Buchwald-Hartwig amination using Pd(i) dimer precatalysts supported by biaryl phosphine ligands.
Kirlikovali, Kent O.; Cho, Eunho; Downard, Tyler J.; Grigoryan, Lilit; Han, Zheng; Hong, Sooji; Jung, Dahee; Quintana, Jason C.; Reynoso, Vanessa; Ro, Sooihk; Shen, Yi; Swartz, Kevin; Ter Sahakyan, Elizabeth; Wixtrom, Alex I.; Yoshida, Brandon; Rheingold, Arnold L.; Spokoyny, Alexander M.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3684–3688; doi:10.1039/c8dt00119g

data_7045617
_publ_section_title
;
 Buchwald-Hartwig amination using Pd(i) dimer precatalysts supported by
 biaryl phosphine ligands.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3684
_journal_page_last               3688
_journal_paper_doi               10.1039/c8dt00119g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C52 H70 O4 P2 Pd2, 2(B F4)'
_chemical_formula_sum            'C52 H70 B2 F8 O4 P2 Pd2'
_chemical_formula_weight         1207.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.22 svn.r3403 for OlexSys, GUI svn.r5332)
;
_audit_update_record
;
2017-12-19 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.142(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9242(6)
_cell_length_b                   15.4346(4)
_cell_length_c                   19.9878(7)
_cell_measurement_reflns_used    6339
_cell_measurement_temperature    180
_cell_measurement_theta_max      27.666
_cell_measurement_theta_min      2.474
_cell_volume                     5904.4(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22573
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.329
_diffrn_reflns_theta_min         1.695
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0723 before and 0.0420 after correction. The Ratio of minimum to maximum transmission is 0.9211. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         7260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+22.7471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5864
_reflns_number_total             7260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00119g2.cif
_cod_data_source_block           spok63_0m_a_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7045616--7045618.cif.
;
_cod_database_code               7045617
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.833
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C5(H5A,H5B), C12(H12A,H12B), C2(H2A,H2B), C4(H4A,H4B), C3(H3A,
 H3B), C9(H9A,H9B), C8(H8A,H8B), C11(H11A,H11B), C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C22(H22), C15(H15), C23(H23), C24(H24), C16(H16), C17(H17)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              35123
_shelx_fab_checksum              95297
_olex2_submission_special_instructions 'No special instructions were received'