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_7122108
_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         'C48 H62 O8 P4 Pd2'
_chemical_formula_sum            'C48 H62 O8 P4 Pd2'
_chemical_formula_weight         1103.65
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-13 deposited with the CCDC.
2018-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.230(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3653(2)
_cell_length_b                   35.4662(5)
_cell_length_c                   10.0227(2)
_cell_measurement_reflns_used    21320
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.1330
_cell_measurement_theta_min      3.3330
_cell_volume                     2968.86(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.18b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.18b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.18b (Rigaku OD, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6095
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.934
_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     35.00 115.00   0.50   20.00    --   15.99 178.00  60.00  160
  2  \w    -25.00 112.00   0.50   20.00    --   15.99  77.00  30.00  274
  3  \w    -26.00 104.00   0.50   20.00    --   15.99  38.00-120.00  260
  4  \w    -72.00  55.00   0.50   20.00    --   15.99 -57.00-180.00  254
  5  \w     35.00 115.00   0.50   20.00    --   15.99 178.00 120.00  160
  6  \w   -114.00 -57.00   0.50   20.00    --  -15.36-178.00 120.00  114
  7  \w    -20.00  34.00   0.50   20.00    --  -15.36 -99.00  60.00  108
  8  \w    -72.00  55.00   0.50   20.00    --   15.99 -57.00 -60.00  254
  9  \w    -25.00  23.00   0.50   20.00    --   15.99  80.00 -52.00   96
 10  \w    -80.00  57.00   0.50   20.00    --   15.99 -77.00 120.00  274
 11  \w    -23.00   2.00   0.50   20.00    --   15.99  57.00-180.00   50
;
_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      -0.0767670000
_diffrn_orient_matrix_UB_12      -0.0071139000
_diffrn_orient_matrix_UB_13      0.0131190000
_diffrn_orient_matrix_UB_21      0.0119433000
_diffrn_orient_matrix_UB_22      -0.0154143000
_diffrn_orient_matrix_UB_23      -0.0434273000
_diffrn_orient_matrix_UB_31      0.0342555000
_diffrn_orient_matrix_UB_32      -0.0105782000
_diffrn_orient_matrix_UB_33      0.0544676000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            55852
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.698
_diffrn_reflns_theta_min         3.264
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.18b (Rigaku Oxford Diffraction, 2015)
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    1.235
_exptl_crystal_description       prism
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 4166 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         12366
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.846
_reflns_number_gt                10286
_reflns_number_total             12366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc06283h2.cif
_cod_data_source_block           av74
_cod_depositor_comments
'Adding full bibliography for 7122108--7122115.cif.'
_cod_original_cell_volume        2968.87(10)
_cod_database_code               7122108
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'c48 h62 o8 p4 Pd2'
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.876
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Riding coordinates:
 O1(H1), O5(H5)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5A), C6(H6), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C23(H23), C24(H24), C25(H25), C27(H27), C30(H30), C31(H31),
  C32(H32), C33(H33), C34(H34), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44)
2.c 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), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C)
;
_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 1.583
_oxdiff_exptl_absorpt_empirical_full_min 0.633