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_7711340
_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         'C28 H36 Cl2 N O P Pd, C H2 Cl2'
_chemical_formula_sum            'C29 H38 Cl4 N O P Pd'
_chemical_formula_weight         695.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 103.717(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.6446(16)
_cell_length_b                   22.8590(14)
_cell_length_c                   11.6653(7)
_cell_measurement_reflns_used    9636
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      23.48
_cell_measurement_theta_min      2.33
_cell_volume                     6125.2(7)
_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      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.1058
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            138141
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         24.560
_diffrn_reflns_theta_min         1.566
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1378 before and 0.0697 after correction.
The Ratio of minimum to maximum transmission is 0.8416.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       prism
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.847
_refine_diff_density_min         -1.320
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         20727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0359P)^2^+3.3961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13545
_reflns_number_total             20727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01354a2.cif
_cod_data_source_block           cla0621a
_cod_database_code               7711340
_shelx_shelxl_version_number     2018/3
_audit_contact_author
;
        Celia M. Maya
        Departamento de Q\'imica Inorg\'anica
        Universidad de Sevilla
        Apdo 1203
        41071 SEVILLA
        Spain
;
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.892
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Cl5A)=Sof(Cl6A)=Sof(C57A)=Sof(H57C)=Sof(H57D)=1-FVAR(1)
 Sof(Cl5)=Sof(Cl6)=Sof(C57)=Sof(H57B)=Sof(H57A)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
3.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C53(H53A,
 H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C58(H58A,H58B),
 C57(H57B,H57A), C57A(H57C,H57D)
3.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), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38), C39(H39), C45(H45),
  C46(H46), C47(H47)
3.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C)
;
_shelx_res_checksum              69212
_shelx_hkl_checksum              33338
_olex2_submission_special_instructions 'No special instructions were received'