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_4341446
_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         'C27 H25 Ag N4 P, C F3 O3 S'
_chemical_formula_sum            'C28 H25 Ag F3 N4 O3 P S'
_chemical_formula_weight         693.42
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.8299(3)
_cell_length_b                   13.12475(11)
_cell_length_c                   22.6416(3)
_cell_measurement_reflns_used    14020
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.5440
_cell_measurement_theta_min      3.8650
_cell_volume                     6487.09(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    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0288846000
_diffrn_orient_matrix_UB_12      -0.1070284000
_diffrn_orient_matrix_UB_13      0.0019371000
_diffrn_orient_matrix_UB_21      -0.0637636000
_diffrn_orient_matrix_UB_22      0.0469785000
_diffrn_orient_matrix_UB_23      -0.0104405000
_diffrn_orient_matrix_UB_31      0.0090738000
_diffrn_orient_matrix_UB_32      -0.0103516000
_diffrn_orient_matrix_UB_33      -0.0672138000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33869
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.60
_diffrn_reflns_theta_min         3.90
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.497
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_correction_T_min  0.173
_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    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.647
_exptl_crystal_size_mid          0.0736
_exptl_crystal_size_min          0.0597
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         6431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0511P)^2^+1.8471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                5638
_reflns_number_total             6431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5019357_si_002.cif
_cod_data_source_block           3_AgoL
_cod_database_code               4341446
_chemical_oxdiff_formula         'Ag S O3 C F3 C27 P N4 H25 Me O H'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H13(0.07) H12(0.098) H11(0.082) H23(0.053) H22(0.07) H21(0.066)
 H7(0.037) H6(0.046) H5(0.053) H4(0.055) H3(0.046) H32(0.043) H33(0.045)
 H35(0.057) H36(0.048) H37a(0.083) H37b(0.083) H37c(0.083) H42(0.05) H43(0.054)
 H45(0.045) H46(0.04) H47a(0.075) H47b(0.075) H47c(0.075)
 Fixed X: H13(0.196) H12(0.2235) H11(0.271) H23(0.3203) H22(0.414) H21(0.3896)
 H7(0.2116) H6(0.0987) H5(0.048) H4(0.0736) H3(0.1522) H32(0.0706) H33(-0.0072)
 H35(0.0987) H36(0.1764) H37a(-0.0501) H37b(-0.0256) H37c(-0.0013) H42(0.229)
 H43(0.3089) H45(0.3742) H46(0.2952) H47a(0.3994) H47b(0.4413) H47c(0.4001)
 Fixed Y: H13(0.5422) H12(0.6906) H11(0.8209) H23(0.4208) H22(0.4666)
 H21(0.6285) H7(0.4952) H6(0.5445) H5(0.6966) H4(0.7856) H3(0.7281) H32(0.3387)
 H33(0.2701) H35(0.2952) H36(0.3687) H37a(0.2219) H37b(0.2843) H37c(0.1712)
 H42(0.5866) H43(0.6103) H45(0.3302) H46(0.3072) H47a(0.5571) H47b(0.4819)
 H47c(0.4377)
 Fixed Z: H13(0.0761) H12(0.0125) H11(0.0795) H23(0.1897) H22(0.2484)
 H21(0.3008) H7(0.1834) H6(0.359) H5(0.3364) H4(0.2513) H3(0.1906) H32(0.2864)
 H33(0.3436) H35(0.4888) H36(0.4326) H37a(0.4339) H37b(0.4899) H37c(0.4777)
 H42(0.3822) H43(0.4483) H45(0.4091) H46(0.3419) H47a(0.4958) H47b(0.4575)
 H47c(0.5101)
;