Synthesis of chiral supramolecular bisphosphinite palladacycles through hydrogen transfer-promoted self-assembly process.
Vasseur, Alexandre; Membrat, Romain; Palpacelli, Davide; Giorgi, Michel; Nuel, Didier; Giordano, Laurent; Martinez, Alexandre; Chemical communications (Cambridge, England) 54 (2018) 10132–10135; doi:10.1039/c8cc06283h

data_7122113
_publ_section_title
;
 Synthesis of chiral supramolecular bisphosphinite palladacycles through
 hydrogen transfer-promoted self-assembly process.
;
_journal_issue                   72
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10132
_journal_page_last               10135
_journal_paper_doi               10.1039/c8cc06283h
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H34 O4 P2 Pd S'
_chemical_formula_sum            'C27 H34 O4 P2 Pd S'
_chemical_formula_weight         622.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-04-25 deposited with the CCDC.
2018-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.421(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9564(3)
_cell_length_b                   12.8239(5)
_cell_length_c                   11.6231(4)
_cell_measurement_reflns_used    15913
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.4890
_cell_measurement_theta_min      3.4980
_cell_volume                     1481.39(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -36.00  66.00   1.00   10.00    --   -7.63  57.00  90.00  102
  2  \w    -88.00  33.00   1.00   10.00    --   -7.63 -19.00 -90.00  121
  3  \w    -20.00  33.00   1.00   10.00    --   -7.63 -99.00-150.00   53
  4  \w    -20.00  49.00   1.00   10.00    --    8.25 -99.00 -90.00   69
  5  \w     -8.00  57.00   1.00   10.00    --    8.25-113.00 158.00   65
  6  \w    -16.00  83.00   1.00   10.00    --    8.25  38.00-120.00   99
  7  \w    -32.00  67.00   1.00   10.00    --   -7.63  38.00 -60.00   99
  8  \w    -20.00  33.00   1.00   10.00    --   -7.63 -99.00  30.00   53
  9  \w    -68.00  41.00   1.00   10.00    --    8.25 -77.00 -90.00  109
 10  \w    -20.00   5.00   1.00   10.00    --    8.25 -99.00   0.00   25
 11  \w    -20.00  49.00   1.00   10.00    --    8.25 -99.00  60.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0082413000
_diffrn_orient_matrix_UB_12      -0.0498460000
_diffrn_orient_matrix_UB_13      -0.0259318000
_diffrn_orient_matrix_UB_21      0.0478007000
_diffrn_orient_matrix_UB_22      -0.0210794000
_diffrn_orient_matrix_UB_23      0.0413159000
_diffrn_orient_matrix_UB_31      -0.0523642000
_diffrn_orient_matrix_UB_32      -0.0114307000
_diffrn_orient_matrix_UB_33      0.0368303000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34067
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.468
_diffrn_reflns_theta_min         3.062
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       prism
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 2353 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.037(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         6575
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0307P)^2^+0.2340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0673
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.819
_reflns_number_gt                5826
_reflns_number_total             6575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc06283h2.cif
_cod_data_source_block           av98
_cod_depositor_comments
'Adding full bibliography for 7122108--7122115.cif.'
_cod_original_cell_volume        1481.39(8)
_cod_database_code               7122113
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'c27 h34 o4 p2 Pd1 s1'
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.851
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(S2) = Uanis(C25)
Uanis(S1) = Uanis(C28)
3. Others
 Fixed Sof: S1(0.5) S2(0.5) C22(0.5) H22(0.5) C23(0.5) H23(0.5) C24(0.5)
 C25(0.5) H25(0.5) H26A(0.5) H26(0.5) H27(0.5) H27A(0.5) C28(0.5) H28(0.5)
 C29(0.5) C30(0.5) H30(0.5) C31(0.5) H31(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C22(H22), C23(H23), C25(H25), C26(H26A), C26(H26),
 C27(H27), C27(H27A), C28(H28), C30(H30), C31(H31)
4.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.269
_oxdiff_exptl_absorpt_empirical_full_min 0.799