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_7716859
_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_absolute_configuration ad
_chemical_formula_moiety
'C90 H88 Al N2 Ni O2 P5, C90 H87 Al N2 Ni O2 P5, 2(C6 H6), 2[C6H6]'
_chemical_formula_sum            'C204 H199 Al2 N4 Ni2 O4 P10'
_chemical_formula_weight         3251.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-06
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-11 deposited with the CCDC.	2024-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4356(2)
_cell_length_b                   48.5980(6)
_cell_length_c                   20.8299(2)
_cell_measurement_reflns_used    36448
_cell_measurement_temperature    100.02(16)
_cell_measurement_theta_max      75.7230
_cell_measurement_theta_min      3.4540
_cell_volume                     17649.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.121a 64-bit (release 24-04-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(16)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.893
_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    -30.00  33.00   0.50   10.47    --  -45.30  19.00 -49.00  126
  2  \w   -172.00 -73.00   0.50   41.87    --  -93.75 -19.00 142.00  198
  3  \w    -87.00 -22.00   0.50   41.87    --  -93.75 126.00 161.00  130
  4  \w     36.00 113.00   0.50   41.87    --  107.26-126.00  84.00  154
  5  \w    105.00 178.00   0.50   41.87    --  107.26 106.00  81.00  146
  6  \w    -43.00  30.00   0.50   10.47    --  -45.30  37.00  30.00  146
  7  \w     34.00  94.00   0.50   10.47    --   45.30-125.00-180.00  120
  8  \w     83.00 118.00   0.50   10.47    --   45.30  57.00-180.00   70
  9  \w     83.00 118.00   0.50   10.47    --   45.30  57.00 -90.00   70
 10  \w    -51.00 -20.00   0.50   41.87    --  -93.75  45.00  30.00   62
 11  \w     34.00 101.00   0.50   41.87    --  107.26 -77.00 -90.00  134
 12  \w     34.00  71.00   0.50   41.87    --  107.26 -61.00  60.00   74
 13  \w     34.00  71.00   0.50   41.87    --  107.26 -61.00-120.00   74
 14  \w     34.00  71.00   0.50   41.87    --  107.26 -61.00 150.00   74
 15  \w     83.00 111.00   0.50   10.47    --   45.30  57.00 -30.00   56
;
_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      -0.0156585000
_diffrn_orient_matrix_UB_12      -0.0259994000
_diffrn_orient_matrix_UB_13      -0.0403652000
_diffrn_orient_matrix_UB_21      -0.0163213000
_diffrn_orient_matrix_UB_22      -0.0163474000
_diffrn_orient_matrix_UB_23      0.0617974000
_diffrn_orient_matrix_UB_31      -0.0854051000
_diffrn_orient_matrix_UB_32      0.0078522000
_diffrn_orient_matrix_UB_33      -0.0048960000
_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  0.0390
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       -59
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            93407
_diffrn_reflns_point_group_measured_fraction_full 0.811
_diffrn_reflns_point_group_measured_fraction_max 0.743
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.089
_diffrn_reflns_theta_min         2.794
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.658
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.559
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.121a (Rigaku Oxford Diffraction, 2024)
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    1.224
_exptl_crystal_description       plate
_exptl_crystal_F_000             6860
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.433(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3658
_refine_ls_number_reflns         54808
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+42.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1496
_reflns_Friedel_coverage         0.644
_reflns_Friedel_fraction_full    0.667
_reflns_Friedel_fraction_max     0.589
_reflns_number_gt                45359
_reflns_number_total             54808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01786b2.cif
_cod_data_source_block           hpd899yy
_cod_depositor_comments
'Adding full bibliography for 7716857--7716860.cif.'
_cod_database_code               7716859
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ni Al C H N O P'
_chemical_oxdiff_usercomment     'Al/Ni sample benzene'
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.628
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.567(19)
 0.433(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H370,H,HA} of C370, All C(H,H) groups
 At 1.5 times of:
  {H19A,H19B,H19C} of C190, {H21A,H21B,H21C} of C214, {H12A,H12B,H12C} of
  C124, {H19D,H19E,H19F} of C197, {H28A,H28B,H28C} of C287, {H10A,H10B,H10C} of
  C107, {H17A,H17B,H17C} of C17, {H34A,H34B,H34C} of C34, {H99A,H99B,H99C} of
  C99, {H26A,H26B,H26C} of C26, {H27A,H27B,H27C} of C27, {H30A,H30B,H30C} of
  C304, {H20A,H20B,H20C} of C205, {H27D,H27E,H27F} of C279, {H18A,H18B,H18C} of
  C188, {H20D,H20E,H20F} of C206, {H25A,H25B,H25C} of C25, {H10G,H10H,H10I} of
  C10, {H11G,H11H,H11I} of C115, {H10D,H10E,H10F} of C100, {H11A,H11B,H11C} of
  C117, {H11D,H11E,H11F} of C116, {H18D,H18E,H18F} of C189, {H8A,H8B,H8C} of C8,
   {H27G,H27H,H27I} of C278, {H29D,H29E,H29F} of C297, {H20G,H20H,H20I} of C207,
   {H98A,H98B,H98C} of C98, {H9A,H9B,H9C} of C9, {H29A,H29B,H29C} of C295,
  {H29G,H29H,H29I} of C296, {H28D,H28E,H28F} of C280
3. Uiso/Uaniso restraints and constraints
Uanis(C370) = Uanis(C369) = Uanis(C368) = Uanis(C367) = Uanis(C372) =
Uanis(C371)
Uanis(C377) = Uanis(C378) = Uanis(C373) = Uanis(C374) = Uanis(C375) =
Uanis(C376)
Uanis(C379) = Uanis(C384) = Uanis(C383) = Uanis(C382) = Uanis(C381) =
Uanis(C380)
Uanis(C115) = Uanis(C114) = Uanis(C116) = Uanis(C117)
Uanis(C316) = Uanis(C311) = Uanis(C312) = Uanis(C313) = Uanis(C314) =
Uanis(C315)
Uanis(C296) = Uanis(C294) = Uanis(C297) = Uanis(C295)
Uanis(C279) = Uanis(C277) = Uanis(C278) = Uanis(C280)
Uanis(P9) = Uanis(C168) = Uanis(P10)
Uanis(C91) = Uanis(C92) = Uanis(C96)
Uanis(C57) = Uanis(C56) = Uanis(C58)
Uanis(C156) = Uanis(C161) = Uanis(C157)
4.a Secondary CH2 refined with riding coordinates:
 C323(H32A,H32B), C78(H78A,H78B), C47(H47A,H47B), C233(H23A,H23B), C258(H25D,
 H25E), C348(H34D,H34E), C168(H16A,H16B), C143(H14A,H14B)
4.b Aromatic/amide H refined with riding coordinates:
 C132(H132), C93(H93), C95(H95), C186(H186), C6(H6), C4(H4), C290(H290),
 C40(H40), C212(H212), C193(H193), C200(H200), C276(H276), C77(H77), C122(H122),
  C46(H46), C217(H217), C203(H203), C33(H33), C325(H325), C239(H239),
 C167(H167), C179(H179), C70(H70), C55(H55), C92(H92), C130(H130), C283(H283),
 C293(H293), C102(H102), C119(H119), C45(H45), C105(H105), C285(H285), C3(H3),
 C16(H16), C216(H216), C59(H59), C343(H343), C322(H322), C14(H14), C183(H183),
 C178(H178), C185(H185), C39(H39), C30(H30), C218(H218), C232(H232), C67(H67),
 C13(H13), C23(H23), C196(H196), C71(H71), C166(H166), C42(H42), C113(H113),
 C310(H310), C104(H104), C286(H286), C75(H75), C202(H202), C235(H235),
 C165(H165), C155(H155), C15(H15), C76(H76), C253(H253), C136(H136), C177(H177),
  C22(H22), C43(H43), C36(H36), C82(H82), C302(H302), C228(H228), C219(H219),
 C300(H300), C315(H315), C58(H58), C292(H292), C74(H74), C352(H352), C87(H87),
 C341(H341), C149(H149), C138(H138), C172(H172), C257(H257), C44(H44),
 C135(H135), C158(H158), C31(H31), C303(H303), C260(H260), C270(H270),
 C327(H327), C350(H350), C231(H231), C340(H340), C84(H84), C194(H194), C56(H56),
  C209(H209), C347(H347), C73(H73), C314(H314), C50(H50), C326(H326),
 C173(H173), C51(H51), C220(H220), C195(H195), C245(H245), C20(H20), C164(H164),
  C90(H90), C53(H53), C223(H223), C142(H142), C238(H238), C275(H275),
 C126(H126), C237(H237), C148(H148), C151(H151), C52(H52), C176(H176),
 C139(H139), C62(H62), C127(H127), C333(H333), C247(H247), C236(H236), C88(H88),
  C32(H32), C180(H180), C121(H121), C241(H241), C49(H49), C80(H80), C89(H89),
 C264(H264), C360(H360), C329(H329), C81(H81), C301(H301), C112(H112),
 C284(H284), C37(H37), C250(H250), C356(H356), C110(H110), C157(H157),
 C321(H321), C273(H273), C226(H226), C248(H248), C210(H210), C103(H103),
 C344(H344), C133(H133), C83(H83), C346(H346), C211(H211), C161(H161),
 C306(H306), C38(H38), C243(H243), C318(H318), C57(H57), C63(H63), C222(H222),
 C120(H120), C69(H69), C309(H309), C255(H255), C254(H254), C229(H229),
 C163(H163), C320(H320), C242(H242), C146(H146), C261(H261), C262(H262),
 C152(H152), C351(H351), C335(H335), C154(H154), C145(H145), C244(H244),
 C338(H338), C339(H339), C266(H266), C159(H159), C61(H61), C249(H249),
 C337(H337), C268(H268), C319(H319), C129(H129), C64(H64), C269(H269),
 C153(H153), C251(H251), C140(H140), C354(H354), C332(H332), C147(H147),
 C225(H225), C263(H263), C86(H86), C359(H359), C256(H256), C230(H230),
 C267(H267), C134(H134), C358(H358), C68(H68), C353(H353), C160(H160),
 C224(H224), C331(H331), C307(H307), C328(H328), C65(H65), C366(H366),
 C334(H334), C312(H312), C128(H128), C345(H345), C174(H174), C170(H170),
 C357(H357), C141(H141), C308(H308), C171(H171), C362(H362), C313(H313),
 C377(H377), C365(H365), C378(H378), C367(H367), C361(H361), C372(H372),
 C363(H363), C368(H368), C376(H376), C383(H383), C384(H384), C379(H379),
 C380(H380), C381(H381), C382(H382), C374(H374), C364(H364), C373(H373),
 C371(H371), C375(H375), C316(H316), C369(H369), C370(H370)
4.c Fitted hexagon refined as free rotating group:
 C383(C384,C379,C380,C381,C382)
4.d Idealised Me refined as rotating group:
 C107(H10A,H10B,H10C), C34(H34A,H34B,H34C), C17(H17A,H17B,H17C), C304(H30A,
 H30B,H30C), C26(H26A,H26B,H26C), C99(H99A,H99B,H99C), C27(H27A,H27B,H27C),
 C205(H20A,H20B,H20C), C190(H19A,H19B,H19C), C287(H28A,H28B,H28C), C214(H21A,
 H21B,H21C), C124(H12A,H12B,H12C), C197(H19D,H19E,H19F), C279(H27D,H27E,H27F),
 C188(H18A,H18B,H18C), C206(H20D,H20E,H20F), C25(H25A,H25B,H25C), C100(H10D,
 H10E,H10F), C117(H11A,H11B,H11C), C189(H18D,H18E,H18F), C10(H10G,H10H,H10I),
 C8(H8A,H8B,H8C), C116(H11D,H11E,H11F), C115(H11G,H11H,H11I), C295(H29A,H29B,
 H29C), C9(H9A,H9B,H9C), C207(H20G,H20H,H20I), C297(H29D,H29E,H29F), C278(H27G,
 H27H,H27I), C98(H98A,H98B,H98C), C280(H28D,H28E,H28F), C296(H29G,H29H,H29I)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31914
_shelx_fab_checksum              9931
_olex2_exptl_crystal_mounting_method 'nylon loop'
_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 2.055
_oxdiff_exptl_absorpt_empirical_full_min 0.686