A rational pre-catalyst design for bis-phosphine mono-oxide palladium catalyzed reactions
Ji, Yining; Li, Hongming; Hyde, Alan M.; Chen, Qinghao; Belyk, Kevin M.; Lexa, Katrina W.; Yin, Jingjun; Sherer, Edward C.; Williamson, R. Thomas; Brunskill, Andrew; Ren, Sumei; Campeau, Louis-Charles; Davies, Ian W.; Ruck, Rebecca T.; Chem. Sci. 8 (2017) 2841–; doi:10.1039/C6SC05472B

data_1545094
_publ_section_title
;
 A rational pre-catalyst design for bis-phosphine mono-oxide palladium
 catalyzed reactions
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2841
_journal_paper_doi               10.1039/C6SC05472B
_journal_volume                  8
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C39 H42 Br Cl2 N3 O2 P2 Pd, C7 H8'
_chemical_formula_sum            'C46 H50 Br Cl2 N3 O2 P2 Pd'
_chemical_formula_weight         996.04
_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_method           SHELXL-2014/7
_audit_update_record
;
2016-10-28 deposited with the CCDC.
2017-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7416(3)
_cell_length_b                   15.3629(4)
_cell_length_c                   22.5851(6)
_cell_measurement_reflns_used    9681
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.20
_cell_measurement_theta_min      3.48
_cell_volume                     4420.99(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28240
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.195
_diffrn_reflns_theta_max         67.195
_diffrn_reflns_theta_min         3.479
_diffrn_source                   'sealed-tube microsource X-ray generator'
_exptl_absorpt_coefficient_mu    6.563
_exptl_absorpt_correction_T_max  0.7691
_exptl_absorpt_correction_T_min  0.5841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
(SADABS; Sheldrick, 2003) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       Cut
_exptl_crystal_F_000             2032
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
; 
 Flack x determined using 3296 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.021(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         7828
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+1.7694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0511
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                7638
_reflns_number_total             7828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc05472b2.cif
_cod_data_source_block           mdk052
_cod_depositor_comments
;Adding full bibliography for 1545094--1545096.cif.

The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               1545094
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.354
_shelx_estimated_absorpt_t_max   0.779
_shelx_res_checksum              32508