Synthesis, structure and palladium coordination of ambiphilic, pyridine- and phosphine-tethered N-boryl imine ligands.
Lorenzini, Fabio; Lagueux-Tremblay, Pierre-Louis; Kayser, Laure V.; Anderson, Ethan; Arndtsen, Bruce A.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5766–5772; doi:10.1039/c8dt05100c

data_7049388
_publ_section_title
;
 Synthesis, structure and palladium coordination of ambiphilic, pyridine-
 and phosphine-tethered N-boryl imine ligands.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5766
_journal_page_last               5772
_journal_paper_doi               10.1039/c8dt05100c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C60 H76 B2 Cl2 N2 P2 Pd2, C H Cl3'
_chemical_formula_sum            'C61 H77 B2 Cl5 N2 P2 Pd2'
_chemical_formula_weight         1311.85
_chemical_name_systematic
bis[(allyl)chloro{?1-P-[N-(diphenylboryl)-2-di-tert-butyl-phosphanylbenzaldimine]}palladium]
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-sensitive
_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-2018/3
_audit_update_record
;
2019-03-16 deposited with the CCDC.    2019-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9999(15)
_cell_length_b                   13.3865(16)
_cell_length_c                   35.007(4)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.1709
_cell_measurement_theta_min      2.2600
_cell_volume                     6092.0(12)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'bruker APEX2'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics
'ShelXle (J. Appl. Cryst. 2011, 44, 1281-1284)'
_computing_publication_material
'ShelXle (J. Appl. Cryst. 2011, 44, 1281-1284)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            51457
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        23.237
_diffrn_reflns_theta_max         23.237
_diffrn_reflns_theta_min         1.629
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'triangular prism'
_exptl_crystal_F_000             2696
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform/diethyl ether'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.6668
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 3454 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         8723
_refine_ls_number_restraints     639
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0246P)^2^+3.0285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0565
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8197
_reflns_number_total             8723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05100c2.cif
_cod_data_source_block           Compound6b
_cod_depositor_comments
'Adding full bibliography for 7049383--7049388.cif.'
_cod_database_code               7049388
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.840
_shelx_estimated_absorpt_t_max   0.915
_shelx_res_checksum              58315