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_7712100
_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         'C70 H102 Li4 Ni2 O4'
_chemical_formula_sum            'C70 H102 Li4 Ni2 O4'
_chemical_formula_weight         1152.69
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-12T17:27:44-00:00
_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
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.16221(10)
_cell_length_b                   28.5694(3)
_cell_length_c                   42.1061(3)
_cell_measurement_reflns_used    62654
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      79.732
_cell_measurement_theta_min      3.237
_cell_volume                     14630.5(2)
_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    -77.00 -19.00   0.50    1.30    --  -23.00 137.00-137.00  116
  2  \w    -74.00 -16.00   0.50    1.30    --  -23.00 132.00  45.00  116
  3  \w    -95.00   0.00   0.50    1.30    --  -23.00 -77.00 -30.00  190
  4  \w    -24.00  71.00   0.50    1.30    --   47.92 -77.00-120.00  190
  5  \w     36.00 121.00   0.50    1.30    --   47.92  38.00-180.00  170
  6  \w    -23.00  63.00   0.50    1.30    --   47.92 -57.00 -90.00  172
  7  \w    100.00 177.00   0.50    8.00    --  113.25  15.00 -60.00  154
  8  \w    101.00 177.00   0.50    8.00    --  113.25  30.00   0.00  152
  9  \w    100.00 177.00   0.50    8.00    --  113.25  15.00-120.00  154
 10  \w     42.00 102.00   0.50    8.00    --  113.25 -77.00  60.00  120
 11  \w     42.00 106.00   0.50    8.00    --  113.25 -94.00 -90.00  128
 12  \w     42.00 106.00   0.50    8.00    --  113.25 -94.00 -60.00  128
 13  \w     42.00 106.00   0.50    8.00    --  113.25 -94.00-120.00  128
 14  \w     42.00 106.00   0.50    8.00    --  113.25 -94.00   0.00  128
 15  \w     42.00  68.00   0.50    8.00    --  113.25 -61.00 -30.00   52
 16  \w    101.00 177.00   0.50    8.00    --  113.25  45.00  60.00  152
 17  \w     42.00  68.00   0.50    8.00    --  113.25 -61.00   0.00   52
 18  \w     42.00 106.00   0.50    8.00    --  113.25 -94.00-150.00  128
 19  \w     42.00  68.00   0.50    8.00    --  113.25 -61.00-150.00   52
 20  \w     42.00  68.00   0.50    8.00    --  113.25 -61.00 -60.00   52
 21  \w    101.00 177.00   0.50    8.00    --  113.25  45.00 150.00  152
 22  \w     42.00 106.00   0.50    8.00    --  113.25 -94.00 -30.00  128
 23  \w     42.00 102.00   0.50    8.00    --  113.25 -77.00 120.00  120
 24  \w     91.00 177.00   0.50    8.00    --  113.25  77.00 -60.00  172
 25  \w     33.00 112.00   0.50    1.30    --   47.92  57.00-120.00  158
;
_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      -0.0037729
_diffrn_orient_matrix_UB_12      0.0101747
_diffrn_orient_matrix_UB_13      -0.0359112
_diffrn_orient_matrix_UB_21      0.0069789
_diffrn_orient_matrix_UB_22      -0.052839
_diffrn_orient_matrix_UB_23      -0.0069492
_diffrn_orient_matrix_UB_31      -0.1265143
_diffrn_orient_matrix_UB_32      -0.0032186
_diffrn_orient_matrix_UB_33      0.0006973
_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  0.0576
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            133411
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        66.915
_diffrn_reflns_theta_max         66.915
_diffrn_reflns_theta_min         3.094
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.59026
_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    1.047
_exptl_crystal_description       plate
_exptl_crystal_F_000             4976
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.305
_exptl_crystal_size_min          0.141
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         13013
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+14.3839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0
_reflns_number_gt                11762
_reflns_number_total             13013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00069a2.cif
_cod_data_source_block           22EH046_AMB-765
_cod_depositor_comments
'Adding full bibliography for 7712094--7712100.cif.'
_cod_database_code               7712100
_shelx_estimated_absorpt_t_min   0.715
_shelx_estimated_absorpt_t_max   0.879
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.689
_oxdiff_exptl_absorpt_empirical_full_min 0.586
_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(C43) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
        3.a Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B), C63(H63A,H63B), C69(H69A,H69B), C59(H59A,H59B), C55(H55A,
 H55B), C57(H57A,H57B), C65(H65A,H65B), C61(H61A,H61B)
        3.b Aromatic/amide H refined with riding coordinates:
 C46(H46), C26(H26), C49(H49), C29(H29), C47(H47), C19(H19), C20(H20),
 C27(H27), C50(H50), C30(H30), C16(H16), C39(H39), C40(H40), C17(H17), C36(H36),
  C37(H37), C4(H4), C14(H14), C10(H10), C6(H6), C8(H8), C5(H5), C11(H11),
 C12(H12), C7(H7), C13(H13)
        3.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C33(H33A,H33B,H33C), C32(H32A,H32B,
 H32C), C34(H34A,H34B,H34C), C54(H54A,H54B,H54C), C53(H53A,H53B,H53C), C52(H52A,
 H52B,H52C), C68(H68A,H68B,H68C), C22(H22A,H22B,H22C), C42(H42A,H42B,H42C),
 C58(H58A,H58B,H58C), C44(H44A,H44B,H44C), C64(H64A,H64B,H64C), C56(H56A,H56B,
 H56C), C60(H60A,H60B,H60C), C70(H70A,H70B,H70C), C66(H66A,H66B,H66C), C43(H43A,
 H43B,H43C), C62(H62A,H62B,H62C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2870
_shelx_fab_checksum              88513