A cavity-shaped <i>cis</i>-chelating P,N ligand for highly selective nickel-catalysed ethylene dimerisation.
Li, Yang; Pelzer, Katrin; Sechet, Damien; Creste, Geordie; Matt, Dominique; Braunstein, Pierre; Armspach, Dominique; Dalton transactions (Cambridge, England : 2003)  (2022) –; doi:10.1039/d2dt01553f

data_7710741
_publ_section_title
;
 A cavity-shaped <i>cis</i>-chelating P,N ligand for highly selective
 nickel-catalysed ethylene dimerisation.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt01553f
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C60 H100 Cl2 N O28 P Pd, C4 H8 O'
_chemical_formula_sum            'C64 H108 Cl2 N O29 P Pd'
_chemical_formula_weight         1563.78
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2022-03-31 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.0630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.9237(6)
_cell_length_b                   17.5343(7)
_cell_length_c                   15.7250(6)
_cell_measurement_reflns_used    6394
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.48
_cell_measurement_theta_min      2.67
_cell_volume                     4038.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0849
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39896
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.021
_diffrn_reflns_theta_min         1.723
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       prism
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
The residual electron density was assigned to one molecule of
the butanone solvent [57/2= 29 e per asymmetric unit; one molecule of C4H8O1 would give 40 e]. 
;
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 4721 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.002(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         18579
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0437P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    0.939
_reflns_Friedel_fraction_max     0.898
_reflns_number_gt                13244
_reflns_number_total             18579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01553f2.cif
_cod_data_source_block           dmda150706
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7710741
_shelx_estimated_absorpt_t_min   0.909
_shelx_estimated_absorpt_t_max   0.962
_shelxl_version_number           2013-4
_shelx_res_checksum              5903