031)
 H7(0.02) H4(0.023) H5(0.026) H6(0.024) H2(0.021) H41(0.027) H42(0.031)
 H43(0.028) H51(0.023) H52(0.026) H53(0.023) H37(0.02) H34(0.026) H35(0.032)
 H36(0.029) H32(0.022)
 Fixed X: H11(0.1683) H12(-0.0364) H13(0.0579) H21(0.5369) H22(0.4394)
 H23(0.3186) H7(0.2963) H4(0.6197) H5(0.8117) H6(0.7869) H2(0.3737) H41(0.6496)
 H42(0.8418) H43(0.9317) H51(0.3458) H52(0.4853) H53(0.7396) H37(0.8711)
 H34(0.7379) H35(0.7753) H36(0.8614) H32(0.871)
 Fixed Y: H11(-0.0529) H12(0.1008) H13(0.3052) H21(0.178) H22(0.3911)
 H23(0.4629) H7(0.3798) H4(0.3349) H5(0.3592) H6(0.3338) H2(0.2624) H41(0.0394)
 H42(-0.1116) H43(-0.2201) H51(-0.2521) H52(-0.4537) H53(-0.4053) H37(-0.2109)
 H34(-0.1604) H35(-0.02) H36(0.171) H32(0.0796)
 Fixed Z: H11(0.3515) H12(0.3406) H13(0.255) H21(-0.0191) H22(-0.0979)
 H23(0.0244) H7(0.193) H4(0.1468) H5(0.2251) H6(0.3803) H2(0.3777) H41(0.4269)
 H42(0.5067) H43(0.3976) H51(0.2355) H52(0.285) H53(0.2836) H37(0.2402)
 H34(0.0716) H35(-0.0726) H36(-0.0898) H32(0.1847)
;