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_7135354
_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         'C42 H63 La N4 Ni P2, C6 H6'
_chemical_formula_sum            'C48 H69 La N4 Ni P2'
_chemical_formula_weight         961.63
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-09-03
_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                104.653(3)
_cell_angle_beta                 104.046(3)
_cell_angle_gamma                96.320(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1638(14)
_cell_length_b                   12.7284(17)
_cell_length_c                   20.816(4)
_cell_measurement_reflns_used    7820
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.706
_cell_measurement_theta_min      2.602
_cell_volume                     2484.9(7)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (Bruker, 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                 'Bruker PHOTON-II area detector'
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.744
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II area detector'
_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  0.0628
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.744
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11978
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.744
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.180
_diffrn_reflns_theta_min         1.054
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.325
_exptl_absorpt_correction_T_max  0.746207
_exptl_absorpt_correction_T_min  0.170064
_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 0.0936 before and 0.0317 after correction.
 
For component 2:
 wR2(int) was 0.1906 before and 0.0594 after correction.
 The Ratio of minimum to maximum transmission is 0.23.

Final HKLF 4 output contains 20735 reflections, Rint = 0.0614
 (13658 with I > 3sig(I), Rint = 0.0628)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_recrystallization_method
;
 The crystals were growth by means of evaporation of a mixture
 of n-hexane and benzene at RT.
;
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.002
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         11978
_refine_ls_number_restraints     523
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0897P)^2^+5.1702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9844
_reflns_number_total             11978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06726j2.cif
_cod_data_source_block           240925a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        2484.9(6)
_cod_database_code               7135354
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.692
_exptl_crystal_mounting_method
;
 Crystals were removed from the crystallisation vial and immediately coated
 with PDMS (polydimethylsiloxane/Dimethicone, CAS: 9006-65-9 on a glass slide.
 A suitable single crystal was selected and mounted on a glass fiber using
 vacuum silicone grease as adhesive. The glass fiber with single crystal was
 mounted on copper pin with solid paraffin. Operator: DJ_Tokyo.
;
_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
 C46-C45 = C45-C44 = C44-C43 = C48-C43 = C48-C47 = C47-C46
 1.39 with sigma of 0.01
3. Restrained planarity
 C43, C44, C48, C45, C47, C46
 with sigma of 0.1
 C44A, C43A, C48A, C45A, C47A, C46A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
P1 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C14A \\sim
C15A \\sim C16A \\sim C17A \\sim C18A \\sim C19A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C34 \\sim C35 \\sim C36 \\sim C37 \\sim C35A \\sim C36A \\sim C37A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C43A \\sim C44A
\\sim C45A \\sim C46A \\sim C47A \\sim C48A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C39 \\sim C40 \\sim C41 \\sim C42 \\sim C40A \\sim C41A \\sim C42A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Same fragment restrains
{C34, C35A, C36A, C37A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C34, C35, C36, C37}
{C39, C40A, C41A, C42A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C39, C40, C41, C42}
{P1, C14A, C15A, C16A, C17A, C18A, C19A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{P1, C14, C15, C16, C17, C18, C19}
{C43A, C44A, C45A, C46A, C47A, C48A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C43, C44, C45, C46, C47, C48}
6. Others
 Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36A)=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(1)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(1)
 Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=
 Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(2)
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(2)
 Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C41A)=Sof(H41D)=Sof(H41E)=
 Sof(H41F)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(3)
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(3)
 Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=
 Sof(H46A)=Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(H48A)=1-FVAR(4)
 Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=
 Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48)=FVAR(4)
7.a Riding coordinates:
 C42(H42A,H42B,H42C), C36A(H36D,H36E,H36F), C37A(H37D,H37E,H37F)
7.b Ternary CH refined with riding coordinates:
 C27(H27), C30(H30), C14(H14), C17(H17), C14A(H14A), C17A(H17A)
7.c Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C13(H13A,H13B)
7.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C5(H5), C4(H4), C21(H21), C22(H22), C23(H23), C24(H24),
 C8(H8), C9(H9), C10(H10), C11(H11), C43(H43), C44(H44), C45(H45), C46(H46),
 C47(H47), C48(H48), C43A(H43A), C44A(H44A), C45A(H45A), C46A(H46A), C47A(H47A),
  C48A(H48A)
7.e Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C15A(H15D,H15E,H15F), C16A(H16D,H16E,
 H16F), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C35A(H35D,H35E,H35F),
 C40A(H40D,H40E,H40F), C41A(H41D,H41E,H41F), C42A(H42D,H42E,H42F)
;
_shelx_res_checksum              33984
_olex2_submission_special_instructions 'No special instructions were received'