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_7712098
_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         'C62 H78 Na4 Ni2 O6'
_chemical_formula_sum            'C62 H78 Na4 Ni2 O6'
_chemical_formula_weight         1128.62
_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             2022-02-18T11:25:28-00:00
_audit_update_record
;
2022-11-22 deposited with the CCDC.	2023-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.2810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9102(2)
_cell_length_b                   17.56450(10)
_cell_length_c                   16.23570(10)
_cell_measurement_reflns_used    27609
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      78.655
_cell_measurement_theta_min      3.279
_cell_volume                     5962.93(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 0.999
_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    -32.00  52.00   0.50    0.40    --  -23.00  23.00 134.00  168
  2  \w    -97.00 -10.00   0.50    0.40    --  -23.00 -23.00 -30.00  174
  3  \w    -26.00  26.00   0.50    0.40    --   47.92 -23.00 -30.00  104
  4  \w     36.00 122.00   0.50    0.40    --   47.92  23.00 134.00  172
  5  \w    101.00 177.00   0.50    5.00    --  113.25  23.00 134.00  152
  6  \w    -70.00 -12.00   0.50    0.40    --  -23.00 125.00 -90.00  116
  7  \w    -30.00  53.00   0.50    0.40    --  -23.00  19.00 120.00  166
  8  \w    -70.00 -12.00   0.50    0.40    --  -23.00 125.00 150.00  116
  9  \w    -36.00  49.00   0.50    0.40    --  -23.00  45.00-150.00  170
 10  \w     25.00 121.00   0.50    0.40    --   47.92  77.00-150.00  192
 11  \w     25.00 121.00   0.50    0.40    --   47.92  77.00 -90.00  192
 12  \w     33.00 120.00   0.50    0.40    --   47.92  57.00-150.00  174
 13  \w     25.00 121.00   0.50    0.40    --   47.92  77.00-120.00  192
 14  \w    -25.00  40.00   0.50    0.40    --   47.92 -38.00-150.00  130
 15  \w     42.00  68.00   0.50    5.00    --  113.25 -61.00   0.00   52
 16  \w     42.00  68.00   0.50    5.00    --  113.25 -61.00 -60.00   52
 17  \w     42.00 106.00   0.50    5.00    --  113.25 -94.00 -60.00  128
 18  \w     91.00 177.00   0.50    5.00    --  113.25  77.00-150.00  172
 19  \w    100.00 177.00   0.50    5.00    --  113.25  51.00 -73.48  154
 20  \w     42.00  68.00   0.50    5.00    --  113.25 -61.00 -30.00   52
 21  \w     42.00 102.00   0.50    5.00    --  113.25 -77.00   0.00  120
 22  \w     91.00 177.00   0.50    5.00    --  113.25  77.00 150.00  172
 23  \w     42.00 106.00   0.50    5.00    --  113.25 -94.00-120.00  128
 24  \w    101.00 177.00   0.50    5.00    --  113.25  30.00 -90.00  152
 25  \w     97.00 122.00   0.50    5.00    --  113.25  61.00-120.00   50
 26  \w    101.00 133.00   0.50    5.00    --  113.25  30.00 -60.00   64
 27  \w     97.00 123.00   0.50    5.00    --  113.25  61.00-150.00   52
 28  \w     97.00 122.00   0.50    5.00    --  113.25  61.00 -60.00   50
 29  \w    152.00 177.00   0.50    5.00    --  113.25  61.00 -60.00   50
 30  \w    101.00 134.00   0.50    5.00    --  113.25  45.00 -60.00   66
 31  \w     91.00 117.00   0.50    5.00    --  113.25  77.00 -90.00   52
 32  \w    141.00 167.00   0.50    5.00    --  113.25  77.00 -90.00   52
 33  \w     97.00 122.00   0.50    5.00    --  113.25  61.00-180.00   50
 34  \w     42.00  67.00   0.50    5.00    --  113.25 -61.00-180.00   50
 35  \w    141.00 167.00   0.50    5.00    --  113.25  77.00-180.00   52
 36  \w     43.00  92.00   0.50    5.00    --  113.25 -77.00  90.00   98
 37  \w     91.00 117.00   0.50    5.00    --  113.25  77.00-180.00   52
 38  \w     43.00  68.00   0.50    5.00    --  113.25 -61.00  90.00   50
 39  \w     48.00 102.00   0.50    5.00    --  113.25 -77.00  30.00  108
 40  \w     91.00 116.00   0.50    5.00    --  113.25  77.00-120.00   50
 41  \w    142.00 174.00   0.50    5.00    --  113.25  77.00-120.00   64
 42  \w    105.00 131.00   0.50    5.00    --  113.25  45.00 150.00   52
 43  \w    139.00 168.00   0.50    5.00    --  113.25  45.00 150.00   58
 44  \w     95.00 121.00   0.50    5.00    --  113.25  65.00 154.14   52
 45  \w    128.00 154.00   0.50    5.00    --  113.25  65.00 154.14   52
 46  \w     80.00 105.00   0.50    5.00    --  113.25 -94.00-150.00   50
 47  \w    103.00 129.00   0.50    5.00    --  113.25  45.00 -90.00   52
 48  \w    102.00 166.00   0.50    5.00    --  113.25  45.00-150.00  128
 49  \w    101.00 126.00   0.50    5.00    --  113.25  45.00-120.00   50
 50  \w     45.00  73.00   0.50    5.00    --  113.25 -94.00-150.00   56
 51  \w    101.00 141.00   0.50    5.00    --  113.25  45.00  60.00   80
 52  \w    101.00 128.00   0.50    5.00    --  113.25  30.00-180.00   54
 53  \w     45.00 102.00   0.50    5.00    --  113.25 -94.00-180.00  114
 54  \w    101.00 147.00   0.50    5.00    --  113.25  45.00-180.00   92
 55  \w    102.00 177.00   0.50    5.00    --  113.25  30.00-120.00  150
 56  \w     42.00  67.00   0.50    5.00    --  113.25 -61.00 -90.00   50
 57  \w     98.00 124.00   0.50    5.00    --  113.25  61.00 -90.00   52
 58  \w     50.00 101.00   0.50    5.00    --  113.25 -77.00-120.00  102
 59  \w    140.00 175.00   0.50    5.00    --  113.25  45.00 -60.00   70
 60  \w     97.00 123.00   0.50    5.00    --  113.25  61.00 150.00   52
 61  \w     46.00  72.00   0.50    5.00    --  113.25 -77.00-150.00   52
 62  \w     43.00  68.00   0.50    5.00    --  113.25 -61.00 120.00   50
 63  \w     91.00 118.00   0.50    5.00    --  113.25  77.00 -60.00   54
 64  \w    101.00 154.00   0.50    5.00    --  113.25  30.00-150.00  106
 65  \w     45.00 104.00   0.50    5.00    --  113.25 -94.00  90.00  118
;
_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      -0.0137419
_diffrn_orient_matrix_UB_12      0.0494981
_diffrn_orient_matrix_UB_13      -0.0764084
_diffrn_orient_matrix_UB_21      -0.0178382
_diffrn_orient_matrix_UB_22      0.0673094
_diffrn_orient_matrix_UB_23      0.0562583
_diffrn_orient_matrix_UB_31      0.0701468
_diffrn_orient_matrix_UB_32      0.0267921
_diffrn_orient_matrix_UB_33      -0.0002144
_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  0.0402
_diffrn_reflns_av_unetI/netI     0.016
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57329
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.266
_diffrn_reflns_theta_min         3.286
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.444
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.84128
_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            colourless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       plate
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         5979
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0665
_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^)+(0.1124P)^2^+4.4521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2015
_refine_ls_wR_factor_ref         0.2093
_reflns_Friedel_coverage         0
_reflns_number_gt                5187
_reflns_number_total             5979
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 7.0987\% 
around [-0.76 0.65 0.04] (reciprocal) or [-0.64 0.77 0.05] (direct)
Component 3 rotated by -174.2847\% 
around [0.08 1.00 0.01] (reciprocal) or [0.05 1.00 0.02] (direct)
Component 4 rotated by 26.2662\% 
around [-0.26 0.97 -0.02] (reciprocal) or [-0.19 0.98 -0.02] (direct)
;
_cod_data_source_file            d3dt00069a2.cif
_cod_data_source_block           22EH016_AMB-720
_cod_depositor_comments
'Adding full bibliography for 7712094--7712100.cif.'
_cod_database_code               7712098
_shelx_estimated_absorpt_t_min   0.59
_shelx_estimated_absorpt_t_max   0.892
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.751
_oxdiff_exptl_absorpt_empirical_full_min 0.45
_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. Restrained distances
 C26A-C25A = C25-C26
 1.54 with sigma of 0.01
 C28A-C29A
 1.53 with sigma of 0.01
 C24A-C25A
 1.53 with sigma of 0.01
 C26-C27
 1.53 with sigma of 0.01
 C26-C25 \\sim C26A-C25A
 with sigma of 0.002
 C22-C21A \\sim C22-C21
 with sigma of 0.002
        3. Rigid bond restraints
 C23A, C21A, C20A, C22, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C25A, C26A, C27A, O0, C24A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C8, C9, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1, C23, C22, C21, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C13A, C12A, C11A, C10A, C9A, C8A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C25, C24, O2, C27, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C28, C29, C30, C31, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O4, C31A, C30A, C29A, C28A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C18, C17, C16, C15, C14, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
        4. Uiso/Uaniso restraints and constraints
Uanis(C20A) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C23)
\\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C4A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C2A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.02 and sigma for
        terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10A) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C12A)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C25) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C28A) \\sim Ueq, Uanis(C30A) \\sim Ueq: with sigma of 0.02 and
        sigma for terminal atoms of 0.02
Uanis(C1D) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
        terminal atoms of 0.02
        5. Others
 Sof(C8A)=Sof(C13A)=Sof(H13A)=Sof(C12A)=Sof(H12A)=Sof(C11A)=Sof(H11A)=
 Sof(C10A)=Sof(H10A)=Sof(C9A)=Sof(H9A)=1-FVAR(1)
 Sof(C8)=Sof(C13)=Sof(H13)=Sof(C10)=Sof(H10)=Sof(C9)=Sof(H9)=Sof(C11)=Sof(H11)=
 Sof(C12)=Sof(H12)=FVAR(1)
 Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C25A)=
 Sof(H25C)=Sof(H25D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(O0)=1-FVAR(2)
 Sof(O2)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C26)=
 Sof(H26A)=Sof(H26B)=Sof(C25)=Sof(H25A)=Sof(H25B)=FVAR(2)
 Sof(H22C)=Sof(H22D)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21C)=
 Sof(H21D)=Sof(C23A)=Sof(H23C)=Sof(H23D)=1-FVAR(3)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H22A)=Sof(H22B)=Sof(C21)=Sof(H21A)=Sof(H21B)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=FVAR(3)
 Sof(C31A)=Sof(H31C)=Sof(H31D)=Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=
 Sof(H30C)=Sof(H30D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(O4)=1-FVAR(4)
 Sof(O3)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=
 Sof(H30A)=Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(H31B)=FVAR(4)
 Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=
 Sof(C7A)=Sof(H7A)=Sof(C2A)=Sof(C1D)=1-FVAR(5)
 Sof(C2)=Sof(C7)=Sof(H7)=Sof(C6)=Sof(H6)=Sof(C5)=Sof(H5)=Sof(C4)=Sof(H4)=
 Sof(C3)=Sof(H3)=Sof(C1)=FVAR(5)
        6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C24(H24A,H24B), C27(H27A,H27B), C22(H22A,H22B), C22(H22C,
 H22D), C21(H21A,H21B), C28(H28A,H28B), C23(H23A,H23B), C29(H29A,H29B),
 C26(H26A,H26B), C25(H25A,H25B), C30(H30A,H30B), C31(H31A,H31B), C27A(H27C,
 H27D), C26A(H26C,H26D), C25A(H25C,H25D), C24A(H24C,H24D), C20A(H20C,H20D),
 C21A(H21C,H21D), C23A(H23C,H23D), C31A(H31C,H31D), C29A(H29C,H29D), C30A(H30C,
 H30D), C28A(H28C,H28D)
        6.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C7(H7), C6(H6), C5(H5), C4(H4), C3(H3), C19(H19), C16(H16),
 C13(H13), C10(H10), C17(H17), C18(H18), C9(H9), C11(H11), C12(H12), C13A(H13A),
  C12A(H12A), C11A(H11A), C10A(H10A), C9A(H9A), C3A(H3A), C4A(H4A), C5A(H5A),
 C6A(H6A), C7A(H7A)
        6.c Fitted hexagon refined as free rotating group:
 C2(C7,C6,C5,C4,C3), C3A(C4A,C5A,C6A,C7A,C2A)
;
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               4
_shelx_res_checksum              77246