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_7715646
_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         'C42 H52 Li2 Ni O4'
_chemical_formula_sum            'C42 H52 Li2 Ni O4'
_chemical_formula_weight         693.42
_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   mixed
_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                 101.5340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7487(2)
_cell_length_b                   12.4289(2)
_cell_length_c                   18.2015(3)
_cell_measurement_reflns_used    46696
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      33.6420
_cell_measurement_theta_min      2.2330
_cell_volume                     3712.45(10)
_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      7.00  61.00   0.50    3.50    --   13.07-111.00-174.00  108
  2  \w    -61.00  -3.00   0.50    3.50    --  -13.54 111.00 -80.00  116
  3  \w    -67.00  33.00   0.50    3.50    --   13.07 -38.00 -90.00  200
  4  \w    -19.00  29.00   0.50    3.50    --  -13.54 -99.00-180.00   96
  5  \w    -25.00  67.00   0.50    3.50    --  -13.54  19.00 -90.00  184
  6  \w    -19.00  29.00   0.50    3.50    --  -13.54 -99.00 -60.00   96
  7  \w    -19.00  29.00   0.50    3.50    --  -13.54 -99.00  30.00   96
  8  \w    -25.00  67.00   0.50    3.50    --  -13.54  19.00-180.00  184
  9  \w    -35.00  63.00   0.50    3.50    --  -13.54  57.00  60.00  196
 10  \w    -19.00  29.00   0.50    3.50    --  -13.54 -99.00-120.00   96
 11  \w    -19.00  29.00   0.50    3.50    --  -13.54 -99.00 -30.00   96
 12  \w    -83.00 -58.00   0.50    3.50    --  -13.54 -77.00 -60.00   50
 13  \w    -94.00   7.00   0.50    3.50    --  -13.54 -38.00 120.00  202
;
_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      0.0209465000
_diffrn_orient_matrix_UB_12      0.0289978000
_diffrn_orient_matrix_UB_13      -0.0238853000
_diffrn_orient_matrix_UB_21      -0.0187346000
_diffrn_orient_matrix_UB_22      -0.0323662000
_diffrn_orient_matrix_UB_23      -0.0307356000
_diffrn_orient_matrix_UB_31      -0.0328451000
_diffrn_orient_matrix_UB_32      0.0369814000
_diffrn_orient_matrix_UB_33      -0.0081680000
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            108687
_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         30.030
_diffrn_reflns_theta_min         2.055
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.758
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         10860
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+1.1336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9205
_reflns_number_total             10860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00889h2.cif
_cod_data_source_block           23eh159_amb-1120
_cod_depositor_comments
'Adding full bibliography for 7715639--7715655.cif.'
_cod_database_code               7715646
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C168  H208  Li8  Ni4  O16  '
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.907
_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 0.02
 C37-C36A \\sim C37-C36
 with sigma of 0.02
 C30A-C29 \\sim C30-C29
 with sigma of 0.02
 O1-C30A \\sim O1-C30
 with sigma of 0.02
 C34-C33A \\sim C34-C33
 with sigma of 0.02
 C33A-C32 \\sim C33-C32
 with sigma of 0.02
 O4-C42 \\sim O4-C42A
 with sigma of 0.02
 C42-C41 \\sim C42A-C41A
 with sigma of 0.02
 C41A-C40 \\sim C41-C40
 with sigma of 0.02
3. Rigid bond restraints
 C42, C42A, C41A, C41, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C24, C23
 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(C36A) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C37)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C30A) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(O1)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C41A) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C42A)
\\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Others
 Sof(H37C)=Sof(H37D)=Sof(H35C)=Sof(H35D)=Sof(C36A)=Sof(H36C)=Sof(H36D)=1-FVAR(1)
 Sof(H37A)=Sof(H37B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H35A)=Sof(H35B)=FVAR(1)
 Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=1-FVAR(2)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H29A)=Sof(H29B)=FVAR(2)
 Sof(H34C)=Sof(H34D)=Sof(H32C)=Sof(H32D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=1-FVAR(3)
 Sof(H34A)=Sof(H34B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H32A)=Sof(H32B)=FVAR(3)
 Sof(H40C)=Sof(H40D)=Sof(C41A)=Sof(H41C)=Sof(H41D)=Sof(C42A)=Sof(H42C)=
 Sof(H42D)=1-FVAR(4)
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H40A)=Sof(H40B)=
 FVAR(4)
6.a Ternary CH refined with riding coordinates:
 C14(H14)
6.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C38(H38A,H38B), C31(H31A,H31B), C39(H39A,H39B), C28(H28A,
 H28B), C34(H34A,H34B), C34(H34C,H34D), C37(H37A,H37B), C37(H37C,H37D),
 C30(H30A,H30B), C42(H42A,H42B), C29(H29A,H29B), C29(H29C,H29D), C41(H41A,H41B),
  C36(H36A,H36B), C35(H35A,H35B), C35(H35C,H35D), C33(H33A,H33B), C32(H32A,
 H32B), C32(H32C,H32D), C40(H40A,H40B), C40(H40C,H40D), C36A(H36C,H36D),
 C30A(H30C,H30D), C33A(H33C,H33D), C41A(H41C,H41D), C42A(H42C,H42D)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C12(H12), C5(H5), C8(H8), C3(H3), C16(H16), C4(H4), C17(H17),
 C11(H11), C19(H19), C9(H9), C18(H18), C10(H10), C22(H22), C25(H25), C23(H23),
 C24(H24)
;
_shelx_res_checksum              3904
_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 1.107
_oxdiff_exptl_absorpt_empirical_full_min 0.931