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_7715643
_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         'C30 H28 K2 Ni O'
_chemical_formula_sum            'C30 H28 K2 Ni O'
_chemical_formula_weight         541.43
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-21T11:38:34-00:00
_audit_update_record
;
2024-01-17 deposited with the CCDC.	2024-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.8253(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.46834(19)
_cell_length_b                   9.88563(16)
_cell_length_c                   20.5241(3)
_cell_measurement_reflns_used    38808
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      32.257
_cell_measurement_theta_min      2.274
_cell_volume                     2524.11(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_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  (Sheldrick, 2015)'
_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-Arc 100'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.995
_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    -37.00  30.00   0.50    3.00    --  -21.50 -81.00  71.00  134
  2  \w    -73.00  41.00   0.50    3.00    --  -21.50  81.00-166.00  228
  3  \w    -24.00  40.00   0.50    3.00    --   27.11  81.00-166.00  128
  4  \w    -38.00  79.00   0.50    3.00    --   27.11 -81.00  71.00  234
  5  \w   -122.00 -42.00   0.50    3.00    --  -21.50-178.00  60.00  160
  6  \w   -122.00 -42.00   0.50    3.00    --  -21.50-178.00-120.00  160
  7  \w    -71.00  28.00   0.50    3.00    --   27.11 -19.00 150.00  198
  8  \w    -71.00  28.00   0.50    3.00    --   27.11 -19.00 -30.00  198
  9  \w    -71.00  28.00   0.50    3.00    --   27.11 -19.00-180.00  198
 10  \w    -60.00  67.00   0.50    3.00    --   27.11 -57.00 150.00  254
 11  \w    -18.00  89.00   0.50    3.00    --   27.11 -99.00 -60.00  214
 12  \w    -18.00  89.00   0.50    3.00    --   27.11 -99.00   0.00  214
 13  \w    -66.00  45.00   0.50    3.00    --   27.11 -38.00 -90.00  222
 14  \w    -18.00  40.00   0.50    3.00    --  -21.50 -99.00 -30.00  116
 15  \w    -13.00 113.00   0.50    3.00    --   27.11  57.00 -60.00  252
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0298506
_diffrn_orient_matrix_UB_12      0.046551
_diffrn_orient_matrix_UB_13      -0.0203056
_diffrn_orient_matrix_UB_21      0.0151028
_diffrn_orient_matrix_UB_22      0.0530937
_diffrn_orient_matrix_UB_23      0.0219963
_diffrn_orient_matrix_UB_31      0.0461597
_diffrn_orient_matrix_UB_32      0.0126897
_diffrn_orient_matrix_UB_33      -0.0174489
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23178
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.522
_diffrn_reflns_theta_min         2.288
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.12
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.42.89a (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            blue
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.212
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.19
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         23178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0503P)^2^+0.9907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1279
_reflns_Friedel_coverage         0
_reflns_number_gt                15762
_reflns_number_total             23178
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
        Component 2 rotated by -179.9272\%
        around [-0.00 -0.00 1.00] (reciprocal) or [0.11 0.00 0.99] (direct)
        Component 3 rotated by -162.9797\%
        around [-0.11 -0.01 0.99] (reciprocal) or [-0.20 -0.05 0.98] (direct)
;
_cod_data_source_file            d4dt00889h2.cif
_cod_data_source_block           23EH179_AMB-1147
_cod_depositor_comments
'Adding full bibliography for 7715639--7715655.cif.'
_cod_database_code               7715643
_shelx_estimated_absorpt_t_min   0.826
_shelx_estimated_absorpt_t_max   0.887
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.698
_oxdiff_exptl_absorpt_empirical_full_min 0.586
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               3
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
        1. Twinned data refinement
 Scales: 0.4890(9)
 0.4870(9) 0.02401(17)
        2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
        3.a Ternary CH refined with riding coordinates:
 C2(H2), C1(H1)
        3.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C29(H29A,H29B), C27(H27A,H27B), C28(H28A,H28B)
        3.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C19(H19), C6(H6), C7(H7), C16(H16), C22(H22), C26(H26), C10(H10),
 C25(H25), C17(H17), C5(H5), C11(H11), C4(H4), C24(H24), C23(H23), C12(H12),
 C18(H18), C13(H13)
;
_shelx_res_checksum              28059