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_7711337
_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         'C37 H44 Cl2 N P Pd, C H2 Cl2'
_chemical_formula_sum            'C38 H46 Cl4 N P Pd'
_chemical_formula_weight         795.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-03-13
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.2644(6)
_cell_length_b                   18.3812(6)
_cell_length_c                   25.6270(9)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      21.98
_cell_measurement_theta_min      2.28
_cell_volume                     7190.4(4)
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0569
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            64427
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         22.000
_diffrn_reflns_theta_min         1.505
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.6243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1275 before and 0.0438 after correction.
The Ratio of minimum to maximum transmission is 0.8383.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       prism
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         8977
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0243P)^2^+9.8579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7208
_reflns_number_total             8977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01354a2.cif
_cod_data_source_block           cla0221a
_cod_database_code               7711337
_shelx_shelxl_version_number     2018/3
_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. Restrained distances
 C38A-Cl3A = C38A-Cl4A
 1.7 with sigma of 0.01
 C38B-Cl3B = C38B-Cl4B
 1.7 with sigma of 0.01
3. Others
 Sof(C38B)=Sof(H38C)=Sof(H38D)=Sof(Cl3B)=Sof(Cl4B)=1-FVAR(1)
 Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(Cl3A)=Sof(Cl4A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C23(H23), C28(H28)
4.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), C38A(H38A,H38B),
 C38B(H38C,H38D)
4.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), C33(H33), C34(H34), C36(H36), C35(H35), C37(H37)
4.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              71929
_shelx_hkl_checksum              12325
_olex2_submission_special_instructions 'No special instructions were received'