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_7045618
_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 H72 N2 P2 Pd2, 2(B F4)'
_chemical_formula_sum            'C52 H72 B2 F8 N2 P2 Pd2'
_chemical_formula_weight         1173.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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     dual
_audit_creation_date             2017-11-14
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-19 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.141(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2989(4)
_cell_length_b                   42.0772(15)
_cell_length_c                   14.9666(7)
_cell_measurement_reflns_used    5039
_cell_measurement_temperature    100
_cell_measurement_theta_max      59.005
_cell_measurement_theta_min      3.150
_cell_volume                     5822.4(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2016)'
_computing_data_collection       'APEX3 v2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      100.0
_diffrn_detector                 'Bruker Platinum135 CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Platinum135'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_av_unetI/netI     0.1175
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24734
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        59.034
_diffrn_reflns_theta_max         59.033
_diffrn_reflns_theta_min         2.100
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker FR-591'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.997
_exptl_absorpt_correction_T_max  0.5152
_exptl_absorpt_correction_T_min  0.3329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0960 before and 0.0693 after correction. The Ratio of minimum to maximum transmission is 0.6462. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       needle
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.877
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         8381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+5.6151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5793
_reflns_number_total             8381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00119g2.cif
_cod_data_source_block           spok79_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               7045618
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.412
_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:
 C17(H17), C23(H23), C47(H47), C41(H41)
2.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C22(H22A,H22B), C52(H52A,H52B), C18(H18A,H18B), C24(H24A,
 H24B), C21(H21A,H21B), C48(H48A,H48B), C46(H46A,H46B), C19(H19A,H19B),
 C51(H51A,H51B), C50(H50A,H50B), C42(H42A,H42B), C20(H20A,H20B), C45(H45A,H45B),
  C26(H26A,H26B), C25(H25A,H25B), C27(H27A,H27B), C49(H49A,H49B), C43(H43A,
 H43B), C44(H44A,H44B)
2.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C5(H5), C11(H11), C38(H38), C36(H36), C12(H12), C4(H4), C3(H3),
 C31(H31), C32(H32), C39(H39), C37(H37), C13(H13), C30(H30), C2(H2), C14(H14)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              93898
_shelx_fab_checksum              32589
_olex2_submission_special_instructions 'No special instructions were received'