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_7135355
_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         'C39 H59 La N4 Ni P2'
_chemical_formula_sum            'C39 H59 La N4 Ni P2'
_chemical_formula_weight         843.46
_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             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                98.310(2)
_cell_angle_beta                 91.120(2)
_cell_angle_gamma                113.988(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7419(16)
_cell_length_b                   12.0017(17)
_cell_length_c                   17.493(3)
_cell_measurement_reflns_used    7290
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.794
_cell_measurement_theta_min      2.362
_cell_volume                     2031.1(5)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker SMART APEX II 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 APEX2 area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'CCD-LDI-APEX2 area detector'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_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  0.0216
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13736
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.047
_diffrn_reflns_theta_min         1.181
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.610
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0912 before and 0.0394 after correction.
The Ratio of minimum to maximum transmission is 0.5940.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_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          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.976
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         10288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0439P)^2^+1.4753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8357
_reflns_number_total             10288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06726j2.cif
_cod_data_source_block           241219a
_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        2031.2(5)
_cod_database_code               7135355
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.689
_shelx_estimated_absorpt_t_min   0.565
_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.a Ternary CH refined with riding coordinates:
 C17(H17), C30(H30), C27(H27), C14(H14), C37(H37), C34(H34)
2.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C13(H13A,H13B)
2.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C11(H11), C2(H2), C23(H23), C33(H33), C10(H10), C4(H4), C22(H22),
 C8(H8), C21(H21), C6(H6), C9(H9), C5(H5)
2.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C19(H19A,H19B,H19C), C31(H31A,H31B,H31C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C38(H38A,H38B,H38C), C28(H28A,H28B,H28C), C39(H39A,
 H39B,H39C), C29(H29A,H29B,H29C), C15(H15A,H15B,H15C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              4415
_olex2_submission_special_instructions 'No special instructions were received'