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_7710746
_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 rmad
_chemical_formula_moiety         '2(C60 H100 Br2 N Ni O28 P), 5(C6 H6), C5 H12'
_chemical_formula_sum            'C155 H242 Br4 N2 Ni2 O56 P2'
_chemical_formula_weight         3528.49
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-07-27
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2022-03-31 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8671(6)
_cell_length_b                   17.8671(6)
_cell_length_c                   53.805(2)
_cell_measurement_reflns_used    9398
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.87
_cell_measurement_theta_min      2.21
_cell_volume                     17176.3(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       '\f and \w shuterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            277051
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.896
_diffrn_reflns_theta_min         1.895
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       prism
_exptl_crystal_F_000             7440
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 5953 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         20499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0693P)^2^+18.4409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1474
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                15880
_reflns_number_total             20499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01553f2.cif
_cod_data_source_block           dayl201124
_cod_original_cell_volume        17176.2(14)
_cod_database_code               7710746
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.705
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C57) = Uanis(C57B)
Uanis(C68) = Uanis(C69) = Uanis(C70) = Uanis(C71) = Uanis(C72) = Uanis(C73)
Uanis(C74) = Uanis(C75) = Uanis(C76) = Uanis(C77) = Uanis(C78) = Uanis(C79)
Uanis(C80) = Uanis(C81) = Uanis(C82) = Uanis(C83) = Uanis(C84) = Uanis(C85)
Uanis(C86) = Uanis(C87) = Uanis(C88) = Uanis(C89) = Uanis(C90)
2. Others
 Fixed Sof: C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C57B(0.5) H57D(0.5)
 H57E(0.5) H57F(0.5) C80(0.5) H80(0.5) C81(0.5) H81(0.5) C82(0.5) H82(0.5)
 C83(0.5) H83(0.5) C84(0.5) H84(0.5) C85(0.5) H85(0.5) C86(0.5) H86A(0.5)
 H86B(0.5) H86C(0.5) C87(0.5) H87A(0.5) H87B(0.5) C88(0.5) H88A(0.5) H88B(0.5)
 C89(0.5) H89A(0.5) H89B(0.5) C90(0.5) H90A(0.5) H90B(0.5) H90C(0.5)
3.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C31(H31),
  C32(H32), C33(H33), C34(H34), C35(H35), C41(H41), C42(H42), C43(H43),
 C44(H44), C45(H45), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C16(H16A,H16B), C26(H26A,H26B), C36(H36A,H36B), C46(H46A,H46B),
 C56(H56A,H56B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B)
3.c Aromatic/amide H refined with riding coordinates:
 C61(H61), C62(H62), C63(H63), C64(H64), C68(H68), C69(H69), C70(H70),
 C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78),
  C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85)
3.d Fitted hexagon refined as free rotating group:
 C68(C69,C70,C71,C72,C73), C74(C75,C76,C77,C78,C79), C80(C81,C82,C83,C84,C85)
3.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C), C57(H57A,H57B,H57C), C57B(H57D,H57E,H57F),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C66(H66A,H66B,H66C), C67(H67A,H67B,
 H67C), C86(H86A,H86B,H86C), C90(H90A,H90B,H90C)
;
_shelx_res_checksum              97624
_olex2_submission_special_instructions 'No special instructions were received'