Synthesis and characterization of NiAl-hydride heterometallics: perturbing electron density within Al-H-Ni subunits.
Gonzalez, Aleida G.; Gonzalez, Fernando; De Leon, Edgardo; Birkhoff, Kaitlyn M.; Yruegas, Sam; Chen, Haoyuan; Shoshani, Manar M.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18932–18945; doi:10.1039/d4dt01786b

data_7716857
_publ_section_title
;
 Synthesis and characterization of NiAl-hydride heterometallics:
 perturbing electron density within Al-H-Ni subunits.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18932
_journal_page_last               18945
_journal_paper_doi               10.1039/d4dt01786b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C76 H74 Al N2 Ni O2 P3'
_chemical_formula_sum            'C76 H74 Al N2 Ni O2 P3'
_chemical_formula_weight         1225.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-06-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2024-06-11 deposited with the CCDC.	2024-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.555(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9928(5)
_cell_length_b                   17.5090(4)
_cell_length_c                   17.8697(4)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      74.4370
_cell_measurement_theta_min      3.5310
_cell_volume                     6836.1(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 150'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1141
_diffrn_reflns_av_unetI/netI     0.1164
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            56087
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         2.022
_exptl_absorpt_coefficient_mu    1.548
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.121.42.49 (Rigaku Oxford Diffraction, 2022)'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       prism
_exptl_crystal_F_000             2584
_exptl_crystal_recrystallization_method 'vapor diffusion beznene/pentane'
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         12180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+3.8257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1814
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7074
_reflns_number_total             12180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01786b2.cif
_cod_data_source_block           edl01_sq
_cod_depositor_comments
'Adding full bibliography for 7716857--7716860.cif.'
_cod_database_code               7716857
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   1.000
_shelx_estimated_absorpt_t_min   0.902
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C15)
Uanis(C33) = Uanis(C15A)
Uanis(C33) = Uanis(C17)
Uanis(C33) = Uanis(C17A)
Uanis(C33) = Uanis(C31)
3. Others
 Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=1-FVAR(1)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(C16)=Sof(H16D)=Sof(H16E)=Sof(H16F)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C19(H19), C2(H2), C13(H13), C75(H75), C22(H22), C28(H28), C60(H60),
 C59(H59), C21(H21), C61(H61), C12(H12), C63(H63), C29(H29), C35(H35), C20(H20),
  C57(H57), C3(H3), C5(H5), C66(H66), C74(H74), C10(H10), C69(H69), C39(H39),
 C47(H47), C71(H71), C41(H41), C56(H56), C65(H65), C73(H73), C4(H4), C38(H38),
 C37(H37), C45(H45), C72(H72), C67(H67), C62(H62), C55(H55), C68(H68), C36(H36),
  C43(H43), C51(H51), C48(H48), C42(H42), C49(H49), C44(H44), C50(H50),
 C53(H53), C54(H54)
4.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C7(H7A,H7B,H7C), C33(H33A,H33B,H33C), C32(H32A,H32B,
 H32C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F),
 C15A(H15D,H15E,H15F), C16A(H16A,H16B,H16C), C16(H16D,H16E,H16F), C31(H31A,H31B,
 H31C)
;
_shelx_res_checksum              6309
_shelx_fab_checksum              98576
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'