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_7715648
_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         'C44 H38 Li Ni O2, C16 H32 Li O4'
_chemical_formula_sum            'C60 H70 Li2 Ni O6'
_chemical_formula_weight         959.75
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-04T17:01:33-00:00
_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                   13.7527(2)
_cell_length_b                   21.6279(4)
_cell_length_c                   34.0256(5)
_cell_measurement_reflns_used    64285
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      31.706
_cell_measurement_theta_min      2.457
_cell_volume                     10120.6(3)
_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 2018/2 (Sheldrick, 2018)'
_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 0.999
_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    -83.00 -24.00   0.50   15.00    --  -13.54 144.00 143.00  118
  2  \w    -72.00 -15.00   0.50   15.00    --  -13.54 127.00 -25.00  114
  3  \w    -87.00 -42.00   0.50   15.00    --  -13.54-178.00-150.00   90
  4  \w    -87.00 -42.00   0.50   15.00    --  -13.54-178.00 -30.00   90
  5  \w    -19.00  29.00   0.50   15.00    --  -13.54 -99.00  60.00   96
  6  \w    -87.00 -42.00   0.50   15.00    --  -13.54-178.00 120.00   90
  7  \w    -25.00  67.00   0.50   15.00    --  -13.54  19.00-180.00  184
  8  \w    -87.00 -44.00   0.50   15.00    --  -13.54-178.00   0.00   86
  9  \w    -87.00 -42.00   0.50   15.00    --  -13.54-178.00 -30.00   90
 10  \w    -19.00  29.00   0.50   15.00    --  -13.54 -99.00  60.00   96
 11  \w    -87.00 -42.00   0.50   15.00    --  -13.54-178.00 120.00   90
 12  \w    -25.00  67.00   0.50   15.00    --  -13.54  19.00-180.00  184
 13  \w    -87.00 -44.00   0.50   15.00    --  -13.54-178.00   0.00   86
;
_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      0.0190117
_diffrn_orient_matrix_UB_12      -0.0267669
_diffrn_orient_matrix_UB_13      -0.0092798
_diffrn_orient_matrix_UB_21      0.0125614
_diffrn_orient_matrix_UB_22      -0.0123796
_diffrn_orient_matrix_UB_23      0.0186315
_diffrn_orient_matrix_UB_31      -0.0462489
_diffrn_orient_matrix_UB_32      -0.014362
_diffrn_orient_matrix_UB_33      0.0012363
_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  0.0536
_diffrn_reflns_av_unetI/netI     0.077
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            242758
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.124
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.726
_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            black
_exptl_crystal_density_diffrn    1.26
_exptl_crystal_description       needle
_exptl_crystal_F_000             4096
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.37
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         15457
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.073
_refine_ls_R_factor_gt           0.046
_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^)+(0.0634P)^2^+3.0589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0
_reflns_number_gt                10933
_reflns_number_total             15457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00889h2.cif
_cod_data_source_block           23EH219_AMB-1182
_cod_depositor_comments
'Adding full bibliography for 7715639--7715655.cif.'
_cod_database_code               7715648
_shelx_estimated_absorpt_t_min   0.888
_shelx_estimated_absorpt_t_max   0.97
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.882
_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, All C(H,H,H,H) groups
        2. Rigid bond restraints
 O1, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1, C37, C38A, C39A, C40A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O6, C57A, C58, C59, C60
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O6, C57, C58, C59, C60
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O5, C53, C54, C55, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O5, C53, C54A, C55A, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
        3. Uiso/Uaniso restraints and constraints
        Uanis(C39) \\sim Ueq, Uanis(C38A) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C40)
        \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
        Uanis(C57A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
        Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
        Uanis(C55A) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C54A) \\sim Ueq, Uanis(C54)
        \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
        4. Others
 Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39C)=
 Sof(H39D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=1-FVAR(1)
 Sof(H37A)=Sof(H37B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(C38)=Sof(H38A)=Sof(H38B)=FVAR(1)
 Sof(H58C)=Sof(H58D)=Sof(C57A)=Sof(H57C)=Sof(H57D)=1-FVAR(2)
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H58A)=Sof(H58B)=FVAR(2)
 Sof(H49C)=Sof(H49D)=Sof(H52C)=Sof(H52D)=Sof(C50A)=Sof(H50C)=Sof(H50D)=
 Sof(C51A)=Sof(H51C)=Sof(H51D)=1-FVAR(3)
 Sof(H49A)=Sof(H49B)=Sof(H52A)=Sof(H52B)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C50)=
 Sof(H50A)=Sof(H50B)=FVAR(3)
 Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=1-FVAR(4)
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H47A)=Sof(H47B)=FVAR(4)
 Sof(H53C)=Sof(H53D)=Sof(H56C)=Sof(H56D)=Sof(C55A)=Sof(H55C)=Sof(H55D)=
 Sof(C54A)=Sof(H54C)=Sof(H54D)=1-FVAR(5)
 Sof(H53A)=Sof(H53B)=Sof(H56A)=Sof(H56B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C55)=
 Sof(H55A)=Sof(H55B)=FVAR(5)
        5.a Ternary CH refined with riding coordinates:
 C13(H13), C14(H14)
        5.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C43(H43A,H43B), C45(H45A,H45B), C49(H49A,H49B), C49(H49C,
 H49D), C59(H59A,H59B), C41(H41A,H41B), C52(H52A,H52B), C52(H52C,H52D),
 C60(H60A,H60B), C46(H46A,H46B), C53(H53A,H53B), C53(H53C,H53D), C42(H42A,H42B),
  C56(H56A,H56B), C56(H56C,H56D), C57(H57A,H57B), C37(H37A,H37B), C37(H37C,
 H37D), C40(H40A,H40B), C58(H58A,H58B), C58(H58C,H58D), C39(H39A,H39B),
 C54(H54A,H54B), C48(H48A,H48B), C47(H47A,H47B), C47(H47C,H47D), C51(H51A,H51B),
  C50(H50A,H50B), C55(H55A,H55B), C38(H38A,H38B), C38A(H38C,H38D), C39A(H39C,
 H39D), C40A(H40C,H40D), C57A(H57C,H57D), C50A(H50C,H50D), C51A(H51C,H51D),
 C48A(H48C,H48D), C55A(H55C,H55D), C54A(H54C,H54D)
        5.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C16(H16), C26(H26), C29(H29), C8(H8), C23(H23), C12(H12), C28(H28),
 C22(H22), C6(H6), C2(H2), C17(H17), C3(H3), C11(H11), C20(H20), C10(H10),
 C9(H9), C19(H19), C4(H4), C5(H5)
;
_shelx_res_checksum              90237