Construction of a monoanionic S,N,S-pincer ligand with a pyrrole core by sequential [1,2] phospho-Fries rearrangement. Characterization of palladium and silver coordination complexes.
Fraix, Aurore; Lutz, Martin; Spek, Anthony L.; Klein Gebbink, Robertus J. M.; van Koten, Gerard; Salaün, Jean-Yves; Jaffrès, Paul-Alain; Dalton transactions (Cambridge, England : 2003) 39 (2010) 2942–2946; doi:10.1039/b923351b

data_7024959
_publ_section_title
;
 Construction of a monoanionic S,N,S-pincer ligand with a pyrrole core by
 sequential [1,2] phospho-Fries rearrangement. Characterization of
 palladium and silver coordination complexes.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2942
_journal_page_last               2946
_journal_paper_doi               10.1039/b923351b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C48 H88 Ag4 N4 O16 P8 S8'
_chemical_formula_sum            'C48 H88 Ag4 N4 O16 P8 S8'
_chemical_formula_weight         1912.94
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.720(2)
_cell_angle_beta                 81.848(2)
_cell_angle_gamma                72.571(2)
_cell_formula_units_Z            1
_cell_length_a                   11.1886(4)
_cell_length_b                   12.7764(6)
_cell_length_c                   14.3823(7)
_cell_measurement_reflns_used    156
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.98
_cell_measurement_theta_min      3.29
_cell_volume                     1916.05(15)
_computing_cell_refinement       Dirax
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44314
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    1.450
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            brownish
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8800
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+1.2576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0568
_reflns_number_gt                7284
_reflns_number_total             8800
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b923351b.txt
_cod_data_source_block           s3395a
_cod_original_cell_volume        1916.05(14)
_cod_database_code               7024959