Synthesis, characterization and Pd(ii)-coordination chemistry of the ligand tris(quinolin-8-yl)phosphite. Application in the catalytic aerobic oxidation of amines.
Rodríguez-Lugo, R E; Chacón-Terán, M A; De León, S; Vogt, M.; Rosenthal, A. J.; Landaeta, V. R.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2061–2072; doi:10.1039/c7dt04000h

data_7045159
_publ_section_title
;
 Synthesis, characterization and Pd(ii)-coordination chemistry of the
 ligand tris(quinolin-8-yl)phosphite. Application in the catalytic aerobic
 oxidation of amines.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2061
_journal_page_last               2072
_journal_paper_doi               10.1039/c7dt04000h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C27 H18 Cl2 N3 O3 P Pd, C H2 Cl2'
_chemical_formula_sum            'C28 H20 Cl4 N3 O3 P Pd'
_chemical_formula_weight         725.64
_chemical_name_common            '[Pd(P(Oquin)3}Cl2]'
_chemical_name_systematic        '[Pd(P(Oquin)3}Cl2]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-01-06
_audit_creation_method
;
Olex2 1.2
(compiled Dec 12 2016 15:38:10 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2017-05-03 deposited with the CCDC.
2017-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.511(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7868(11)
_cell_length_b                   23.313(2)
_cell_length_c                   10.9533(11)
_cell_measurement_reflns_used    5784
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.55
_cell_volume                     2751.8(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0922
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28444
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.367
_diffrn_reflns_theta_min         1.747
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'BRUKER APEX'
_exptl_absorpt_coefficient_mu    1.159
_exptl_absorpt_correction_T_max  0.8363
_exptl_absorpt_correction_T_min  0.6804
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Sheldrick, 2015)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1448
_exptl_crystal_recrystallization_method 'slow diffusion dichloromethane'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.332
_refine_diff_density_min         -1.653
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0452P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5961
_reflns_number_total             6876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04000h2.cif
_cod_data_source_block           p21n
_cod_depositor_comments
;

2018-02-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 7045158--7045159.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_moiety     '4(C27 H18 Cl2 N3 O3 P Pd), 4(C H2 Cl2)'
_cod_original_formula_sum        'C112 H80 Cl16 N12 O12 P4 Pd4'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     2902.56
_cod_database_code               7045159
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.836
_shelx_estimated_absorpt_t_min   0.680
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
;
_shelx_res_checksum              40800
_olex2_submission_special_instructions 'No special instructions were received'