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_7716858
_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         '2(C46 H62 Al N2 Ni O2 P3), C4 H6 O'
_chemical_formula_sum            'C96 H130 Al2 N4 Ni2 O5 P6'
_chemical_formula_weight         1777.23
_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     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                103.6970(10)
_cell_angle_beta                 97.8500(10)
_cell_angle_gamma                90.4850(10)
_cell_formula_units_Z            2
_cell_length_a                   13.39500(10)
_cell_length_b                   15.9482(2)
_cell_length_c                   23.2712(3)
_cell_measurement_reflns_used    39743
_cell_measurement_temperature    101(1)
_cell_measurement_theta_max      74.4730
_cell_measurement_theta_min      1.9790
_cell_volume                     4780.40(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      101.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -81.00 -36.00   0.50    0.67    --  -54.75 -15.00 120.00   90
  2  \w    -54.00 -24.00   0.50    0.67    --  -54.75 -15.00  60.00   60
  3  \w    -95.00 -58.00   0.50    0.67    --  -54.75 -15.00  60.00   74
  4  \w    -89.00 -60.00   0.50    0.67    --  -54.75   0.00  30.00   58
  5  \w    -58.00 -32.00   0.50    0.67    --  -54.75   0.00  30.00   52
  6  \w    -98.00 -31.00   0.50    0.67    --  -54.75 -15.00-180.00  134
  7  \w     30.00  82.00   0.50    0.67    --   63.40   0.00  90.00  104
  8  \w     41.00  94.00   0.50    0.67    --   63.40  15.00 120.00  106
  9  \w     49.00  75.00   0.50    0.67    --   75.19  15.00  60.00   52
 10  \w     84.00 119.00   0.50    0.67    --   75.19  15.00  60.00   70
 11  \w     58.00 107.00   0.50    0.67    --   63.40  15.00   0.00   98
 12  \w     62.00 119.00   0.50    0.67    --   75.19  15.00   0.00  114
 13  \w     50.00 121.00   0.50    0.67    --   75.77  15.00-150.00  142
 14  \w     70.00 111.00   0.50    0.67    --   75.19   0.00 -90.00   82
 15  \w     49.00 113.00   0.50    0.67    --   75.19   0.00 150.00  128
 16  \w     49.00  79.00   0.50    0.67    --   75.19 -95.00  30.00   60
 17  \w     40.00  70.00   0.50    0.67    --   79.16-131.00 102.06   60
 18  \w     84.00 110.00   0.50    0.67    --   79.16-131.00 102.06   52
 19  \w     62.00  97.00   0.50    0.67    --   63.40-135.00  10.00   70
 20  \w     37.00  71.00   0.50    0.67    --   79.16-129.00 -43.91   68
 21  \w     37.00 103.00   0.50    0.67    --   79.16-128.00  40.59  132
 22  \w     84.00 109.00   0.50    0.67    --   79.16-129.00 -43.91   50
 23  \w     41.00  87.00   0.50    0.67    --   63.40-125.00  30.00   92
 24  \w     41.00 110.00   0.50    0.67    --   79.16-130.00-111.11  138
 25  \w     50.00 109.00   0.50    0.67    --   75.19-135.00-169.00  118
 26  \w     37.00  65.00   0.50    0.67    --   63.40-125.00-180.00   56
 27  \w     44.00  89.00   0.50    0.67    --   63.40-125.00-150.00   90
 28  \w     47.00  87.00   0.50    0.67    --   63.40-125.00 -30.00   80
 29  \w     79.00  98.00   0.50    0.67    --   79.16-122.00 -80.33   38
 30  \w     48.00 102.00   0.50    0.67    --   75.19-125.00 120.00  108
 31  \w     57.00  89.00   0.50    0.67    --   63.40-125.00 150.00   64
 32  \w     80.00 102.00   0.50    0.67    --   79.16-123.00 165.15   44
 33  \w     36.00  71.00   0.50    0.67    --   75.19-125.00 150.00   70
 34  \w     26.00  72.00   0.50    0.67    --   63.40 -95.00  30.00   92
 35  \w     27.00  70.00   0.50    0.67    --   63.40 -95.00  90.00   86
 36  \w     42.00  95.50   0.50    0.67    --   79.16-120.00 -14.62  107
 37  \w     38.00  64.00   0.50    0.67    --   79.16-122.00 -80.33   52
 38  \w     37.00  62.00   0.50    0.67    --   75.19 -95.00-180.00   50
 39  \w     31.00  69.00   0.50    0.67    --   63.40 -95.00-120.00   76
 40  \w     55.00  83.00   0.50    0.67    --   75.19 -95.00-120.00   56
 41  \w     53.00  83.00   0.50    0.67    --   75.77 -95.00 -60.00   60
 42  \w     57.00  84.00   0.50    0.67    --   75.77 -95.00  60.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            68604
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         1.974
_exptl_absorpt_coefficient_mu    2.015
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       needle
_exptl_crystal_F_000             1892
_exptl_crystal_recrystallization_method 'Slow evaporation for diethyl ether'
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1139
_refine_ls_number_reflns         16801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0466P)^2^+3.2606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14404
_reflns_number_total             16801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01786b2.cif
_cod_data_source_block           aggdelete
_cod_depositor_comments
'Adding full bibliography for 7716857--7716860.cif.'
_cod_original_cell_volume        4780.39(10)
_cod_database_code               7716858
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.668
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C103) = Uanis(C102)
Uanis(O6) = Uanis(O7)
Uanis(C103) = Uanis(C101)
3. Others
 Sof(C99)=Sof(C94)=Sof(C96)=Sof(H96)=Sof(C97)=Sof(H97)=Sof(C98)=Sof(H98)=
 Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(O4)=Sof(C95)=Sof(H95)=1-FVAR(1)
 Sof(O5)=Sof(C62)=Sof(H62)=Sof(C59)=Sof(H59)=Sof(C60)=Sof(H60)=Sof(C57)=
 Sof(C58)=Sof(C61)=Sof(H61)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(1)
 Sof(O6)=1-FVAR(2)
 Sof(O7)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C62(H62), C77(H77), C29(H29), C74(H74), C30(H30), C49(H49), C19(H19),
 C27(H27), C22(H22), C5(H5), C20(H20), C16(H16), C76(H76), C2(H2), C36(H36),
 C67(H67), C51(H51), C40(H40), C66(H66), C21(H21), C83(H83), C69(H69), C39(H39),
  C3(H3), C68(H68), C87(H87), C52(H52), C13(H13), C84(H84), C85(H85), C86(H86),
 C38(H38), C15(H15), C37(H37), C14(H14), C59(H59), C60(H60), C61(H61), C96(H96),
  C97(H97), C98(H98), C95(H95)
4.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C79(H79A,H79B,
 H79C), C41(H41A,H41B,H41C), C71(H71A,H71B,H71C), C88(H88A,H88B,H88C), C32(H32A,
 H32B,H32C), C54(H54A,H54B,H54C), C80(H80A,H80B,H80C), C90(H90A,H90B,H90C),
 C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C89(H89A,H89B,
 H89C), C46(H46A,H46B,H46C), C17(H17A,H17B,H17C), C43(H43A,H43B,H43C), C9(H9A,
 H9B,H9C), C56(H56A,H56B,H56C), C55(H55A,H55B,H55C), C10(H10D,H10E,H10F),
 C81(H81A,H81B,H81C), C93(H93A,H93B,H93C), C8(H8A,H8B,H8C), C91(H91A,H91B,H91C),
  C92(H92A,H92B,H92C), C63(H63A,H63B,H63C), C100(H10A,H10B,H10C), C104(H10G,
 H10H,H10I), C101(H10J,H10K,H10L)
;
_shelx_res_checksum              4143
_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
;