LPdCl2(amine) Complexes Supported by Terphenyl Phosphanes: Applications in Aryl Amination Reactions
Santamaría, Nazaret; Velasco, Clara; Marín, Mario; Maya, Celia; Nicasio, M. Carmen; Dalton Transactions  (2022) –; doi:10.1039/D2DT01354A

data_7711338
_publ_section_title
;
 LPdCl2(amine) Complexes Supported by Terphenyl Phosphanes: Applications
 in Aryl Amination Reactions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01354A
_journal_year                    2022
_chemical_formula_moiety         'C41 H56 Cl2 N P Pd'
_chemical_formula_sum            'C41 H56 Cl2 N P Pd'
_chemical_formula_weight         771.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-03-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-29 deposited with the CCDC.	2022-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                97.274(2)
_cell_angle_beta                 97.470(2)
_cell_angle_gamma                102.579(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1723(5)
_cell_length_b                   11.6910(8)
_cell_length_c                   18.9911(13)
_cell_measurement_reflns_used    8225
_cell_measurement_temperature    173
_cell_measurement_theta_max      22.69
_cell_measurement_theta_min      2.53
_cell_volume                     1945.3(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35017
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         22.841
_diffrn_reflns_theta_min         1.545
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1134 before and 0.0529 after correction.
The Ratio of minimum to maximum transmission is 0.8706.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         10675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0266P)^2^+0.9529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8494
_reflns_number_total             10675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01354a2.cif
_cod_data_source_block           2a
_cod_database_code               7711338
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.869
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C12(H12), C22(H22), C24(H24),
 C26(H26), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
1.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              56345
_shelx_hkl_checksum              49748
_olex2_submission_special_instructions 'No special instructions were received'