Isomerizing Methoxycarbonylation of Alkenes to Esters Using a Bis(phosphorinone)xylene Palladium Catalyst
Nobbs, James D.; Low, Choon Heng; Stubbs, Ludger P.; Wang, Cun; Drent, Eite; van Meurs, Martin; Organometallics 36 (2017) 391–; doi:10.1021/acs.organomet.6b00813

data_4086811
_publ_section_title
;
 Isomerizing Methoxycarbonylation of Alkenes to Esters Using a
 Bis(phosphorinone)xylene Palladium Catalyst
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              391
_journal_paper_doi               10.1021/acs.organomet.6b00813
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C31 H40 Cl3 D F6 O6 P2 Pd'
_chemical_formula_weight         899.33
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.14(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.475(2)
_cell_length_b                   16.524(3)
_cell_length_c                   19.999(4)
_cell_measurement_reflns_used    8897
_cell_measurement_temperature    140.1500
_cell_measurement_theta_max      31.1515
_cell_measurement_theta_min      1.6221
_cell_volume                     3660.4(13)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Saturn70 (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26150
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.62
_diffrn_standards_number         10964
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.4400
_exptl_crystal_size_mid          0.2200
_exptl_crystal_size_min          0.1800
_refine_diff_density_max         1.788
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         9037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+7.0685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                8592
_reflns_number_total             9037
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00813_si_002.cif
_cod_data_source_block           (BPX)Pd(TFA)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4086811--4086812.cif.
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4086811