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_7135353
_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         'C66 H88 La2 N6 Ni2 P4, 2(C4 H8 O)'
_chemical_formula_sum            'C74 H104 La2 N6 Ni2 O2 P4'
_chemical_formula_weight         1628.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-10-18
_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                75.419(2)
_cell_angle_beta                 70.756(2)
_cell_angle_gamma                66.803(2)
_cell_formula_units_Z            1
_cell_length_a                   11.5616(12)
_cell_length_b                   11.8002(12)
_cell_length_c                   16.2436(17)
_cell_measurement_reflns_used    2844
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.051
_cell_measurement_theta_min      2.163
_cell_volume                     1904.0(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker SMART APEX II 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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0634
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6865
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         2.163
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.716
_exptl_absorpt_correction_T_max  0.745983
_exptl_absorpt_correction_T_min  0.491935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0914 before and 0.0458 after correction.
 
For component 2:
 wR2(int) was 0.0764 before and 0.0495 after correction.
 The Ratio of minimum to maximum transmission is 0.67.

Final HKLF 4 output contains 24098 reflections, Rint = 0.0765
 (10288 with I > 3sig(I), Rint = 0.0634)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.100
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6865
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0876P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1630
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4669
_reflns_number_total             6865
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06726j2.cif
_cod_data_source_block           241017b
_cod_original_cell_volume        1904.1(3)
_cod_database_code               7135353
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.674
_shelx_estimated_absorpt_t_min   0.627
_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
 O1-C33 = O1-C36
 1.43 with sigma of 0.01
 C36-C35 = C35-C34 = C34-C33
 1.54 with sigma of 0.01
 C36-C34 = C35-C33
 2.515 with sigma of 0.02
 C33-C36
 2.336 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C36A \\sim O1A \\sim C33A \\sim C34A \\sim C35A \\sim C34 \\sim O1 \\sim C33
\\sim C36 \\sim C35: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
4. Same fragment restrains
{O1A, C33A, C34A, C35A, C36A} sigma for 1-2: 0.02, 1-3: 0.02
as in
{O1, C33, C34, C35, C36}
5. Others
 Sof(O1A)=Sof(C33A)=Sof(H33C)=Sof(H33D)=Sof(C34A)=Sof(H34C)=Sof(H34D)=
 Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C36A)=Sof(H36C)=Sof(H36D)=1-FVAR(1)
 Sof(O1)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=
 Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C27(H27), C30(H30), C14(H14), C17(H17)
6.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C13(H13A,H13B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C33A(H33C,H33D), C34A(H34C,H34D), C35A(H35C,H35D),
 C36A(H36C,H36D)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C9(H9), C4(H4), C21(H21), C8(H8), C10(H10), C24(H24), C11(H11),
 C23(H23), C6(H6), C22(H22), C5(H5)
6.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C29(H29A,H29B,
 H29C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C16(H16A,H16B,H16C), C18(H18A,
 H18B,H18C)
;
_shelx_res_checksum              35712
_olex2_submission_special_instructions 'No special instructions were received'