Oxidative Addition of Secondary C‒X Bonds to Palladium(0): A Beneficial Anomeric Acceleration
Munro-Leighton, Colleen; Adduci, Laura L.; Becker, Jennifer J.; Gagné, Michel R.; Organometallics 30 (2011) 2646–; doi:10.1021/om200221r

data_4089366
_publ_section_title
;
 Oxidative Addition of Secondary C--X Bonds to Palladium(0): A Beneficial
 Anomeric Acceleration
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2646
_journal_paper_doi               10.1021/om200221r
_journal_volume                  30
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H49 Br1 O9 P2 Pd1'
_chemical_formula_sum            'C26 H49 Br O9 P2 Pd'
_chemical_formula_weight         753.92
_chemical_melting_point          ?;
_chemical_name_systematic        Pd(PEt3)2(Br)(aceto-glucopyranose)
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 96.4120(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4902(2)
_cell_length_b                   28.3899(4)
_cell_length_c                   11.5768(2)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100
_cell_measurement_theta_max      70
_cell_measurement_theta_min      4
_cell_volume                     3426.19(10)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24530
_diffrn_reflns_theta_full        70.050
_diffrn_reflns_theta_max         70.052
_diffrn_reflns_theta_min         3.113
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.989
_exptl_absorpt_correction_T_max  0.26
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.288
_exptl_crystal_size_min          0.193
_refine_diff_density_max         1.61
_refine_diff_density_min         -0.90
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.009(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9384
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         11099
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.0092277
_refine_ls_shift/su_mean         0.0207740
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.00P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0559
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0559
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              29
_reflns_limit_k_min              -33
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                10646
_reflns_number_total             11140
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.54
_oxford_diffrn_Wilson_scale      101.70
_oxford_refine_ls_r_factor_ref   0.0265
_oxford_refine_ls_scale          0.099594(14)
_oxford_reflns_number_all        11099
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'x1006014 in P2(1)'
_cod_data_source_file            om200221r_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3426.19(9)
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C26 H49 Br1 O9 P2 Pd1'
_cod_database_code               4089366