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_1545096
_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         'C25 H32 Br N3 O P2 Pd'
_chemical_formula_sum            'C25 H32 Br N3 O P2 Pd'
_chemical_formula_weight         638.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 95.3448(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4340(11)
_cell_length_b                   10.7208(5)
_cell_length_c                   10.6091(5)
_cell_measurement_reflns_used    9798
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.55
_cell_measurement_theta_min      3.79
_cell_volume                     2653.7(2)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            23472
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.577
_diffrn_reflns_theta_max         66.577
_diffrn_reflns_theta_min         3.789
_diffrn_source                   'sealed-tube microsource X-ray generator'
_exptl_absorpt_coefficient_mu    8.720
_exptl_absorpt_correction_T_max  0.418
_exptl_absorpt_correction_T_min  0.289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
(SADABS; Sheldrick, 2003) 
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1288
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
; 
 Flack x determined using 2111 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.016(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         4648
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0229
_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^)+(0.0292P)^2^+4.0320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0566
_reflns_Friedel_coverage         0.891
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                4584
_reflns_number_total             4648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc05472b2.cif
_cod_data_source_block           mdk105
_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               1545096
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.180
_shelx_estimated_absorpt_t_max   0.476
_shelx_res_checksum              61914