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_7715647
_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         'C40 H38 Li Ni O2, C16 H31 Li O4'
_chemical_formula_sum            'C56 H69 Li2 Ni O6'
_chemical_formula_weight         910.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 111.093(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8080(4)
_cell_length_b                   13.0662(2)
_cell_length_c                   22.5123(4)
_cell_measurement_reflns_used    46578
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      33.5160
_cell_measurement_theta_min      2.3800
_cell_volume                     4887.25(17)
_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      173.00(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    -72.00 -15.00   0.50    0.80    --  -13.54 127.00  36.00  114
  2  \w    -83.00 -24.00   0.50    0.80    --  -13.54 144.00-154.00  118
  3  \w     -8.00  90.00   0.50    0.80    --   13.07  57.00 -90.00  196
  4  \w    -16.00  83.00   0.50    0.80    --   13.07  77.00  30.00  198
  5  \w    -19.00  29.00   0.50    0.80    --  -13.54 -99.00-150.00   96
  6  \w    -87.00 -42.00   0.50    0.80    --  -13.54-178.00 120.00   90
  7  \w    -19.00  29.00   0.50    0.80    --  -13.54 -99.00-120.00   96
  8  \w    -87.00 -42.00   0.50    0.80    --  -13.54-178.00-180.00   90
  9  \w    -19.00  29.00   0.50    0.80    --  -13.54 -99.00  90.00   96
 10  \w    -94.00   7.00   0.50    0.80    --  -13.54 -38.00   0.00  202
 11  \w    -25.00  67.00   0.50    0.80    --  -13.54  19.00-180.00  184
 12  \w    -87.00 -57.00   0.50    0.80    --  -13.54-178.00 -30.00   60
 13  \w    -25.00  67.00   0.50    0.80    --  -13.54  19.00   0.00  184
;
_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      -0.0181228000
_diffrn_orient_matrix_UB_12      -0.0005783000
_diffrn_orient_matrix_UB_13      -0.0336880000
_diffrn_orient_matrix_UB_21      -0.0079714000
_diffrn_orient_matrix_UB_22      -0.0530623000
_diffrn_orient_matrix_UB_23      0.0008609000
_diffrn_orient_matrix_UB_31      -0.0378222000
_diffrn_orient_matrix_UB_32      0.0114910000
_diffrn_orient_matrix_UB_33      0.0022171000
_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  0.0386
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            145032
_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         30.507
_diffrn_reflns_theta_min         2.393
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.459
_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_colour_primary    black
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             1948
_exptl_crystal_size_max          0.528
_exptl_crystal_size_mid          0.451
_exptl_crystal_size_min          0.298
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         14918
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+1.1244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11158
_reflns_number_total             14918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00889h2.cif
_cod_data_source_block           23eh177_amb-1142
_cod_depositor_comments
'Adding full bibliography for 7715639--7715655.cif.'
_cod_database_code               7715647
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C224  H280  Li8  Ni4  O24  '
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.798
_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
 O4-C48 \\sim O4A-C48A
 with sigma of 0.02
 O4-C45A \\sim O4A-C45
 with sigma of 0.02
 C46A-C45A \\sim C46-C45
 with sigma of 0.02
 C34-C33 \\sim C34A-C33
 with sigma of 0.02
 C47-C46A \\sim C47A-C46
 with sigma of 0.02
 C35A-C34 \\sim C35-C34A
 with sigma of 0.02
 C48-C47 \\sim C48A-C47A
 with sigma of 0.02
 O2-C40 \\sim O2-C40A
 with sigma of 0.02
 C40-C39 \\sim C40A-C39A
 with sigma of 0.02
 C39-C38 \\sim C39A-C38A
 with sigma of 0.02
 C38-C37 \\sim C38A-C37
 with sigma of 0.02
 C36-C35A \\sim C36A-C35
 with sigma of 0.02
 O1-C36 \\sim O1-C36A
 with sigma of 0.02
3. Rigid bond restraints
 O4, C48, C47, C46A, C45A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4A, C48A, C47A, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, C33, C34A, C34, C35A, C35, C36, C36A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C45) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(C45A) \\sim Ueq, Uanis(C46A) \\sim Ueq,
Uanis(C48A) \\sim Ueq, Uanis(C47A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C49A) \\sim Ueq, Uanis(C49B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C36) \\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C33) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C38A) \\sim Ueq, Uanis(C39A)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C40A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Others
 Sof(H50C)=Sof(H50D)=Sof(C49B)=Sof(H49C)=Sof(H49D)=1-FVAR(1)
 Sof(H50A)=Sof(H50B)=Sof(C49A)=Sof(H49A)=Sof(H49B)=FVAR(1)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(O4A)=Sof(C48A)=
 Sof(H48C)=Sof(H48D)=Sof(C47A)=Sof(H47C)=Sof(H47D)=1-FVAR(2)
 Sof(O4)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C45A)=
 Sof(H45D)=Sof(H45C)=Sof(C46A)=Sof(H46C)=Sof(H46D)=FVAR(2)
 Sof(H37C)=Sof(H37D)=Sof(C40A)=Sof(H40D)=Sof(H40C)=Sof(C39A)=Sof(H39C)=
 Sof(H39D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=1-FVAR(3)
 Sof(H37A)=Sof(H37B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=FVAR(3)
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C34A)=
 Sof(H34C)=Sof(H34D)=1-FVAR(4)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C34)=Sof(H34B)=
 Sof(H34A)=FVAR(4)
 Sof(H33C)=Sof(H33D)=1-FVAR(5)
 Sof(H33A)=Sof(H33B)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C15(H15), C14(H14), C13(H13)
6.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C51(H51A,H51B), C50(H50A,H50B), C50(H50C,H50D), C37(H37A,
 H37B), C37(H37C,H37D), C33(H33A,H33B), C33(H33C,H33D), C53(H53A,H53B),
 C43(H43A,H43B), C55(H55A,H55B), C49A(H49A,H49B), C41(H41A,H41B), C54(H54A,
 H54B), C56(H56A,H56B), C40(H40A,H40B), C45(H45A,H45B), C42(H42A,H42B),
 C48(H48A,H48B), C38(H38A,H38B), C46(H46A,H46B), C36(H36A,H36B), C35(H35A,H35B),
  C47(H47A,H47B), C39(H39A,H39B), C49B(H49C,H49D), C45A(H45D,H45C), C46A(H46C,
 H46D), C48A(H48C,H48D), C47A(H47C,H47D), C40A(H40D,H40C), C39A(H39C,H39D),
 C38A(H38C,H38D), C36A(H36C,H36D), C35A(H35C,H35D), C34(H34B,H34A), C34A(H34C,
 H34D)
6.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C6(H6), C18(H18), C2(H2), C32(H32), C19(H19), C12(H12), C27(H27),
 C26(H26), C8(H8), C3(H3), C4(H4), C11(H11), C5(H5), C10(H10), C28(H28),
 C31(H31), C30(H30), C9(H9), C52(H52)
;
_shelx_res_checksum              57038
_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 1.249
_oxdiff_exptl_absorpt_empirical_full_min 0.864