Palladium-catalyzed N-(2-pyridyl)sulfonyl-directed C(sp3)‒H γ-arylation of amino acid derivatives
Rodríguez, Nuria; Romero-Revilla, Jose A.; Fernández-Ibáñez, M. Ángeles; Carretero, Juan C.; Chemical Science 4 (2013) 175–; doi:10.1039/c2sc21162a

data_1514849
_publ_section_title
;
 Palladium-catalyzed N-(2-pyridyl)sulfonyl-directed C(sp3)--H \g-arylation
 of amino acid derivatives
;
_journal_issue                   1
_journal_name_full               'Chemical Science'
_journal_page_first              175
_journal_paper_doi               10.1039/c2sc21162a
_journal_volume                  4
_journal_year                    2013
_chemical_absolute_configuration rm
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H32 N4 O8 Pd2 S2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C24.5 H33 Cl N4 O8 Pd2 S2'
_chemical_formula_weight         823.94
_chemical_name_systematic
;
?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-12-28T10:56:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.4525(4)
_cell_length_b                   15.4860(10)
_cell_length_c                   46.1840(30)
_cell_measurement_reflns_used    12430
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.9
_cell_measurement_theta_min      2.2
_cell_measurement_wavelength     0.71073
_cell_volume                     6045.3(6)
_computing_cell_refinement       'APPEX2 (BRUKER AXS, 2005)'
_computing_data_collection       'APPEX2 (BRUKER AXS, 2005)'
_computing_data_reduction        'APPEX2 (BRUKER AXS, 2005)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al, 2004)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1004
_diffrn_reflns_av_unetI/netI     0.1228
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            45187
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         0.88
_exptl_absorpt_coefficient_mu    1.469
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3304
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.163
_refine_diff_density_min         -1.495
_refine_diff_density_rms         0.212
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         12387
_refine_ls_number_restraints     732
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0713
_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^)+(0.0465P)^2^+60.6519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1588
_reflns_number_gt                9188
_reflns_number_total             12387
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2sc21162a.txt
_cod_data_source_block           jd01afi
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_radiation_monochromador' tag replaced with
'_diffrn_radiation_monochromator'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

2019-08-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C49 H66 Cl2 N8 O16 Pd4 S4'
_cod_original_formula_weight         1647.88
_cod_original_formula_moiety         '2(C24 H32 N4 O8 Pd2 S2), C H2 Cl2'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        6045.2(6)
_cod_database_code               1514849