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_7715651
_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_absolute_configuration ad
_chemical_formula_moiety         'C52 H62 K2 Ni O8'
_chemical_formula_sum            'C52 H62 K2 Ni O8'
_chemical_formula_weight         951.92
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-22T17:11:13-00:00
_audit_update_record
;
2024-01-17 deposited with the CCDC.	2024-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.7188(3)
_cell_length_b                   26.1144(5)
_cell_length_c                   19.8447(3)
_cell_measurement_reflns_used    15202
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      73.756
_cell_measurement_theta_min      4.457
_cell_volume                     9700.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.101a 64-bit (release 31-08-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (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 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 0.984
_diffrn_measured_fraction_theta_max 0.977
_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   -120.00 -95.00   0.50    6.00    --  -49.99-128.00-107.00   50
  2  \w    -83.00 -14.00   0.50    6.00    --  -49.99 128.00 -32.00  138
  3  \w   -104.00 -79.00   0.50    6.00    --  -49.99-142.00  81.00   50
  4  \w     50.00  75.00   0.50    6.00    --   49.99-142.00  81.00   50
  5  \w     37.00  94.00   0.50    6.00    --   49.99-128.00-107.00  114
  6  \w    -78.00 -53.00   0.50   10.00    --  -90.00 128.00 -32.00   50
  7  \w   -140.00-115.00   0.50   10.00    --  -90.00-128.00-107.00   50
  8  \w    -68.00 -43.00   0.50   10.00    --  -90.00 142.00 137.00   50
  9  \w   -133.00-108.00   0.50   10.00    --  -90.00-142.00  81.00   50
 10  \w    104.00 129.00   0.50   10.00    --  111.50 142.00 137.00   50
 11  \w    111.00 136.00   0.50   10.00    --  111.50 128.00 -32.00   50
 12  \w     55.00  80.00   0.50   10.00    --  111.50-128.00-107.00   50
 13  \w    -86.00 -45.00   0.50    6.00    --  -49.99 -38.00  30.00   82
 14  \w     47.00 112.00   0.50    6.00    --   49.99  19.00   0.00  130
 15  \w     48.00 121.00   0.50    6.00    --   49.99  19.00  60.00  146
 16  \w   -154.00-127.00   0.50   10.00    --  -90.00 -73.00  16.66   54
 17  \w     42.00  68.00   0.50   10.00    --  111.50 -77.00-120.00   52
 18  \w     47.00  89.00   0.50   10.00    --  111.50 -77.00   0.00   84
 19  \w     99.00 158.00   0.50   10.00    --  111.50  61.00  30.00  118
 20  \w    129.00 176.00   0.50   10.00    --  111.50  77.00  30.00   94
 21  \w     85.00 118.00   0.50   10.00    --  111.50   0.00 120.00   66
 22  \w     92.00 120.00   0.50   10.00    --  111.50  77.00  30.00   56
 23  \w    110.00 169.00   0.50   10.00    --  111.50  30.00 150.00  118
 24  \w    140.00 171.00   0.50   10.00    --  111.50  45.00  90.00   62
 25  \w    128.00 177.00   0.50   10.00    --  111.50  15.00   0.00   98
 26  \w     94.00 147.00   0.50   10.00    --  111.50  77.00  60.00  106
 27  \w     98.00 178.00   0.50   10.00    --  111.50  61.00  60.00  160
 28  \w     41.00  67.00   0.50   10.00    --  111.50 -61.00-150.00   52
 29  \w    124.00 178.00   0.50   10.00    --  111.50  77.00   0.00  108
 30  \w    153.00 178.00   0.50   10.00    --  111.50  61.00  90.00   50
 31  \w     41.00  71.00   0.50   10.00    --  111.50 -61.00  90.00   60
 32  \w    104.00 129.00   0.50   10.00    --  111.50  61.00  90.00   50
 33  \w     59.00 108.00   0.50   10.00    --  111.50-125.00  90.00   98
 34  \w     92.00 160.00   0.50   10.00    --  111.50  77.00 -60.00  136
;
_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      0.0755822
_diffrn_orient_matrix_UB_12      0.0199078
_diffrn_orient_matrix_UB_13      -0.0161983
_diffrn_orient_matrix_UB_21      0.0277881
_diffrn_orient_matrix_UB_22      -0.0555022
_diffrn_orient_matrix_UB_23      -0.002594
_diffrn_orient_matrix_UB_31      -0.0170575
_diffrn_orient_matrix_UB_32      -0.002331
_diffrn_orient_matrix_UB_33      -0.0758399
_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  0.0773
_diffrn_reflns_av_unetI/netI     0.1091
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            87034
_diffrn_reflns_point_group_measured_fraction_full 0.882
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.49
_diffrn_reflns_theta_min         3.661
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.532
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023)
        Analytical numeric absorption correction using a multifaceted crystal
        model based on expressions derived by R.C. Clark & J.S. Reid.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       plate
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 3931 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(6)
_refine_ls_extinction_coef       0.000126(19)
_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   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1168
_refine_ls_number_reflns         17300
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0542P)^2^+3.2655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1253
_reflns_Friedel_coverage         0.731
_reflns_Friedel_fraction_full    0.774
_reflns_Friedel_fraction_max     0.76
_reflns_number_gt                12004
_reflns_number_total             17300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00889h2.cif
_cod_data_source_block           23EH333_AMB-1249
_cod_depositor_comments
'Adding full bibliography for 7715639--7715655.cif.'
_cod_database_code               7715651
_shelx_estimated_absorpt_t_min   0.673
_shelx_estimated_absorpt_t_max   0.863
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.32
_oxdiff_exptl_absorpt_empirical_full_min 0.768
_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(C88) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
        3.a Ternary CH refined with riding coordinates:
 C100(H100)
        3.b Secondary CH2 refined with riding coordinates:
 C78(H78A,H78B), C26(H26A,H26B), C27(H27A,H27B), C79(H79A,H79B), C31(H31A,
 H31B), C30(H30B,H30A), C34(H34A,H34B), C86(H86A,H86B), C83(H83A,H83B),
 C87(H87A,H87B), C39(H39B,H39A), C35(H35A,H35B), C82(H82A,H82B), C91(H91A,H91B),
  C38(H38B,H38A), C90(H90A,H90B)
        3.c Aromatic/amide H refined with riding coordinates:
 C45(H45), C68(H68), C43(H43), C94(H94), C5(H5), C69(H69), C42(H42), C46(H46),
 C16(H16), C97(H97), C66(H66), C50(H50), C62(H62), C63(H63), C56(H56), C44(H44),
  C13(H13), C52(H52), C98(H98), C60(H60), C96(H96), C51(H51), C103(H103),
 C95(H95), C17(H17), C14(H14), C59(H59), C57(H57), C8(H8), C7(H7), C65(H65),
 C49(H49), C4(H4), C48(H48), C10(H10), C101(H101), C104(H104), C11(H11),
 C102(H102)
        3.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C28(H28C,H28A,H28B), C40(H40A,H40B,H40C), C80(H80A,H80B,
 H80C), C77(H77A,H77B,H77C), C29(H29A,H29B,H29C), C92(H92A,H92B,H92C), C81(H81A,
 H81B,H81C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C),
 C85(H85A,H85B,H85C), C84(H84A,H84B,H84C), C89(H89A,H89B,H89C), C37(H37A,H37B,
 H37C), C88(H88A,H88B,H88C)
;
_shelx_res_checksum              66215