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_7716860
_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
'C45 H59 Al N2 Ni O2 P3, C12 H23 N2, 2(C4 H8 O)'
_chemical_formula_sum            'C65 H97 Al N4 Ni O4 P3'
_chemical_formula_weight         1177.06
_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
_audit_creation_date             2023-10-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-06-11 deposited with the CCDC.	2024-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.0440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.6897(2)
_cell_length_b                   18.2605(2)
_cell_length_c                   40.6637(4)
_cell_measurement_reflns_used    47860
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      75.3980
_cell_measurement_theta_min      2.6450
_cell_volume                     14396.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -117.00 -68.00   0.50    2.50    --  -45.70-134.00  74.00   98
  2  \w    -92.00 -18.00   0.50    2.50    --  -45.70 134.00 -38.00  148
  3  \w    -92.00 -18.00   0.50    2.50    --  -45.70 134.00 141.00  148
  4  \w   -117.00 -68.00   0.50    2.50    --  -45.70-134.00-105.00   98
  5  \w     39.00  99.00   0.50    2.50    --   45.70-134.00-105.00  120
  6  \w     39.00  99.00   0.50    2.50    --   45.70-134.00  74.00  120
  7  \w   -161.00 -68.00   0.50   10.00    --  -93.75-134.00-105.00  186
  8  \w    -92.00 -22.00   0.50   10.00    --  -93.75 134.00 141.00  140
  9  \w   -161.00 -68.00   0.50   10.00    --  -93.75-134.00  74.00  186
 10  \w    -92.00 -22.00   0.50   10.00    --  -93.75 134.00 -38.00  140
 11  \w     89.00 178.00   0.50   10.00    --  107.11 134.00 141.00  178
 12  \w     39.00 118.00   0.50   10.00    --  107.11-134.00  74.00  158
 13  \w     39.00 118.00   0.50   10.00    --  107.11-134.00-105.00  158
 14  \w     89.00 178.00   0.50   10.00    --  107.11 134.00 -38.00  178
 15  \w   -118.00 -83.00   0.50    2.50    --  -45.70 -57.00 120.00   70
 16  \w   -118.00 -83.00   0.50    2.50    --  -45.70 -57.00-120.00   70
 17  \w   -118.00 -83.00   0.50    2.50    --  -45.70 -57.00 -30.00   70
 18  \w   -118.00 -83.00   0.50    2.50    --  -45.70 -57.00-150.00   70
 19  \w   -118.00 -83.00   0.50    2.50    --  -45.70 -57.00  90.00   70
 20  \w   -167.00 -83.00   0.50   10.00    --  -93.75 -57.00 -31.69  168
 21  \w    -71.00 -20.00   0.50   10.00    --  -93.75  61.00-180.00  102
 22  \w   -167.00 -83.00   0.50   10.00    --  -93.75 -57.00 -99.26  168
 23  \w    -85.00 -23.00   0.50   10.00    --  -93.75 125.00-180.00  124
 24  \w    -51.00 -20.00   0.50   10.00    --  -93.75  45.00 -30.00   62
 25  \w   -167.00-101.00   0.50   10.00    --  -93.75 -77.00-180.00  132
 26  \w     34.00  71.00   0.50   10.00    --  107.11 -61.00 -30.00   74
 27  \w     36.00 107.00   0.50   10.00    --  107.11-101.00 150.56  142
 28  \w     35.00  68.00   0.50   10.00    --  107.11 -61.00-150.00   66
 29  \w     38.00  68.00   0.50   10.00    --  107.11 -61.00 -90.00   60
 30  \w     46.00 101.00   0.50   10.00    --  107.11 -77.00 -90.00  110
 31  \w     35.00 102.00   0.50   10.00    --  107.11 -94.00 -90.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0268340000
_diffrn_orient_matrix_UB_12      0.0260254000
_diffrn_orient_matrix_UB_13      0.0359787000
_diffrn_orient_matrix_UB_21      0.0083511000
_diffrn_orient_matrix_UB_22      -0.0801933000
_diffrn_orient_matrix_UB_23      0.0118040000
_diffrn_orient_matrix_UB_31      0.0743338000
_diffrn_orient_matrix_UB_32      -0.0001714000
_diffrn_orient_matrix_UB_33      -0.0070428000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            170067
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.476
_diffrn_reflns_theta_min         2.700
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.469
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.177
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       block
_exptl_crystal_F_000             5064
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.202
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1453
_refine_ls_number_reflns         28267
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0737
_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^)+(0.0586P)^2^+45.6424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1798
_refine_ls_wR_factor_ref         0.1877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23455
_reflns_number_total             28267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01786b2.cif
_cod_data_source_block           hpd782c
_cod_depositor_comments
'Adding full bibliography for 7716857--7716860.cif.'
_cod_database_code               7716860
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ni Al C H N O P'
_chemical_oxdiff_usercomment     AGG-64
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.690
_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
 C127-C128
 1.5 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C95(H95), C112(H112), C107(H107), C100(H100)
3.b Secondary CH2 refined with riding coordinates:
 C115(H11O,H11P), C118(H11Q,H11R), C116(H11S,H11T), C121(H12A,H12B), C117(H11U,
 H11V), C122(H12C,H12D), C119(H11M,H11N), C120(H12E,H12F), C130(H13A,H13B),
 C129(H12O,H12P), C126(H12G,H12H), C123(H12I,H12J), C127(H12Q,H12R), C125(H12K,
 H12L), C128(H12S,H12T), C124(H12M,H12N)
3.c Aromatic/amide H refined with riding coordinates:
 C75(H75), C11(H11), C53(H53), C78(H78), C48(H48), C85(H85), C8(H8), C26(H26),
 C56(H56), C51(H51), C31(H31), C50(H50), C5(H5), C83(H83), C23(H23), C54(H54),
 C9(H9), C82(H82), C21(H21), C25(H25), C33(H33), C17(H17), C34(H34), C4(H4),
 C77(H77), C6(H6), C76(H76), C63(H63), C3(H3), C24(H24), C67(H67), C49(H49),
 C66(H66), C64(H64), C65(H65), C19(H19), C20(H20), C18(H18)
3.d Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C68(H68A,H68B,H68C), C28(H28A,H28B,H28C), C80(H80A,H80B,
 H80C), C43(H43A,H43B,H43C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,
 H42B,H42C), C99(H99A,H99B,H99C), C59(H59A,H59B,H59C), C69(H69A,H69B,H69C),
 C111(H11A,H11B,H11C), C98(H98A,H98B,H98C), C97(H97A,H97B,H97C), C70(H70A,H70B,
 H70C), C96(H96A,H96B,H96C), C110(H11D,H11E,H11F), C45(H45A,H45B,H45C),
 C89(H89A,H89B,H89C), C72(H72A,H72B,H72C), C90(H90A,H90B,H90C), C113(H11G,H11H,
 H11I), C108(H10A,H10B,H10C), C94(H94A,H94B,H94C), C36(H36A,H36B,H36C),
 C114(H11J,H11K,H11L), C37(H37A,H37B,H37C), C106(H10D,H10E,H10F), C71(H71A,H71B,
 H71C), C88(H88A,H88B,H88C), C44(H44A,H44B,H44C), C14(H14A,H14B,H14C), C60(H60A,
 H60B,H60C), C61(H61A,H61B,H61C), C109(H10G,H10H,H10I), C101(H10J,H10K,H10L),
 C38(H38A,H38B,H38C), C102(H10M,H10N,H10O), C73(H73A,H73B,H73C), C15(H15A,H15B,
 H15C)
;
_shelx_res_checksum              88859
_shelx_fab_checksum              57334
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.523
_oxdiff_exptl_absorpt_empirical_full_min 0.481