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_7710745
_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 rm
_chemical_formula_moiety         'C60 H100 Au Cl N O28 P, C6 H6'
_chemical_formula_sum            'C66 H106 Au Cl N O28 P'
_chemical_formula_weight         1624.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-06-27 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.007(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.308(2)
_cell_length_b                   14.1787(8)
_cell_length_c                   15.4860(9)
_cell_measurement_reflns_used    9538
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      66.90
_cell_measurement_theta_min      4.35
_cell_volume                     8399.8(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            108770
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.321
_diffrn_reflns_theta_max         67.321
_diffrn_reflns_theta_min         2.310
_diffrn_source                   'Cu-ImuS Diamond microfocus tube'
_exptl_absorpt_coefficient_mu    4.367
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       prism
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_platon_squeeze_details
;
 The residual electron density was assigned to one molecule
 and a half of the benzene solvent [269/4 = 67 e per
 asymmetric unit; 1.5 molecule of C6H6 would give 63e].
;
_refine_diff_density_max         1.300
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 6564 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.171(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         14764
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0309P)^2^+31.8829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                14501
_reflns_number_total             14764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01553f2.cif
_cod_data_source_block           dayl190213
_cod_original_cell_volume        8399.7(8)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7710745
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.310
_shelx_estimated_absorpt_t_max   0.560
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              77496
_shelx_fab_checksum              96103