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_4341447
_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         'C46 H40 Ag F3 N4 O3 P2 S'
_chemical_formula_sum            'C46 H40 Ag F3 N4 O3 P2 S'
_chemical_formula_weight         955.69
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.3273(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.34515(15)
_cell_length_b                   13.8176(3)
_cell_length_c                   33.1325(6)
_cell_measurement_reflns_used    22446
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.0950
_cell_measurement_theta_min      3.1940
_cell_volume                     4278.25(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 (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0185785000
_diffrn_orient_matrix_UB_12      0.0337804000
_diffrn_orient_matrix_UB_13      -0.0152181000
_diffrn_orient_matrix_UB_21      0.0235798000
_diffrn_orient_matrix_UB_22      -0.0384536000
_diffrn_orient_matrix_UB_23      -0.0124860000
_diffrn_orient_matrix_UB_31      -0.0697179000
_diffrn_orient_matrix_UB_32      -0.0040238000
_diffrn_orient_matrix_UB_33      -0.0084030000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            48712
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.52
_diffrn_reflns_theta_min         2.85
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.904
_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    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.2567
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.0955
_refine_diff_density_max         1.238
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         10814
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0326P)^2^+6.1362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                9469
_reflns_number_total             10814
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5019357_si_002.cif
_cod_data_source_block           AgoLPPh3_4
_cod_original_cell_volume        4278.26(13)
_cod_database_code               4341447
_chemical_oxdiff_formula         'Ag C F3 S O3 P Ph3 C27 N7 P H25'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Shared sites
{N22a, N22}
{H7a, H7b}
2. Others
 Fixed Sof: H7a(0.5) H7b(0.5)
 Fixed Uiso: H3(0.032) H4(0.038) H5(0.036) H6(0.03) H7a(0.027) H7b(0.027)
 H11(0.038) H12(0.042) H13(0.035) H21(0.058) H21a(0.051) H22(0.051) H22a(0.058)
 H23(0.06) H23a(0.077) H32(0.034) H33(0.04) H35(0.035) H36(0.029) H37a(0.092)
 H37b(0.092) H37c(0.092) H42(0.035) H43(0.054) H45(0.04) H46(0.032) H47a(0.122)
 H47b(0.122) H47c(0.122) H52(0.042) H53(0.049) H54(0.04) H55(0.039) H56(0.033)
 H62(0.031) H63(0.039) H64(0.038) H65(0.037) H66(0.032) H72(0.034) H73(0.044)
 H74(0.048) H75(0.05) H76(0.038)
 Fixed X: H3(0.9369) H4(1.0095) H5(0.8418) H6(0.6007) H7a(0.5717) H7b(0.5717)
 H11(0.6843) H12(0.9047) H13(0.911) H21(0.7494) H21a(0.9157) H22(0.9809)
 H22a(0.6827) H23(0.9243) H23a(0.5375) H32(0.3587) H33(0.2464) H35(0.1627)
 H36(0.2848) H37a(0.1446) H37b(0.0136) H37c(0.1373) H42(0.2002) H43(0.1265)
 H45(0.482) H46(0.5559) H47a(0.2662) H47b(0.1516) H47c(0.307) H52(0.4822)
 H53(0.5568) H54(0.5503) H55(0.4671) H56(0.3941) H62(0.111) H63(-0.1323) H64(-
 0.2174) H65(-0.0588) H66(0.1844) H72(0.6089) H73(0.7284) H74(0.6424)
 H75(0.4354) H76(0.3131)
 Fixed Y: H3(0.2808) H4(0.4402) H5(0.5626) H6(0.5255) H7a(0.2008) H7b(0.2008)
 H11(0.1438) H12(0.0616) H13(0.0852) H21(0.0124) H21a(0.0628) H22(0.071) H22a(-
 0.0149) H23(0.1895) H23a(0.066) H32(0.5003) H33(0.6483) H35(0.6072)
 H36(0.4624) H37a(0.7784) H37b(0.7281) H37c(0.7714) H42(0.2345) H43(0.1678)
 H45(0.2628) H46(0.3328) H47a(0.1989) H47b(0.1394) H47c(0.0985) H52(0.4009)
 H53(0.3219) H54(0.1552) H55(0.0664) H56(0.144) H62(0.3255) H63(0.3412)
 H64(0.3796) H65(0.4075) H66(0.3921) H72(0.414) H73(0.5601) H74(0.6908)
 H75(0.6758) H76(0.5302)
 Fixed Z: H3(0.0809) H4(0.078) H5(0.0716) H6(0.0697) H7a(0.0797) H7b(0.0797)
 H11(0.2085) H12(0.1848) H13(0.1102) H21(-0.0267) H21a(-0.0171) H22(-0.002)
 H22a(-0.0203) H23(0.0521) H23a(0.0331) H32(0.1332) H33(0.1303) H35(0.0131)
 H36(0.0148) H37a(0.0922) H37b(0.0712) H37c(0.045) H42(0.0513) H43(-0.0087)
 H45(-0.0623) H46(-0.0024) H47a(-0.1029) H47b(-0.079) H47c(-0.084) H52(0.2857)
 H53(0.3438) H54(0.3472) H55(0.2929) H56(0.2345) H62(0.1606) H63(0.1713)
 H64(0.2345) H65(0.2869) H66(0.2771) H72(0.172) H73(0.1705) H74(0.2061)
 H75(0.2436) H76(0.2448)
;