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_7715655
_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         'C76 H90 Li4 N2 Ni2 O6'
_chemical_formula_sum            'C76 H90 Li4 N2 Ni2 O6'
_chemical_formula_weight         1272.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-01-17 deposited with the CCDC.	2024-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.2280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.77390(10)
_cell_length_b                   19.3181(2)
_cell_length_c                   14.30610(10)
_cell_measurement_reflns_used    98531
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      33.6440
_cell_measurement_theta_min      2.2460
_cell_volume                     3800.61(6)
_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 1.5 (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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_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    -75.00 -18.00   0.50    2.30    --  -13.54 132.00  55.00  114
  2  \w    -79.00 -21.00   0.50    2.30    --  -13.54 138.00-128.00  116
  3  \w     -8.00  90.00   0.50    2.30    --   13.07  57.00 -30.00  196
  4  \w    -25.00  67.00   0.50    2.30    --  -13.54  19.00  60.00  184
  5  \w    -90.00   8.00   0.50    2.30    --  -13.54 -57.00-180.00  196
  6  \w    -35.00  63.00   0.50    2.30    --  -13.54  57.00 -60.00  196
  7  \w    -25.00  67.00   0.50    2.30    --  -13.54  19.00 150.00  184
  8  \w    -78.00 -20.00   0.50    2.30    --  -13.54 136.00 -68.21  116
  9  \w    -19.00  29.00   0.50    2.30    --  -13.54 -99.00 -30.00   96
 10  \w    -78.00 -20.00   0.50    2.30    --  -13.54 136.00-178.94  116
 11  \w    -25.00  67.00   0.50    2.30    --  -13.54  19.00-120.00  184
 12  \w    -90.00   8.00   0.50    2.30    --  -13.54 -57.00  90.00  196
 13  \w    -68.00  28.00   0.50    2.30    --   13.07 -19.00-120.00  192
 14  \w    -62.00 -13.00   0.50    2.30    --   13.07   0.00-150.00   98
 15  \w    -62.00  88.00   0.50    2.30    --   13.07   0.00-180.00  300
 16  \w    -90.00   8.00   0.50    2.30    --  -13.54 -57.00   0.00  196
 17  \w    -81.00 -22.00   0.50    2.30    --  -13.54 141.00  32.71  118
 18  \w    -78.00 -20.00   0.50    2.30    --  -13.54 136.00  73.79  116
 19  \w    -25.00  67.00   0.50    2.30    --  -13.54  19.00  90.00  184
 20  \w    -67.00 -10.00   0.50    2.30    --  -13.54 120.00 147.03  114
 21  \w    -80.00 -21.00   0.50    2.30    --  -13.54 139.00  -8.69  118
 22  \w    -78.00 -20.00   0.50    2.30    --  -13.54 136.00  98.84  116
;
_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      0.0174821000
_diffrn_orient_matrix_UB_12      -0.0343759000
_diffrn_orient_matrix_UB_13      -0.0037168000
_diffrn_orient_matrix_UB_21      -0.0469031000
_diffrn_orient_matrix_UB_22      -0.0128947000
_diffrn_orient_matrix_UB_23      0.0085062000
_diffrn_orient_matrix_UB_31      -0.0124317000
_diffrn_orient_matrix_UB_32      0.0003886000
_diffrn_orient_matrix_UB_33      -0.0487816000
_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  0.0408
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            225483
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.222
_diffrn_reflns_theta_min         2.108
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.802
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         11310
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+1.7017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10010
_reflns_number_total             11310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00889h2.cif
_cod_data_source_block           23eh145_amb-1106
_cod_depositor_comments
'Adding full bibliography for 7715639--7715655.cif.'
_cod_database_code               7715655
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C168  H208  Li8  N4  Ni4  O16  '
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.871
_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. Restrained distances
 C36A-C35 \\sim C36-C35
 with sigma of 0.01
 C37-C36 \\sim C37A-C36A
 with sigma of 0.01
 C38-C37 \\sim C38-C37A
 with sigma of 0.01
 C32A-C31 \\sim C32-C31
 with sigma of 0.01
 C33-C32 \\sim C33A-C32A
 with sigma of 0.01
 C34-C33 \\sim C34-C33A
 with sigma of 0.01
3. Rigid bond restraints
 C38, C37A, C37, C36A, C36, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(C37) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C36A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
5. Others
 Sof(H38C)=Sof(H38D)=Sof(H35C)=Sof(H35D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=1-FVAR(1)
 Sof(H38A)=Sof(H38B)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=
 Sof(H37A)=Sof(H37B)=FVAR(1)
 Sof(H31C)=Sof(H31D)=Sof(H34C)=Sof(H34D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=
 Sof(C32A)=Sof(H32C)=Sof(H32D)=1-FVAR(2)
 Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H34A)=Sof(H34B)=Sof(C33)=
 Sof(H33A)=Sof(H33B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C14(H14)
6.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C28(H28A,H28B), C29(H29A,H29B), C27(H27A,H27B), C31(H31A,
 H31B), C31(H31C,H31D), C38(H38A,H38B), C38(H38C,H38D), C35(H35A,H35B),
 C35(H35C,H35D), C32(H32A,H32B), C34(H34A,H34B), C34(H34C,H34D), C33(H33A,H33B),
  C36(H36A,H36B), C37(H37A,H37B), C37A(H37C,H37D), C36A(H36C,H36D), C33A(H33C,
 H33D), C32A(H32C,H32D)
6.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C22(H22), C23(H23), C20(H20), C12(H12), C8(H8), C24(H24), C25(H25),
 C16(H16), C11(H11), C9(H9), C6(H6), C19(H19), C2(H2), C3(H3), C18(H18),
 C17(H17), C10(H10), C5(H5), C4(H4)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20353
_shelx_fab_checksum              44960
_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 1.140
_oxdiff_exptl_absorpt_empirical_full_min 0.882