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_7712099
_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         'C42 H50 Li2 Ni O4'
_chemical_formula_sum            'C42 H50 Li2 Ni O4'
_chemical_formula_weight         691.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-06-24
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_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                   15.49117(5)
_cell_length_b                   19.31164(7)
_cell_length_c                   24.55861(9)
_cell_measurement_reflns_used    53769
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      79.8310
_cell_measurement_theta_min      3.3370
_cell_volume                     7346.95(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -79.00 -20.00   0.50    0.25    --  -23.00 140.00 102.00  118
  2  \w    -72.00 -14.00   0.50    0.25    --  -23.00 129.00 -70.00  116
  3  \w    -70.00 -12.00   0.50    0.25    --  -23.00 125.00-120.00  116
  4  \w    -70.00 -12.00   0.50    0.25    --  -23.00 125.00  60.00  116
  5  \w    -70.00 -12.00   0.50    0.25    --  -23.00 125.00  30.00  116
  6  \w    -26.00  23.00   0.50    0.25    --   47.92 -19.00 -60.00   98
  7  \w    -26.00  23.00   0.50    0.25    --   47.92 -19.00  30.00   98
  8  \w    -25.00  40.00   0.50    0.25    --   47.92 -38.00-180.00  130
  9  \w    101.00 177.00   0.50    1.00    --  113.25  45.00 -30.00  152
 10  \w     42.00  68.00   0.50    1.00    --  113.25 -61.00 -90.00   52
 11  \w     42.00  68.00   0.50    1.00    --  113.25 -61.00 -60.00   52
 12  \w     42.00  68.00   0.50    1.00    --  113.25 -61.00 150.00   52
 13  \w    101.00 177.00   0.50    1.00    --  113.25  30.00-150.00  152
 14  \w     42.00  68.00   0.50    1.00    --  113.25 -61.00   0.00   52
 15  \w     42.00  68.00   0.50    1.00    --  113.25 -61.00  90.00   52
 16  \w     42.00  68.00   0.50    1.00    --  113.25 -61.00  30.00   52
 17  \w     42.00  68.00   0.50    1.00    --  113.25 -61.00 120.00   52
 18  \w    100.00 177.00   0.50    1.00    --  113.25  15.00   0.00  154
 19  \w     42.00 102.00   0.50    1.00    --  113.25 -77.00 120.00  120
 20  \w     42.00  68.00   0.50    1.00    --  113.25 -61.00 -30.00   52
 21  \w     42.00 102.00   0.50    1.00    --  113.25 -77.00  90.00  120
 22  \w     97.00 177.00   0.50    1.00    --  113.25  61.00 120.00  160
 23  \w    101.00 177.00   0.50    1.00    --  113.25  45.00 -90.00  152
 24  \w    100.00 177.00   0.50    1.00    --  113.25  15.00 -90.00  154
 25  \w     42.00 106.00   0.50    1.00    --  113.25 -94.00  60.00  128
 26  \w     42.00 106.00   0.50    1.00    --  113.25 -94.00  90.00  128
 27  \w     42.00 102.00   0.50    1.00    --  113.25 -77.00 -90.00  120
 28  \w    101.00 177.00   0.50    1.00    --  113.25  45.00-180.00  152
 29  \w     25.00  68.00   0.50    0.25    --   47.92  77.00 -60.00   86
 30  \w     33.00 120.00   0.50    0.25    --   47.92  57.00  90.00  174
;
_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      0.0602698000
_diffrn_orient_matrix_UB_12      -0.0592178000
_diffrn_orient_matrix_UB_13      0.0178872000
_diffrn_orient_matrix_UB_21      -0.0149929000
_diffrn_orient_matrix_UB_22      0.0195603000
_diffrn_orient_matrix_UB_23      0.0600849000
_diffrn_orient_matrix_UB_31      -0.0776761000
_diffrn_orient_matrix_UB_32      -0.0497296000
_diffrn_orient_matrix_UB_33      0.0023327000
_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  0.0302
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            72965
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.502
_diffrn_reflns_theta_min         3.600
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.067
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.508
_exptl_crystal_size_mid          0.423
_exptl_crystal_size_min          0.186
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.00017(2)
_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    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         7508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+4.2926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7241
_reflns_number_total             7508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00069a2.cif
_cod_data_source_block           22EH076_AMB-840
_cod_depositor_comments
'Adding full bibliography for 7712094--7712100.cif.'
_cod_original_cell_volume        7346.96(5)
_cod_database_code               7712099
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C34H34Li2Ni1O2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C36(H36A,H36B), C42(H42A,H42B)
;
_shelx_res_checksum              58719
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.532
_oxdiff_exptl_absorpt_empirical_full_min 0.795