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_7712094
_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(C27 H35 Li2 Ni O2)'
_chemical_formula_sum            'C54 H70 Li4 Ni2 O4'
_chemical_formula_weight         928.28
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-27T09:13:22-00:00
_audit_update_record
;
2022-11-22 deposited with the CCDC.	2023-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.9245(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.10128(7)
_cell_length_b                   32.53880(15)
_cell_length_c                   20.86994(9)
_cell_measurement_reflns_used    62037
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      79.587
_cell_measurement_theta_min      2.708
_cell_volume                     10217.17(8)
_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      173.01(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 0.999
_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  52.00   0.50    0.25    --  -23.00  34.00  56.00  176
  2  \w    -96.00 -10.00   0.50    0.25    --  -23.00 -34.00-101.00  172
  3  \w     35.00 121.00   0.50    0.25    --   47.95  34.00  56.00  172
  4  \w    -25.00  36.00   0.50    0.25    --   47.95 -34.00-101.00  122
  5  \w    100.00 177.00   0.50    1.80    --  113.25  34.00  56.00  154
  6  \w    -46.00  50.00   0.50    0.25    --  -23.00  77.00-150.00  192
  7  \w    -38.00  50.00   0.50    0.25    --  -23.00  57.00 120.00  176
  8  \w    -70.00 -12.00   0.50    0.25    --  -23.00 125.00  60.00  116
  9  \w     33.00 119.00   0.50    0.25    --   47.95  57.00 150.00  172
 10  \w     25.00 120.00   0.50    0.25    --   47.95  77.00-150.00  190
 11  \w     25.00 120.00   0.50    0.25    --   47.95  77.00 150.00  190
 12  \w     25.00 120.00   0.50    0.25    --   47.95  77.00 -90.00  190
 13  \w    -25.00  22.00   0.50    0.25    --   47.95 -19.00 120.00   94
 14  \w     34.00 119.00   0.50    0.25    --   47.95  57.00-150.00  170
 15  \w     46.00  97.00   0.50    1.80    --  113.25 -77.00 120.00  102
 16  \w     42.00  88.00   0.50    1.80    --  113.25 -77.00-120.00   92
 17  \w     97.00 123.00   0.50    1.80    --  113.25  61.00  90.00   52
 18  \w     93.00 118.00   0.50    1.80    --  113.25  73.00 145.85   50
 19  \w    101.00 136.00   0.50    1.80    --  113.25  43.00 155.95   70
 20  \w     42.00  68.00   0.50    1.80    --  113.25 -64.00 173.90   52
 21  \w    101.00 126.00   0.50    1.80    --  113.25  15.00 150.00   50
 22  \w     42.00  67.00   0.50    1.80    --  113.25 -61.00  30.00   50
 23  \w     97.00 123.00   0.50    1.80    --  113.25  61.00-180.00   52
 24  \w    149.00 174.00   0.50    1.80    --  113.25  72.00-161.59   50
 25  \w     42.00  67.00   0.50    1.80    --  113.25 -61.00 -30.00   50
 26  \w     92.00 118.00   0.50    1.80    --  113.25  74.00 115.75   52
 27  \w    145.00 172.00   0.50    1.80    --  113.25  74.00 115.75   54
 28  \w     97.00 123.00   0.50    1.80    --  113.25  61.00 150.00   52
 29  \w    142.00 168.00   0.50    1.80    --  113.25  61.00  90.00   52
 30  \w     79.00 105.00   0.50    1.80    --  113.25 -94.00-180.00   52
 31  \w     91.00 117.00   0.50    1.80    --  113.25  77.00 120.00   52
 32  \w     56.00  96.00   0.50    1.80    --  113.25 -77.00 -90.00   80
 33  \w    152.00 177.00   0.50    1.80    --  113.25  73.00 145.85   50
 34  \w     42.00  67.00   0.50    1.80    --  113.25 -61.00-180.00   50
 35  \w    101.00 128.00   0.50    1.80    --  113.25  45.00 120.00   54
 36  \w     43.00  68.00   0.50    1.80    --  113.25 -61.00-120.00   50
 37  \w     93.00 119.00   0.50    1.80    --  113.25  72.00-161.59   52
 38  \w    104.00 172.00   0.50    1.80    --  113.25   0.00   0.00  136
 39  \w     44.00  97.00   0.50    1.80    --  113.25   0.00   0.00  106
 40  \w    149.00 175.00   0.50    1.80    --  113.25  58.00 -61.92   52
 41  \w    101.00 146.00   0.50    1.80    --  113.25  45.00  90.00   90
 42  \w     91.00 117.00   0.50    1.80    --  113.25  77.00 150.00   52
 43  \w     43.00  92.00   0.50    1.80    --  113.25 -77.00  60.00   98
 44  \w     97.00 123.00   0.50    1.80    --  113.25  61.00 120.00   52
 45  \w    149.00 175.00   0.50    1.80    --  113.25  61.00 120.00   52
 46  \w     95.00 121.00   0.50    1.80    --  113.25  67.00 134.96   52
 47  \w     95.00 120.00   0.50    1.80    --  113.25  67.00-168.33   50
 48  \w    128.00 174.00   0.50    1.80    --  113.25  67.00-168.33   92
 49  \w     92.00 117.00   0.50    1.80    --  113.25  77.00  90.00   50
 50  \w    133.00 176.00   0.50    1.80    --  113.25  77.00  90.00   86
 51  \w     45.00  81.00   0.50    1.80    --  113.25 -77.00 150.00   72
 52  \w     97.00 123.00   0.50    1.80    --  113.25  61.00 127.88   52
 53  \w     93.00 128.00   0.50    1.80    --  113.25  71.00  83.31   70
 54  \w    100.00 141.00   0.50    1.80    --  113.25  47.00  96.45   82
 55  \w     45.00  75.00   0.50    1.80    --  113.25 -94.00-180.00   60
 56  \w     98.00 136.00   0.50    1.80    --  113.25  58.00 -61.92   76
 57  \w    151.00 177.00   0.50    1.80    --  113.25  45.00-150.00   52
 58  \w    102.00 128.00   0.50    1.80    --  113.25  45.00 150.00   52
 59  \w     42.00  67.00   0.50    1.80    --  113.25 -61.00   0.00   50
 60  \w    102.00 167.00   0.50    1.80    --  113.25  30.00 150.00  130
 61  \w    101.00 129.00   0.50    1.80    --  113.25  30.00-150.00   56
 62  \w    103.00 128.00   0.50    1.80    --  113.25  30.00-120.00   50
 63  \w    142.00 168.00   0.50    1.80    --  113.25  30.00-120.00   52
 64  \w    106.00 132.00   0.50    1.80    --  113.25  42.00-156.15   52
 65  \w     96.00 123.00   0.50    1.80    --  113.25  69.00 145.94   54
 66  \w     91.00 117.00   0.50    1.80    --  113.25  77.00-150.00   52
 67  \w    103.00 172.00   0.50    1.80    --  113.25  45.00-180.00  138
 68  \w    101.00 127.00   0.50    1.80    --  113.25  45.00-150.00   52
 69  \w    141.00 177.00   0.50    1.80    --  113.25  43.00 155.95   72
 70  \w    103.00 158.00   0.50    1.80    --  113.25  30.00-180.00  110
 71  \w     98.00 123.00   0.50    1.80    --  113.25  59.00 128.29   50
 72  \w     42.00  67.00   0.50    1.80    --  113.25 -61.00  90.00   50
 73  \w     93.00 119.00   0.50    1.80    --  113.25  72.00 141.74   52
 74  \w     43.00 101.00   0.50    1.80    --  113.25-105.00  36.54  116
 75  \w     42.00  67.00   0.50    1.80    --  113.25 -61.00 120.00   50
 76  \w     42.00  67.00   0.50    1.80    --  113.25 -61.00  60.00   50
;
_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      -0.0233121
_diffrn_orient_matrix_UB_12      -0.0188246
_diffrn_orient_matrix_UB_13      -0.0670385
_diffrn_orient_matrix_UB_21      -0.0993537
_diffrn_orient_matrix_UB_22      0.0079713
_diffrn_orient_matrix_UB_23      0.006627
_diffrn_orient_matrix_UB_31      0.0082294
_diffrn_orient_matrix_UB_32      0.0427129
_diffrn_orient_matrix_UB_33      -0.0308321
_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  0.0327
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            102249
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.765
_diffrn_reflns_theta_min         2.716
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.68994
_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            red
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       block
_exptl_crystal_F_000             3952
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         10477
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.036
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+7.1253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0
_reflns_number_gt                9827
_reflns_number_total             10477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00069a2.cif
_cod_data_source_block           21EH165_AMB-558
_cod_depositor_comments
'Adding full bibliography for 7712094--7712100.cif.'
_cod_original_cell_volume        10217.16(8)
_cod_database_code               7712094
_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 1.4
_oxdiff_exptl_absorpt_empirical_full_min 0.76
_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
 At 1.5 times of:
  All C(H,H,H) groups
        2. Uiso/Uaniso restraints and constraints
Uanis(C27A) \\sim Ueq, Uanis(C24A) \\sim Ueq: with sigma of 0.01 and sigma for
        terminal atoms of 0.02
Uanis(C26A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C51A) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52A) \\sim Ueq: with sigma
        of 0.01 and sigma for terminal atoms of 0.02
Uanis(C53A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
        3. Others
 Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C27A)=
 Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(O2A)=
 1-FVAR(1)
 Sof(O2)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(1)
 Sof(O4A)=Sof(C54A)=Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(C52A)=Sof(H52D)=
 Sof(H52E)=Sof(H52F)=Sof(C53A)=Sof(H53C)=Sof(H53D)=Sof(C51A)=Sof(H51C)=
 Sof(H51D)=1-FVAR(2)
 Sof(O4)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=
 Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(2)
 Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C47A)=Sof(H47C)=Sof(H47D)=
 Sof(O3A)=Sof(C49A)=Sof(H49C)=Sof(H49D)=Sof(C50A)=Sof(H50D)=Sof(H50E)=Sof(H50F)=
 1-FVAR(3)
 Sof(O3)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C47)=Sof(H47A)=Sof(H47B)=
 Sof(C49)=Sof(H49B)=Sof(H49A)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(3)
        4.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C26(H26A,H26B), C22(H22A,H22B), C47(H47A,H47B), C20(H20A,
 H20B), C49(H49B,H49A), C53(H53A,H53B), C51(H51A,H51B), C53A(H53C,H53D),
 C51A(H51C,H51D), C26A(H26C,H26D), C24A(H24C,H24D), C47A(H47C,H47D), C49A(H49C,
 H49D)
        4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C9(H9), C19(H19), C3(H3), C15(H15), C6(H6), C42(H42),
 C36(H36), C46(H46), C34(H34), C12(H12), C10(H10), C5(H5), C11(H11), C16(H16),
 C4(H4), C17(H17), C30(H30), C40(H40), C37(H37), C18(H18), C32(H32), C38(H38),
 C33(H33), C43(H43), C39(H39), C45(H45), C44(H44), C31(H31)
        4.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C50(H50A,H50B,
 H50C), C21(H21A,H21B,H21C), C48(H48A,H48B,H48C), C52(H52A,H52B,H52C), C54(H54A,
 H54B,H54C), C54A(H54D,H54E,H54F), C52A(H52D,H52E,H52F), C27A(H27D,H27E,H27F),
 C25A(H25D,H25E,H25F), C48A(H48D,H48E,H48F), C50A(H50D,H50E,H50F)
;
_shelx_res_checksum              37226