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_4341444
_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         'C56 H50 Ag2 F6 N8 O6 P2 S2, C3 H6 O'
_chemical_formula_sum            'C59 H56 Ag2 F6 N8 O7 P2 S2'
_chemical_formula_weight         1444.92
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 99.9683(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.6768(3)
_cell_length_b                   11.79225(13)
_cell_length_c                   23.7381(3)
_cell_measurement_reflns_used    34071
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.3190
_cell_measurement_theta_min      3.2090
_cell_volume                     6251.99(14)
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9095
_diffrn_measurement_details
;
  1 omega   35.00   72.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -       11.3572  178.0000  -30.0000 37

  2 omega  -20.00   23.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -      -11.7478  -99.0000 -180.0000 43

  3 omega  -20.00    5.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -      -11.7478  -99.0000  -30.0000 25

  4 omega  -36.00   15.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -      -11.7478  -37.0000   90.0000 51

  5 omega  -15.00   16.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -      -11.7478  -77.0000   60.0000 31

  6 omega  -27.00   61.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -      -11.7478   37.0000  -30.0000 88

  7 omega  -87.00  -61.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -      -11.7478  -77.0000   60.0000 26

  8 omega   34.00  100.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -       11.3572 -178.0000 -180.0000 66

  9 omega  -93.00  -10.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -      -11.7478  -19.0000 -120.0000 83
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0312174000
_diffrn_orient_matrix_UB_12      0.0023958000
_diffrn_orient_matrix_UB_13      -0.0002511000
_diffrn_orient_matrix_UB_21      0.0054759000
_diffrn_orient_matrix_UB_22      -0.0333016000
_diffrn_orient_matrix_UB_23      0.0252519000
_diffrn_orient_matrix_UB_31      -0.0021819000
_diffrn_orient_matrix_UB_32      -0.0500304000
_diffrn_orient_matrix_UB_33      -0.0167991000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            72140
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         2.76
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.727
_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    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.6155
_exptl_crystal_size_mid          0.4246
_exptl_crystal_size_min          0.3425
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         15868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0276P)^2^+4.9138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                13712
_reflns_number_total             15868
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5019357_si_002.cif
_cod_data_source_block           1_p5acetone_AgpL
_cod_database_code               4341444
_chemical_oxdiff_formula         'Ag S F3 O3 C28 N4 P H25'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H11(0.03) H12(0.033) H2Sa(0.066) H2Sb(0.066) H2Sc(0.066)
 H13(0.029) H3Sa(0.061) H3Sb(0.061) H3Sc(0.061) H21(0.028) H22(0.031)
 H23(0.027) H7(0.022) H3(0.025) H5(0.023) H6(0.023) H2(0.025) H42(0.026)
 H43(0.029) H45(0.031) H46(0.028) H47a(0.047) H47b(0.047) H47c(0.047)
 H32(0.029) H33(0.031) H35(0.038) H36(0.032) H37a(0.056) H37b(0.056)
 H37c(0.056) H61(0.025) H62(0.026) H63(0.021) H71(0.026) H72(0.03) H73(0.025)
 H57(0.019) H55(0.023) H56(0.024) H52(0.025) H53(0.026) H82(0.034) H83(0.039)
 H85(0.028) H86(0.025) H87a(0.069) H87b(0.069) H87c(0.069) H92(0.03) H93(0.035)
 H95(0.037) H96(0.032) H97a(0.062) H97b(0.062) H97c(0.062)
 Fixed X: H11(0.4341) H12(0.387) H2Sa(-0.0136) H2Sb(-0.026) H2Sc(0.0408)
 H13(0.2767) H3Sa(-0.071) H3Sb(-0.0644) H3Sc(-0.0331) H21(0.2718) H22(0.1912)
 H23(0.1715) H7(0.2096) H3(0.2877) H5(0.1596) H6(0.1259) H2(0.2547) H42(0.0361)
 H43(-0.0553) H45(0.0135) H46(0.1051) H47a(-0.1051) H47b(-0.0836) H47c(-0.1181)
 H32(0.0853) H33(0.0733) H35(0.1914) H36(0.2021) H37a(0.1035) H37b(0.1581)
 H37c(0.0916) H61(0.2493) H62(0.3349) H63(0.4071) H71(0.2316) H72(0.3295)
 H73(0.41) H57(0.4123) H55(0.3182) H56(0.3179) H52(0.4056) H53(0.4067)
 H82(0.4523) H83(0.543) H85(0.5361) H86(0.4471) H87a(0.6011) H87b(0.6306)
 H87c(0.6317) H92(0.2478) H93(0.1728) H95(0.2887) H96(0.3638) H97a(0.1903)
 H97b(0.1559) H97c(0.1428)
 Fixed Y: H11(0.2831) H12(0.0922) H2Sa(0.8583) H2Sb(0.8916) H2Sc(0.8946)
 H13(0.1271) H3Sa(0.6922) H3Sb(0.6655) H3Sc(0.5847) H21(0.6658) H22(0.5646)
 H23(0.3835) H7(0.2963) H3(0.3146) H5(0.5063) H6(0.5647) H2(0.3743) H42(0.5786)
 H43(0.4886) H45(0.1988) H46(0.2889) H47a(0.2952) H47b(0.192) H47c(0.2974)
 H32(0.6491) H33(0.8434) H35(0.8976) H36(0.7029) H37a(1.0349) H37b(1.0564)
 H37c(1.042) H61(0.1517) H62(0.076) H63(0.2378) H71(0.6072) H72(0.6741)
 H73(0.5824) H57(0.4407) H55(0.6416) H56(0.7268) H52(0.4555) H53(0.3713)
 H82(0.7394) H83(0.8353) H85(0.863) H86(0.7604) H87a(1.0023) H87b(0.9008)
 H87c(0.8983) H92(0.6739) H93(0.8095) H95(1.0473) H96(0.9108) H97a(1.1057)
 H97b(1.0314) H97c(1.012)
 Fixed Z: H11(0.6312) H12(0.6379) H2Sa(0.5555) H2Sb(0.4892) H2Sc(0.5246)
 H13(0.6286) H3Sa(0.4592) H3Sb(0.5261) H3Sc(0.4859) H21(0.7105) H22(0.7513)
 H23(0.6957) H7(0.6119) H3(0.5129) H5(0.5653) H6(0.4716) H2(0.4186) H42(0.3801)
 H43(0.3769) H45(0.3255) H46(0.3265) H47a(0.3869) H47b(0.3515) H47c(0.3184)
 H32(0.2797) H33(0.2674) H35(0.412) H36(0.4262) H37a(0.2929) H37b(0.3442)
 H37c(0.3573) H61(0.3028) H62(0.2596) H63(0.2607) H71(0.1745) H72(0.1502)
 H73(0.2215) H57(0.3014) H55(0.3295) H56(0.4184) H52(0.4969) H53(0.4084)
 H82(0.4614) H83(0.4761) H85(0.6444) H86(0.6308) H87a(0.5711) H87b(0.541)
 H87c(0.6085) H92(0.5501) H93(0.5431) H95(0.5073) H96(0.5125) H97a(0.5125)
 H97b(0.553) H97c(0.4852)
;