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_7715639
_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         'C18 H23 Ni, C16 H32 Li O8'
_chemical_formula_sum            'C34 H55 Li Ni O8'
_chemical_formula_weight         657.43
_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             2023-10-17
_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                 93.3440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.15520(10)
_cell_length_b                   10.28020(10)
_cell_length_c                   21.0871(2)
_cell_measurement_reflns_used    82498
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      33.6930
_cell_measurement_theta_min      2.1990
_cell_volume                     3279.74(5)
_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      100.01(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 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    -21.00  40.00   0.50    6.00    --   13.91  86.00   0.00  122
  2  \w    -38.00  50.00   0.50    6.00    --   13.91 -86.00-117.00  176
  3  \w    -50.00  41.00   0.50    6.00    --  -14.37  86.00   0.00  182
  4  \w    -37.00  21.00   0.50    6.00    --  -14.37 -86.00-117.00  116
  5  \w    -17.00  85.00   0.50    6.00    --   13.91  77.00 120.00  204
  6  \w    -18.00  58.00   0.50    6.00    --   13.91 -99.00 -30.00  152
  7  \w    -25.00  68.00   0.50    6.00    --  -14.37  19.00-150.00  186
  8  \w    -82.00 -21.00   0.50    6.00    --  -14.37 138.00 128.53  122
  9  \w    -18.00  29.00   0.50    6.00    --  -14.37 -99.00 120.00   94
 10  \w    -96.00   9.00   0.50    6.00    --  -14.37 -38.00   0.00  210
 11  \w    -25.00  68.00   0.50    6.00    --  -14.37  19.00 150.00  186
 12  \w    -25.00  68.00   0.50    6.00    --  -14.37  19.00  30.00  186
 13  \w    -93.00 -29.00   0.50    6.00    --  -14.37 154.00   2.35  128
 14  \w    -96.00   9.00   0.50    6.00    --  -14.37 -38.00-150.00  210
 15  \w    -85.00 -23.00   0.50    6.00    --  -14.37 143.00-172.00  124
 16  \w    -84.00 -22.00   0.50    6.00    --  -14.37 141.00  78.50  124
 17  \w    -80.00 -19.00   0.50    6.00    --  -14.37 135.00 -35.57  122
 18  \w    -18.00  29.00   0.50    6.00    --  -14.37 -99.00 -90.00   94
 19  \w    -97.00  28.00   0.50    6.00    --  -14.37 -19.00-150.00  250
 20  \w    -18.00  29.00   0.50    6.00    --  -14.37 -99.00-180.00   94
 21  \w    -81.00 -20.00   0.50    6.00    --  -14.37 137.00  66.47  122
 22  \w    -83.00 -22.00   0.50    6.00    --  -14.37 140.00-134.24  122
 23  \w    -92.00 -45.00   0.50    6.00    --  -14.37   0.00-180.00   94
 24  \w    -76.00 -16.00   0.50    6.00    --  -14.37 129.00 -76.69  120
;
_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      0.0346003000
_diffrn_orient_matrix_UB_12      0.0360010000
_diffrn_orient_matrix_UB_13      0.0158505000
_diffrn_orient_matrix_UB_21      0.0273768000
_diffrn_orient_matrix_UB_22      -0.0121062000
_diffrn_orient_matrix_UB_23      -0.0255156000
_diffrn_orient_matrix_UB_31      -0.0158622000
_diffrn_orient_matrix_UB_32      0.0575966000
_diffrn_orient_matrix_UB_33      -0.0152622000
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_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            191061
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.081
_diffrn_reflns_theta_min         2.205
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.894
_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    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         9636
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+1.6257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0794
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8756
_reflns_number_total             9636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00889h2.cif
_cod_data_source_block           23eh139_amb-1072
_cod_depositor_comments
'Adding full bibliography for 7715639--7715655.cif.'
_cod_database_code               7715639
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C136  H224  Li4  Ni4  O32  '
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.897
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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
 C7-C18 \\sim C7A-C18
 with sigma of 0.02
 C8A-C7A \\sim C8-C7
 with sigma of 0.02
 C9-C8 \\sim C9-C8A
 with sigma of 0.02
 C11A-C10 \\sim C11-C10
 with sigma of 0.02
 C12-C11 \\sim C12A-C11A
 with sigma of 0.02
 C13-C12 \\sim C13-C12A
 with sigma of 0.02
 C15A-C14 \\sim C15-C14
 with sigma of 0.02
 C16A-C15A \\sim C16-C15
 with sigma of 0.02
 C17-C16 \\sim C17-C16A
 with sigma of 0.02
3. Rigid bond restraints
 C27A, O5A, C28A, C34A, O10, C32A, C33A, O6A, C30A, C31A, C29A, O7A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C28, C27, O5, C34, C33, O8A, C32, C31, C29, C30, O7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C17, C16, C16A, C18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C7A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O5) \\sim Ueq, Uanis(O8A) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(C28A)
\\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C32A) \\sim Ueq,
Uanis(C33A) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(O6A) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(C31A) \\sim Ueq,
Uanis(C29A) \\sim Ueq, Uanis(O7A) \\sim Ueq, Uanis(C27A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.02
Uanis(C11A) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C12A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C15A) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C16A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H14C)=Sof(H14D)=Sof(H13C)=Sof(H13D)=Sof(H9BC)=Sof(H9BD)=Sof(H10C)=
 Sof(H10D)=Sof(H18C)=Sof(H18D)=Sof(H17C)=Sof(H17D)=Sof(C8A)=Sof(H8A)=Sof(C7A)=
 Sof(H7A)=Sof(C12A)=Sof(H12A)=Sof(C11A)=Sof(H11A)=Sof(C16A)=Sof(H16A)=Sof(C15A)=
 Sof(H15A)=1-FVAR(1)
 Sof(H14A)=Sof(H14B)=Sof(H13A)=Sof(H13B)=Sof(H9AA)=Sof(H9AB)=Sof(H10A)=
 Sof(H10B)=Sof(H18A)=Sof(H18B)=Sof(H17A)=Sof(H17B)=Sof(C16)=Sof(H16)=Sof(C12)=
 Sof(H12)=Sof(C11)=Sof(H11)=Sof(C15)=Sof(H15)=Sof(C8)=Sof(H8)=Sof(C7)=Sof(H7)=
 FVAR(1)
 Sof(O5A)=Sof(O6A)=Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C34A)=Sof(H34C)=Sof(H34D)=
 Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=Sof(O10)=Sof(C32A)=
 Sof(H32C)=Sof(H32D)=Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C33A)=Sof(H33C)=
 Sof(H33D)=Sof(O7A)=Sof(C27A)=Sof(H27C)=Sof(H27D)=1-FVAR(2)
 Sof(O7)=Sof(O5)=Sof(O8A)=Sof(O6)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(C29)=Sof(H29A)=Sof(H29B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C16(H16), C12(H12), C11(H11), C15(H15), C8(H8), C7(H7), C8A(H8A), C12A(H12A),
 C11A(H11A), C16A(H16A), C15A(H15A)
6.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C14(H14C,H14D), C13(H13A,H13B), C13(H13C,H13D), C19(H19A,
 H19B), C25(H25A,H25B), C20(H20A,H20B), C9(H9AA,H9AB), C9(H9BC,H9BD), C22(H22A,
 H22B), C10(H10A,H10B), C10(H10C,H10D), C23(H23A,H23B), C26(H26A,H26B),
 C21(H21A,H21B), C18(H18A,H18B), C18(H18C,H18D), C24(H24A,H24B), C17(H17A,H17B),
  C17(H17C,H17D), C34(H34A,H34B), C28(H28A,H28B), C33(H33A,H33B), C32(H32A,
 H32B), C31(H31A,H31B), C30(H30A,H30B), C27(H27A,H27B), C29(H29A,H29B),
 C28A(H28C,H28D), C34A(H34C,H34D), C30A(H30C,H30D), C31A(H31C,H31D), C32A(H32C,
 H32D), C29A(H29C,H29D), C33A(H33C,H33D), C27A(H27C,H27D)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C2(H2), C5(H5), C4(H4), C7A(H7A)
;
_shelx_res_checksum              67966
_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 1.139
_oxdiff_exptl_absorpt_empirical_full_min 0.924