The coordination of alkali-metal nickelates to organic π-systems: synthetic, structural and spectroscopic insights.
Borys, Andryj M.; Vedani, Luca; Hevia, Eva; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8382–8390; doi:10.1039/d4dt00889h

data_7715645
_publ_section_title
;
 The coordination of alkali-metal nickelates to organic &#x3c0;-systems:
 synthetic, structural and spectroscopic insights.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8382
_journal_page_last               8390
_journal_paper_doi               10.1039/d4dt00889h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C16 H40 K O8, C20 H12'
_chemical_formula_sum            'C36 H52 K O8'
_chemical_formula_weight         651.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-17 deposited with the CCDC.	2024-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.5740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.11620(10)
_cell_length_b                   13.75360(10)
_cell_length_c                   11.45110(10)
_cell_measurement_reflns_used    25110
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      79.8500
_cell_measurement_theta_min      3.7450
_cell_volume                     3616.72(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(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 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    -45.00  21.00   0.50    0.50    --  -50.24  40.00  61.00  132
  2  \w   -122.00 -44.00   0.50    0.50    --  -50.24 -40.00 -91.00  156
  3  \w    -20.00  45.00   0.50    0.50    --   50.24 -40.00 -91.00  130
  4  \w     44.00 122.00   0.50    0.50    --   50.24  40.00  61.00  156
  5  \w    -45.00 -18.00   0.50    2.00    --  -90.00  40.00  61.00   54
  6  \w   -160.00 -84.00   0.50    2.00    --  -90.00 -40.00 -91.00  152
  7  \w    105.00 178.00   0.50    2.00    --  111.50  40.00  61.00  146
  8  \w   -121.00 -44.00   0.50    0.50    --  -50.24 -38.00 120.00  154
  9  \w    -86.00 -13.00   0.50    0.50    --  -50.24 125.00 -90.00  146
 10  \w    -26.00  22.00   0.50    0.50    --  -50.24  19.00  90.00   96
 11  \w     -1.00  79.00   0.50    0.50    --   50.24 -99.00 -90.00  160
 12  \w    -21.00  26.00   0.50    0.50    --   50.24 -19.00-180.00   94
 13  \w     34.00  93.00   0.50    0.50    --   50.24-125.00-120.00  118
 14  \w   -138.00 -83.00   0.50    2.00    --  -90.00   0.00 150.00  110
 15  \w    -85.00 -21.00   0.50    2.00    --  -90.00 125.00 120.00  128
 16  \w     63.00 118.00   0.50    2.00    --  111.50   0.00  30.00  110
 17  \w     48.00 131.00   0.50    2.00    --  111.50-152.00 154.07  166
 18  \w     41.00 106.00   0.50    2.00    --  111.50 -94.00 -60.00  130
 19  \w     43.00 111.00   0.50    2.00    --  111.50-125.00  30.00  136
 20  \w    108.00 178.00   0.50    2.00    --  111.50  30.00  90.00  140
 21  \w     92.00 178.00   0.50    2.00    --  111.50  77.00 -30.00  172
 22  \w     41.00  71.00   0.50    2.00    --  111.50 -61.00-150.00   60
 23  \w     41.00 105.00   0.50    2.00    --  111.50 -77.00-180.00  128
 24  \w     43.00 111.00   0.50    2.00    --  111.50-125.00-120.00  136
 25  \w     41.00  71.00   0.50    2.00    --  111.50 -61.00  90.00   60
 26  \w     43.00 111.00   0.50    2.00    --  111.50-125.00 150.00  136
 27  \w    101.00 178.00   0.50    2.00    --  111.50  55.00 -44.11  154
 28  \w     63.00 118.00   0.50    2.00    --  111.50   0.00 -60.00  110
 29  \w     98.00 178.00   0.50    2.00    --  111.50  61.00   0.00  160
 30  \w     42.00 116.00   0.50    2.00    --  111.50-131.00  58.04  148
 31  \w    104.00 178.00   0.50    2.00    --  111.50  45.00 -90.00  148
 32  \w     42.00 107.00   0.50    2.00    --  111.50-104.00 -84.24  130
 33  \w     95.00 178.00   0.50    2.00    --  111.50 125.00  30.00  166
 34  \w     43.00 111.00   0.50    2.00    --  111.50-125.00   0.00  136
 35  \w     92.00 178.00   0.50    2.00    --  111.50  77.00-150.00  172
 36  \w     41.00  71.00   0.50    2.00    --  111.50 -61.00-120.00   60
 37  \w     61.00  86.00   0.50    2.00    --  111.50-149.00 -54.82   50
 38  \w     72.00 110.00   0.50    2.00    --  111.50-125.00-150.00   76
 39  \w    103.00 129.00   0.50    2.00    --  111.50-149.00 -54.82   52
 40  \w     76.00 110.00   0.50    2.00    --  111.50   0.00-120.00   68
 41  \w    102.00 173.00   0.50    2.00    --  111.50  61.00-120.00  142
 42  \w    110.00 177.00   0.50    2.00    --  111.50 125.00 -30.00  134
 43  \w     45.00  71.00   0.50    2.00    --  111.50-125.00-150.00   52
 44  \w     43.00  80.00   0.50    2.00    --  111.50-106.00 169.55   74
 45  \w     83.00 108.00   0.50    2.00    --  111.50-106.00 169.55   50
 46  \w     44.00  83.00   0.50    2.00    --  111.50-125.00-180.00   78
 47  \w     61.00 101.00   0.50    2.00    --  111.50 -94.00  30.00   80
 48  \w     44.00  69.00   0.50    2.00    --  111.50 -61.00  30.00   50
 49  \w     52.00  79.00   0.50    2.00    --  111.50-146.00-151.21   54
 50  \w     97.00 126.00   0.50    2.00    --  111.50-146.00-151.21   58
 51  \w    131.00 170.00   0.50    2.00    --  111.50 125.00  90.00   78
 52  \w     65.00  91.00   0.50    2.00    --  111.50 -77.00-150.00   52
 53  \w    118.00 145.00   0.50    2.00    --  111.50  30.00  30.00   54
 54  \w     61.00 108.00   0.50    2.00    --  111.50-106.00-113.12   94
;
_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      -0.0331722000
_diffrn_orient_matrix_UB_12      -0.0488575000
_diffrn_orient_matrix_UB_13      0.0935314000
_diffrn_orient_matrix_UB_21      0.0088581000
_diffrn_orient_matrix_UB_22      -0.1000348000
_diffrn_orient_matrix_UB_23      -0.0558847000
_diffrn_orient_matrix_UB_31      0.0576066000
_diffrn_orient_matrix_UB_32      -0.0127707000
_diffrn_orient_matrix_UB_33      0.0803909000
_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  0.0296
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            36959
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.497
_diffrn_reflns_theta_min         3.746
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.670
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         3694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+1.6708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3548
_reflns_number_total             3694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00889h2.cif
_cod_data_source_block           23eh320_absorption
_cod_depositor_comments
'Adding full bibliography for 7715639--7715655.cif.'
_cod_database_code               7715645
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C144  H200  K4  O32  '
_shelx_estimated_absorpt_t_max   0.839
_shelx_estimated_absorpt_t_min   0.766
_olex2_refinement_description
;
;
_shelx_res_checksum              35716
_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 1.116
_oxdiff_exptl_absorpt_empirical_full_min 0.890