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_7711339
_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         '2(C32 H39 Cl2 P Pd), C H2 Cl2'
_chemical_formula_sum            'C65 H80 Cl6 P2 Pd2'
_chemical_formula_weight         1348.73
_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     dual
_audit_creation_date             2022-03-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-15 deposited with the CCDC.	2022-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                95.311(3)
_cell_angle_beta                 98.986(3)
_cell_angle_gamma                98.963(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9169(8)
_cell_length_b                   15.0027(9)
_cell_length_c                   15.8900(10)
_cell_measurement_reflns_used    7366
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      21.79
_cell_measurement_theta_min      2.45
_cell_volume                     2982.7(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_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  0.0725
_diffrn_reflns_av_unetI/netI     0.0920
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            65774
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         23.679
_diffrn_reflns_theta_min         1.589
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1248 before and 0.0617 after correction.
The Ratio of minimum to maximum transmission is 0.8616.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       prism
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.093
_refine_diff_density_min         -1.259
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         18172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0557P)^2^+1.4602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11246
_reflns_number_total             18172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01354a2.cif
_cod_data_source_block           mmr1416a
_cod_database_code               7711339
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.893
_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. Shared sites
{C60A, C60B}
{C61A, C61B}
3. Uiso/Uaniso restraints and constraints
Uanis(C60A) = Uanis(C60B)
Uanis(C61A) = Uanis(C61B)
4. Others
 Sof(C60B)=Sof(H60B)=Sof(C61B)=Sof(H61C)=Sof(H61D)=Sof(C62B)=Sof(H62C)=
 Sof(H62D)=Sof(C63B)=Sof(H63C)=Sof(H63D)=Sof(C64B)=Sof(H64C)=Sof(H64D)=1-FVAR(1)
 Sof(C60A)=Sof(H60A)=Sof(C61A)=Sof(H61A)=Sof(H61B)=Sof(C62A)=Sof(H62A)=
 Sof(H62B)=Sof(C63A)=Sof(H63A)=Sof(H63B)=Sof(C64A)=Sof(H64A)=Sof(H64B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C23(H23), C28(H28), C55(H55), C60A(H60A), C60B(H60B)
5.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C56(H56A,H56B),
 C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C61A(H61A,H61B), C62A(H62A,
 H62B), C63A(H63A,H63B), C64A(H64A,H64B), C61B(H61C,H61D), C62B(H62C,H62D),
 C63B(H63C,H63D), C64B(H64C,H64D), C65(H65A,H65B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18),
 C19(H19), C35(H35), C36(H36), C37(H37), C41(H41), C42(H42), C43(H43), C49(H49),
  C50(H50), C51(H51)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C53(H53A,H53B,H53C), C54(H54A,
 H54B,H54C)
;
_shelx_res_checksum              6404
_shelx_hkl_checksum              26260
_olex2_submission_special_instructions 'No special instructions were received'