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_4341445
_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         'C54 H50 Ag2 N8 P2, 2(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C60 H56 Ag2 F6 N10 O6 P2 S2'
_chemical_formula_weight         1468.95
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90.00
_cell_angle_beta                 109.318(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.8539(2)
_cell_length_b                   15.5905(3)
_cell_length_c                   17.6390(4)
_cell_measurement_reflns_used    14148
_cell_measurement_temperature    100.05(10)
_cell_measurement_theta_max      29.1650
_cell_measurement_theta_min      3.5880
_cell_volume                     3076.29(11)
_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      100.05(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.9983
_diffrn_measured_fraction_theta_max 0.8987
_diffrn_measurement_details
;
  1 omega  -67.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3572  -77.0000 -180.0000 111

  2 omega   36.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3572  178.0000   30.0000 25

  3 omega  -11.00   38.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3572  -37.0000 -150.0000 49

  4 omega   28.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7478   57.0000 -150.0000 27

  5 omega  -32.00   -6.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7478   57.0000 -150.0000 26

  6 omega    1.00   27.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7478  -99.0000 -120.0000 26

  7 omega  -18.00   45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3572   57.0000 -120.0000 63

  8 omega   35.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3572  178.0000  120.0000 66
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0233212000
_diffrn_orient_matrix_UB_12      0.0382706000
_diffrn_orient_matrix_UB_13      0.0211286000
_diffrn_orient_matrix_UB_21      -0.0322989000
_diffrn_orient_matrix_UB_22      0.0245226000
_diffrn_orient_matrix_UB_23      -0.0341753000
_diffrn_orient_matrix_UB_31      -0.0493094000
_diffrn_orient_matrix_UB_32      0.0020240000
_diffrn_orient_matrix_UB_33      0.0142302000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31390
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.49
_diffrn_reflns_theta_min         2.77
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.911
_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    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.1497
_exptl_crystal_size_mid          0.1098
_exptl_crystal_size_min          0.0902
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         7707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+2.6929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                6415
_reflns_number_total             7707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5019357_si_002.cif
_cod_data_source_block           2_CH3CN_AgmL
_cod_original_cell_volume        3076.30(11)
_cod_database_code               4341445
_chemical_oxdiff_formula         'Ag C27 H25 N4 P C2 H3 N S O3 C F3'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H11(0.026) H12(0.029) H13(0.026) H21(0.03) H22(0.037) H23(0.032)
 H7(0.021) H2(0.02) H6(0.023) H5(0.026) H4(0.025) H42(0.026) H43(0.028)
 H45(0.029) H46(0.024) H47a(0.054) H47b(0.054) H47c(0.054) H32(0.027)
 H33(0.029) H35(0.028) H36(0.025) H37a(0.05) H37b(0.05) H37c(0.05) H2sa(0.07)
 H2sb(0.07) H2sc(0.07)
 Fixed X: H11(0.5141) H12(0.6968) H13(0.708) H21(0.1501) H22(0.2195)
 H23(0.4424) H7(0.5957) H2(0.6617) H6(0.6525) H5(0.5485) H4(0.4952) H42(0.6106)
 H43(0.6208) H45(0.9322) H46(0.9211) H47a(0.7042) H47b(0.8252) H47c(0.8305)
 H32(0.9404) H33(1.1296) H35(1.0835) H36(0.8958) H37a(1.2951) H37b(1.2337)
 H37c(1.2834) H2sa(0.8287) H2sb(0.9625) H2sc(0.9077)
 Fixed Y: H11(0.2213) H12(0.1801) H13(0.283) H21(0.4517) H22(0.4569)
 H23(0.433) H7(0.4159) H2(0.4234) H6(0.679) H5(0.7008) H4(0.5837) H42(0.4033)
 H43(0.2548) H45(0.2542) H46(0.4022) H47a(0.1191) H47b(0.1181) H47c(0.1287)
 H32(0.5874) H33(0.6461) H35(0.635) H36(0.5739) H37a(0.6551) H37b(0.7474)
 H37c(0.6994) H2sa(0.5042) H2sb(0.5388) H2sc(0.474)
 Fixed Z: H11(0.5747) H12(0.6895) H13(0.8014) H21(0.6893) H22(0.8399)
 H23(0.8851) H7(0.8153) H2(0.6559) H6(0.6115) H5(0.7018) H4(0.7658) H42(0.4552)
 H43(0.446) H45(0.6313) H46(0.6432) H47a(0.5081) H47b(0.5834) H47c(0.4945)
 H32(0.5032) H33(0.5633) H35(0.78) H36(0.7205) H37a(0.7583) H37b(0.7369)
 H37c(0.6742) H2sa(0.8432) H2sb(0.8825) H2sc(0.9315)
;