Mechanistic insights into the tropo-inversion of the biphenyl moiety in chiral bis-amido phosphites and in their palladium(ii) complexes.
Passera, Alessandro; Iuliano, Anna; Pérez-Torrente, Jesús J; Passarelli, Vincenzo; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2292–2305; doi:10.1039/c7dt04829g

data_7045263
_publ_section_title
;
 Mechanistic insights into the tropo-inversion of the biphenyl moiety in
 chiral bis-amido phosphites and in their palladium(ii) complexes.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2292
_journal_page_last               2305
_journal_paper_doi               10.1039/c7dt04829g
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C48 H66 Cl4 N4 O2 P2 Pd2, C7 H8'
_chemical_formula_sum            'C55 H74 Cl4 N4 O2 P2 Pd2'
_chemical_formula_weight         1239.72
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-12-21 deposited with the CCDC.
2018-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                82.1650(10)
_cell_angle_beta                 74.8310(10)
_cell_angle_gamma                66.0270(10)
_cell_formula_units_Z            1
_cell_length_a                   10.2297(7)
_cell_length_b                   10.7327(7)
_cell_length_c                   14.5425(10)
_cell_measurement_reflns_used    9210
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.044
_cell_measurement_theta_min      2.238
_cell_volume                     1407.28(16)
_computing_cell_refinement       'SAINT+ in APEX2 (Bruker AXS,2008)'
_computing_data_collection       'SMART in APEX2 (Bruker AXS,2008)'
_computing_data_reduction        'SAINT+ in APEX2 (Bruker AXS,2008)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21566
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.549
_diffrn_reflns_theta_min         2.078
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  0.8496
_exptl_absorpt_correction_T_min  0.7556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Multi-scan correction included in APEX2 package (Bruker AXS, 2008)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       prism
_exptl_crystal_F_000             638
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 5171 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         12500
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0113P)^2^+1.7897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.826
_reflns_number_gt                11814
_reflns_number_total             12500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04829g2.cif
_cod_data_source_block           compound_MP_1a_VPX102_AP
_cod_depositor_comments          'Adding full bibliography for 7045263.cif.'
_cod_database_code               7045263
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              82555