A tetranuclear lanthanum-nickel hydrido complex supported by an arene-anchored bis(phosphinomethylamido) ligand.
He, Xiuyan; Wu, Changjiang; Hong, Dongjing; Fang, Huayi; Cui, Peng; Chemical communications (Cambridge, England) 62 (2026) 3807–3810; doi:10.1039/d5cc06726j

data_7135358
_publ_section_title
;
 A tetranuclear lanthanum-nickel hydrido complex supported by an
 arene-anchored bis(phosphinomethylamido) ligand.
;
_journal_issue                   12
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3807
_journal_page_last               3810
_journal_paper_doi               10.1039/d5cc06726j
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C64 H90 La2 N4 Ni2 P4, 2(C7 H8)'
_chemical_formula_sum            'C78 H106 La2 N4 Ni2 P4'
_chemical_formula_weight         1618.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-10-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-09-03 deposited with the CCDC.	2026-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.0530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8479(5)
_cell_length_b                   20.5016(7)
_cell_length_c                   14.9962(6)
_cell_measurement_reflns_used    6483
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      27.442
_cell_measurement_theta_min      2.469
_cell_volume                     3661.0(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            123124
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         2.044
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.782
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1490 before and 0.0803 after correction.
The Ratio of minimum to maximum transmission is 0.6042.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_recrystallization_method
'The crystals were growth by means of evaporation of a mixture of n-hexane and toluene at RT.'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8413
_refine_ls_number_restraints     239
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+2.5436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7352
_reflns_number_total             8413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06726j2.cif
_cod_data_source_block           20231009c
_cod_database_code               7135358
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.801
_exptl_crystal_mounting_method
'Crystals were removed from the crystallisation vial and immediately coated with polybutenes oil (CAS: 9003-29-6) on a glass slide. A suitable single crystal coated with polybutenes oil as less as possible was sealed in capillary tube filled with argon. The capillary tube with single crystal was mounted on copper pin with solid paraffin.'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C39-C33 = C39A-C33A
 1.5 with sigma of 0.01
 C39-C34 \\sim C39-C38
 with sigma of 0.02
3. Restrained planarity
 C33A, C38A, C34A, C39A, C37A, C35A, C36A
 with sigma of 0.1
 C33, C34, C35, C38, C39, C36, C37
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C33 \\sim C34 \\sim C35 \\sim C38 \\sim C39 \\sim C36 \\sim C37 \\sim C38A
\\sim C33A \\sim C34A \\sim C39A \\sim C37A \\sim C35A \\sim C36A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Others
 Sof(C33A)=Sof(C38A)=Sof(H38A)=Sof(C37A)=Sof(H37A)=Sof(C36A)=Sof(H36A)=
 Sof(C35A)=Sof(H35A)=Sof(C34A)=Sof(H34A)=Sof(C39A)=Sof(H39D)=Sof(H39E)=
 Sof(H39F)=1-FVAR(1)
 Sof(C33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=Sof(C37)=
 Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C30(H30), C27(H27), C14(H14), C17(H17)
6.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C13(H13A,H13B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C11(H11), C21(H21), C10(H10), C24(H24), C9(H9), C4(H4), C22(H22),
 C5(H5), C8(H8), C6(H6), C23(H23), C34(H34), C35(H35), C36(H36), C37(H37),
 C38(H38), C38A(H38A), C37A(H37A), C36A(H36A), C35A(H35A), C34A(H34A)
6.d Fitted hexagon refined as free rotating group:
 C33(C34,C35,C36,C37,C38), C33A(C38A,C37A,C36A,C35A,C34A)
6.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C28(H28A,H28B,H28C), C16(H16A,H16B,H16C), C32(H32A,H32B,
 H32C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C31(H31A,
 H31B,H31C), C39(H39A,H39B,H39C), C39A(H39D,H39E,H39F)
;
_shelx_res_checksum              84194
_olex2_submission_special_instructions 'No special instructions were received'