Diphenylacetylene stabilised alkali-metal nickelates: synthesis, structure and catalytic applications.
Borys, Andryj M.; Hevia, Eva; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2098–2105; doi:10.1039/d3dt00069a

data_7712097
_publ_section_title
;
 Diphenylacetylene stabilised alkali-metal nickelates: synthesis,
 structure and catalytic applications.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2098
_journal_page_last               2105
_journal_paper_doi               10.1039/d3dt00069a
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         '2(C39 H43 Li2 Ni O3)'
_chemical_formula_sum            'C78 H86 Li4 Ni2 O6'
_chemical_formula_weight         1264.64
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-31T20:59:13-00:00
_audit_update_record
;
2022-11-22 deposited with the CCDC.	2023-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.3646(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.15833(13)
_cell_length_b                   11.80124(6)
_cell_length_c                   25.58438(14)
_cell_measurement_reflns_used    73973
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      78.982
_cell_measurement_theta_min      2.225
_cell_volume                     6998.57(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_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    -36.00  50.00   0.50    0.60    --  -23.00  46.00  24.00  172
  2  \w    -94.00 -10.00   0.50    0.60    --  -23.00 -46.00-125.00  168
  3  \w     35.00 120.00   0.50    0.60    --   47.92  46.00  24.00  170
  4  \w    -23.00  49.00   0.50    0.60    --   47.92 -46.00-125.00  144
  5  \w    101.00 177.00   0.50    5.00    --  113.25  46.00  24.00  152
  6  \w    -70.00 -12.00   0.50    0.60    --  -23.00 125.00-150.00  116
  7  \w    -70.00 -12.00   0.50    0.60    --  -23.00 125.00 120.00  116
  8  \w    -70.00 -12.00   0.50    0.60    --  -23.00 125.00  30.00  116
  9  \w    -28.00  52.00   0.50    0.60    --  -23.00  15.00-120.00  160
 10  \w     33.00 120.00   0.50    0.60    --   47.92  57.00-180.00  174
 11  \w     33.00 120.00   0.50    0.60    --   47.92  57.00 120.00  174
 12  \w     25.00 121.00   0.50    0.60    --   47.92  77.00-180.00  192
 13  \w    -25.00  40.00   0.50    0.60    --   47.92 -38.00  60.00  130
 14  \w     33.00 120.00   0.50    0.60    --   47.92  57.00 150.00  174
 15  \w    -26.00  23.00   0.50    0.60    --   47.92 -19.00  90.00   98
 16  \w     42.00  76.00   0.50    5.00    --  113.25 -66.00 -61.73   68
 17  \w     42.00 102.00   0.50    5.00    --  113.25 -77.00 -30.00  120
 18  \w     91.00 177.00   0.50    5.00    --  113.25  77.00  90.00  172
 19  \w    101.00 177.00   0.50    5.00    --  113.25  45.00-180.00  152
 20  \w    101.00 177.00   0.50    5.00    --  113.25  45.00  60.00  152
 21  \w    101.00 143.00   0.50    5.00    --  113.25  45.00 150.00   84
 22  \w     42.00  68.00   0.50    5.00    --  113.25 -61.00 150.00   52
 23  \w     98.00 123.00   0.50    5.00    --  113.25  61.00 150.00   50
 24  \w     97.00 176.00   0.50    5.00    --  113.25  61.00-180.00  158
 25  \w     43.00  87.00   0.50    5.00    --  113.25 -77.00 -60.00   88
 26  \w     54.00 101.00   0.50    5.00    --  113.25 -77.00-180.00   94
 27  \w     43.00 105.00   0.50    5.00    --  113.25 -94.00   0.00  124
 28  \w    104.00 174.00   0.50    5.00    --  113.25  48.00-158.89  140
 29  \w     42.00  67.00   0.50    5.00    --  113.25 -61.00-120.00   50
 30  \w     97.00 123.00   0.50    5.00    --  113.25  61.00  90.00   52
 31  \w     58.00  84.00   0.50    5.00    --  113.25   0.00   0.00   52
 32  \w     97.00 123.00   0.50    5.00    --  113.25  61.00  60.00   52
 33  \w    102.00 175.00   0.50    5.00    --  113.25  45.00  90.00  146
 34  \w     42.00 101.00   0.50    5.00    --  113.25 -77.00   0.00  118
 35  \w     42.00  67.00   0.50    5.00    --  113.25 -61.00  90.00   50
 36  \w     48.00  96.00   0.50    5.00    --  113.25 -77.00 120.00   96
 37  \w     91.00 127.00   0.50    5.00    --  113.25  77.00-120.00   72
 38  \w    145.00 171.00   0.50    5.00    --  113.25  61.00 120.00   52
 39  \w     42.00  68.00   0.50    5.00    --  113.25 -61.00-180.00   52
 40  \w    105.00 132.00   0.50    5.00    --  113.25 -87.00  42.76   54
 41  \w    139.00 169.00   0.50    5.00    --  113.25  77.00-120.00   60
 42  \w     91.00 117.00   0.50    5.00    --  113.25  77.00 120.00   52
 43  \w     42.00  99.00   0.50    5.00    --  113.25 -87.00  42.76  114
 44  \w    101.00 142.00   0.50    5.00    --  113.25  25.00 150.98   82
 45  \w     54.00  85.00   0.50    5.00    --  113.25 -77.00-150.00   62
 46  \w     97.00 154.00   0.50    5.00    --  113.25  61.00 -90.00  114
 47  \w     97.00 123.00   0.50    5.00    --  113.25  61.00 120.00   52
 48  \w    102.00 176.00   0.50    5.00    --  113.25  30.00-180.00  148
 49  \w    101.00 149.00   0.50    5.00    --  113.25  30.00 120.00   96
 50  \w    147.00 173.00   0.50    5.00    --  113.25  77.00 150.00   52
 51  \w     96.00 166.00   0.50    5.00    --  113.25  64.00  62.63  140
 52  \w    101.00 128.00   0.50    5.00    --  113.25  30.00 150.00   54
 53  \w    131.00 177.00   0.50    5.00    --  113.25  77.00 -90.00   92
 54  \w     93.00 120.00   0.50    5.00    --  113.25  77.00 150.00   54
 55  \w     43.00 111.00   0.50    5.00    --  113.25   0.00-120.00  136
 56  \w    152.00 177.00   0.50    5.00    --  113.25   0.00-120.00   50
 57  \w    102.00 128.00   0.50    5.00    --  113.25  45.00 120.00   52
 58  \w    152.00 177.00   0.50    5.00    --  113.25  45.00 150.00   50
 59  \w     42.00  67.00   0.50    5.00    --  113.25 -61.00  60.00   50
 60  \w    105.00 175.00   0.50    5.00    --  113.25   0.00   0.00  140
 61  \w     43.00 106.00   0.50    5.00    --  113.25 -99.00 -58.12  126
;
_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      0.0317864
_diffrn_orient_matrix_UB_12      -0.0474417
_diffrn_orient_matrix_UB_13      -0.0396858
_diffrn_orient_matrix_UB_21      -0.0443433
_diffrn_orient_matrix_UB_22      0.0576849
_diffrn_orient_matrix_UB_23      -0.0478927
_diffrn_orient_matrix_UB_31      0.0380066
_diffrn_orient_matrix_UB_32      0.1070332
_diffrn_orient_matrix_UB_33      0.0082569
_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  0.0498
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            133747
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.074
_diffrn_reflns_theta_min         2.222
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.60284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.2
_exptl_crystal_description       block
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.499
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         13317
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.07
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0880P)^2^+9.1049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.185
_refine_ls_wR_factor_ref         0.1863
_reflns_Friedel_coverage         0
_reflns_number_gt                12716
_reflns_number_total             13317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00069a2.cif
_cod_data_source_block           22EH067_AMB-797-THF
_cod_depositor_comments
'Adding full bibliography for 7712094--7712100.cif.'
_cod_original_cell_volume        6998.56(7)
_cod_database_code               7712097
_shelx_estimated_absorpt_t_min   0.771
_shelx_estimated_absorpt_t_max   0.893
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.871
_oxdiff_exptl_absorpt_empirical_full_min 0.68
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
        1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
        2. Rigid bond restraints
 C20, C24, C26, C21, C25, C22, C27, C23, C18, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
        3. Uiso/Uaniso restraints and constraints
Uanis(C70A) \\sim Ueq, Uanis(C69A) \\sim Ueq: with sigma of 0.01 and sigma for
        terminal atoms of 0.02
Uanis(C69) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C72A) \\sim Ueq, Uanis(C73A) \\sim Ueq: with sigma of 0.01 and sigma for
        terminal atoms of 0.02
        4. Others
 Sof(H67C)=Sof(H67D)=Sof(C68A)=Sof(H68C)=Sof(H68D)=Sof(C69A)=Sof(H69C)=
 Sof(H69D)=Sof(C70A)=Sof(H70C)=Sof(H70D)=1-FVAR(1)
 Sof(H67A)=Sof(H67B)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C68)=Sof(H68A)=Sof(H68B)=
 Sof(C69)=Sof(H69A)=Sof(H69B)=FVAR(1)
 Sof(H48A)=Sof(H55A)=Sof(C54A)=Sof(H54A)=Sof(C53A)=Sof(H53A)=Sof(C52A)=
 Sof(H52A)=Sof(C51A)=Sof(C50A)=Sof(H50A)=Sof(C49A)=Sof(H49A)=1-FVAR(2)
 Sof(H48)=Sof(C49)=Sof(H49)=Sof(C51)=Sof(H55)=Sof(C50)=Sof(H50)=Sof(C52)=
 Sof(H52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=FVAR(2)
 Sof(H39C)=Sof(H39D)=Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=1-FVAR(3)
 Sof(H39A)=Sof(H39B)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=FVAR(3)
 Sof(H71C)=Sof(H71D)=Sof(H74C)=Sof(H74D)=Sof(C73A)=Sof(H73C)=Sof(H73D)=
 Sof(C72A)=Sof(H72C)=Sof(H72D)=1-FVAR(4)
 Sof(H71A)=Sof(H71B)=Sof(H74A)=Sof(H74B)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(C73)=
 Sof(H73A)=Sof(H73B)=FVAR(4)
        5.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C78(H78A,H78B), C67(H67A,H67B), C67(H67C,H67D), C39(H39A,
 H39B), C39(H39C,H39D), C35(H35A,H35B), C75(H75A,H75B), C71(H71A,H71B),
 C71(H71C,H71D), C28(H28A,H28B), C31(H31A,H31B), C74(H74A,H74B), C74(H74C,H74D),
  C30(H30A,H30B), C32(H32A,H32B), C34(H34A,H34B), C76(H76A,H76B), C37(H37A,
 H37B), C37(H37C,H37D), C29(H29A,H29B), C77(H77A,H77B), C33(H33A,H33B),
 C70(H70A,H70B), C72(H72A,H72B), C38(H38A,H38B), C73(H73A,H73B), C68(H68A,H68B),
  C69(H69A,H69B), C68A(H68C,H68D), C69A(H69C,H69D), C70A(H70C,H70D), C38A(H38C,
 H38D), C73A(H73C,H73D), C72A(H72C,H72D)
        5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C48(H48A), C48(H48), C42(H42), C9(H9), C6(H6), C16(H16), C3(H3),
 C46(H46), C58(H58), C43(H43), C5(H5), C44(H44), C10(H10), C49(H49), C65(H65),
 C4(H4), C59(H59), C15(H15), C19(H19), C11(H11), C60(H60), C45(H45), C64(H64),
 C20(H20), C55(H55), C55(H55A), C26(H26), C62(H62), C14(H14), C13(H13),
 C50(H50), C63(H63), C25(H25), C52(H52), C21(H21), C23(H23), C53(H53), C54(H54),
  C24(H24), C54A(H54A), C53A(H53A), C52A(H52A), C50A(H50A), C49A(H49A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              65496
_shelx_fab_checksum              35439