Nitrogen-Based Chirality Effects in Novel Mixed Phosphorus/Nitrogen Ligands Applied to Palladium-Catalyzed Allylic Substitutions
Schnitzler, Verena; Nonglaton, Guillaume; Roussière, Hélène; Maillet, Céline; Evain, Michel; Janvier, Pascal; Bujoli, Bruno; Petit, Marc; Organometallics 27 (2008) 5997–; doi:10.1021/om800498a

data_4071977
_publ_section_title
;
 Nitrogen-Based Chirality Effects in Novel Mixed Phosphorus/Nitrogen
 Ligands Applied to Palladium-Catalyzed Allylic Substitutions
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5997
_journal_paper_doi               10.1021/om800498a
_journal_volume                  27
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H26 Br2 N2 P S, C4 H2 O6, 3(H2 O)'
_chemical_formula_sum            'C32 H38 Br2 N2 O9 P S'
_chemical_formula_weight         818.5
_chemical_name_systematic        ' ?'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0672(3)
_cell_length_b                   11.0184(13)
_cell_length_c                   46.319(5)
_cell_measurement_temperature    293
_cell_volume                     3606.8(6)
_computing_publication_material  '(Jana2000; Petricek and Dusek, 2000)'
_computing_structure_refinement  '(Jana2000; Petricek and Dusek, 2000)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            24037
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         5.01
_exptl_absorpt_coefficient_mu    2.402
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(Jana2000; Petricek and Dusek, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.5068(2)
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.01
_refine_diff_density_min         -0.66
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.29
_refine_ls_goodness_of_fit_ref   1.17
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8056
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.001936I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1047
_reflns_number_gt                5213
_reflns_number_total             8056
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800498a_si_003.cif
_cod_data_source_block           (I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_formula_sum        'C32 H38 Br2 N2 O9 P1 S1'
_cod_database_code               4071977