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_7712095
_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         'C38 H48 Li2 Ni O2'
_chemical_formula_sum            'C38 H48 Li2 Ni O2'
_chemical_formula_weight         609.35
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-12T21:59:33-00:00
_audit_update_record
;
2022-11-22 deposited with the CCDC.	2023-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.1129(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.30135(14)
_cell_length_b                   14.29224(10)
_cell_length_c                   15.04570(13)
_cell_measurement_reflns_used    53293
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      79.852
_cell_measurement_theta_min      3.107
_cell_volume                     3368.75(5)
_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    -56.00  27.00   0.50    0.25    --  -23.00  98.00 -74.00  166
  2  \w     -5.00  81.00   0.50    0.25    --   47.92 -98.00 178.00  172
  3  \w     42.00 106.00   0.50    0.80    --  113.25 -98.00 178.00  128
  4  \w    106.00 177.00   0.50    0.80    --  113.25  98.00 -74.00  142
  5  \w    -70.00 -12.00   0.50    0.25    --  -23.00 125.00  30.00  116
  6  \w    -28.00  52.00   0.50    0.25    --  -23.00  15.00-180.00  160
  7  \w    -97.00 -10.00   0.50    0.25    --  -23.00 -30.00  90.00  174
  8  \w    -70.00 -12.00   0.50    0.25    --  -23.00 125.00 -60.00  116
  9  \w    -70.00 -12.00   0.50    0.25    --  -23.00 125.00  90.00  116
 10  \w    -26.00  23.00   0.50    0.25    --   47.92 -19.00 -90.00   98
 11  \w    -25.00  40.00   0.50    0.25    --   47.92 -38.00-180.00  130
 12  \w    -26.00  23.00   0.50    0.25    --   47.92 -19.00-120.00   98
 13  \w     25.00 121.00   0.50    0.25    --   47.92  77.00-150.00  192
 14  \w    -26.00  23.00   0.50    0.25    --   47.92 -19.00-150.00   98
 15  \w     42.00  68.00   0.50    0.80    --  113.25 -61.00 150.00   52
 16  \w     97.00 177.00   0.50    0.80    --  113.25  61.00   0.00  160
 17  \w     91.00 177.00   0.50    0.80    --  113.25  77.00 -30.00  172
 18  \w     42.00  68.00   0.50    0.80    --  113.25 -61.00-150.00   52
 19  \w     42.00 106.00   0.50    0.80    --  113.25 -94.00 120.00  128
 20  \w     42.00  68.00   0.50    0.80    --  113.25 -61.00   0.00   52
 21  \w     42.00  68.00   0.50    0.80    --  113.25 -61.00  30.00   52
 22  \w     97.00 177.00   0.50    0.80    --  113.25  61.00 120.00  160
 23  \w     42.00 106.00   0.50    0.80    --  113.25 -94.00  60.00  128
 24  \w     91.00 177.00   0.50    0.80    --  113.25  77.00  30.00  172
 25  \w     42.00 102.00   0.50    0.80    --  113.25 -77.00-150.00  120
 26  \w     42.00 102.00   0.50    0.80    --  113.25 -77.00  90.00  120
 27  \w     42.00 106.00   0.50    0.80    --  113.25 -94.00   0.00  128
 28  \w     91.00 177.00   0.50    0.80    --  113.25  77.00-150.00  172
 29  \w     42.00 102.00   0.50    0.80    --  113.25 -77.00  60.00  120
 30  \w     42.00 102.00   0.50    0.80    --  113.25 -77.00 -90.00  120
 31  \w     42.00 106.00   0.50    0.80    --  113.25 -94.00-120.00  128
 32  \w     97.00 177.00   0.50    0.80    --  113.25  61.00-120.00  160
 33  \w     42.00  68.00   0.50    0.80    --  113.25 -61.00 -90.00   52
 34  \w     42.00 106.00   0.50    0.80    --  113.25 -94.00 -60.00  128
 35  \w     97.00 177.00   0.50    0.80    --  113.25  61.00 150.00  160
 36  \w     42.00 106.00   0.50    0.80    --  113.25 -94.00-150.00  128
 37  \w    101.00 177.00   0.50    0.80    --  113.25  45.00 -90.00  152
 38  \w     42.00 106.00   0.50    0.80    --  113.25 -94.00 150.00  128
 39  \w     91.00 177.00   0.50    0.80    --  113.25  77.00  90.00  172
 40  \w     42.00 102.00   0.50    0.80    --  113.25 -77.00-180.00  120
 41  \w     42.00 102.00   0.50    0.80    --  113.25 -77.00-120.00  120
 42  \w    100.00 177.00   0.50    0.80    --  113.25  15.00  30.00  154
 43  \w     42.00 102.00   0.50    0.80    --  113.25 -77.00 -60.00  120
 44  \w     42.00 106.00   0.50    0.80    --  113.25 -94.00 -30.00  128
 45  \w     42.00 106.00   0.50    0.80    --  113.25 -94.00 -90.00  128
 46  \w     42.00  68.00   0.50    0.80    --  113.25 -61.00 -60.00   52
 47  \w     42.00 102.00   0.50    0.80    --  113.25 -77.00 120.00  120
 48  \w     97.00 177.00   0.50    0.80    --  113.25  61.00  60.00  160
 49  \w    112.00 160.00   0.50    0.80    --  113.25   0.00  90.00   96
 50  \w     42.00  67.00   0.50    0.80    --  113.25 -61.00 -30.00   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      -0.0081196
_diffrn_orient_matrix_UB_12      0.0625885
_diffrn_orient_matrix_UB_13      0.0788995
_diffrn_orient_matrix_UB_21      0.0447594
_diffrn_orient_matrix_UB_22      0.0803146
_diffrn_orient_matrix_UB_23      -0.0281161
_diffrn_orient_matrix_UB_31      -0.0871914
_diffrn_orient_matrix_UB_32      0.035364
_diffrn_orient_matrix_UB_33      -0.0760344
_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  0.0323
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            67317
_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         74.756
_diffrn_reflns_theta_min         2.821
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.80397
_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            'dark red'
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.176
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.00051(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         6899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.03
_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^)+(0.0385P)^2^+1.2158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0
_reflns_number_gt                6758
_reflns_number_total             6899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00069a2.cif
_cod_data_source_block           22EH042_AMB-763
_cod_depositor_comments
'Adding full bibliography for 7712094--7712100.cif.'
_cod_original_cell_volume        3368.74(5)
_cod_database_code               7712095
_shelx_estimated_absorpt_t_min   0.717
_shelx_estimated_absorpt_t_max   0.834
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.655
_oxdiff_exptl_absorpt_empirical_full_min 0.737
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
;
_shelx_res_checksum              25041