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_7715653
_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         'C63 H40 D24 Li Ni2 O6 P3'
_chemical_formula_sum            'C63 H40 D24 Li Ni2 O6 P3'
_chemical_formula_weight         1158.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-02
_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                93.0750(10)
_cell_angle_beta                 90.7380(10)
_cell_angle_gamma                111.0290(10)
_cell_formula_units_Z            2
_cell_length_a                   11.81670(10)
_cell_length_b                   12.24780(10)
_cell_length_c                   22.25210(10)
_cell_measurement_reflns_used    64387
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      32.3330
_cell_measurement_theta_min      2.2210
_cell_volume                     2999.91(4)
_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  64.00   0.50    9.00    --   14.06-111.00 -53.00  114
  2  \w    -64.00  -3.00   0.50    9.00    --  -14.53 111.00  39.00  122
  3  \w     -9.00  96.00   0.50    9.00    --   14.06  38.00 120.00  210
  4  \w    -64.00  38.00   0.50    9.00    --   14.06 -57.00 -30.00  204
  5  \w     -9.00  96.00   0.50    9.00    --   14.06  38.00 -30.00  210
  6  \w    -64.00  38.00   0.50    9.00    --   14.06 -57.00-180.00  204
  7  \w    -18.00  29.00   0.50    9.00    --  -14.53 -99.00 -60.00   94
  8  \w    -25.00  68.00   0.50    9.00    --  -14.53  19.00  30.00  186
  9  \w    -18.00  29.00   0.50    9.00    --  -14.53 -99.00 120.00   94
 10  \w    -87.00 -24.00   0.50    9.00    --  -14.53 145.00-148.66  126
 11  \w    -83.00 -21.00   0.50    9.00    --  -14.53 139.00  86.61  124
 12  \w    -82.00 -21.00   0.50    9.00    --  -14.53 138.00 -34.27  122
 13  \w    -93.00   9.00   0.50    9.00    --  -14.53 -57.00-120.00  204
 14  \w    -63.00  19.00   0.50    9.00    --   14.06   0.00-150.00  164
 15  \w      6.50  58.00   0.50    9.00    --   14.06 -99.00-150.00  103
 16  \w    -63.00  92.00   0.50    9.00    --   14.06   0.00-180.00  310
 17  \w    -91.00 -51.00   0.50    9.00    --  -14.53-178.00 -90.00   80
 18  \w    -25.00  68.00   0.50    9.00    --  -14.53  19.00-180.00  186
 19  \w    -81.00 -20.00   0.50    9.00    --  -14.53 137.00  29.37  122
 20  \w    -88.00 -26.00   0.50    9.00    --  -14.53 148.00-165.92  124
 21  \w    -71.50 -36.00   0.50    9.00    --  -14.53 144.00 -73.67   71
 22  \w    -91.00 -61.00   0.50    9.00    --  -14.53-178.00 -30.00   60
;
_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      -0.0168223000
_diffrn_orient_matrix_UB_12      -0.0122182000
_diffrn_orient_matrix_UB_13      -0.0310433000
_diffrn_orient_matrix_UB_21      -0.0172290000
_diffrn_orient_matrix_UB_22      -0.0608735000
_diffrn_orient_matrix_UB_23      0.0038642000
_diffrn_orient_matrix_UB_31      -0.0596711000
_diffrn_orient_matrix_UB_32      -0.0031175000
_diffrn_orient_matrix_UB_33      0.0064483000
_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  0.0331
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            156694
_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         29.574
_diffrn_reflns_theta_min         2.034
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.871
_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    1.283
_exptl_crystal_description       plate
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.058
_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     715
_refine_ls_number_reflns         16811
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0489P)^2^+1.2813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13983
_reflns_number_total             16811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00889h2.cif
_cod_data_source_block           23eh113_amb-1078
_cod_depositor_comments
'Adding full bibliography for 7715639--7715655.cif.'
_cod_database_code               7715653
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C126  H126  Li2  Ni4  O12  P6  '
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.890
_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
 C55-C54A \\sim C55-C54
 with sigma of 0.02
 C54A-C53 \\sim C54-C53
 with sigma of 0.02
 C63-C62A \\sim C63-C62
 with sigma of 0.02
 C62A-C61 \\sim C62-C61
 with sigma of 0.02
 C59-C58 \\sim C59-C58A
 with sigma of 0.02
 C57-C56 \\sim C57A-C56
 with sigma of 0.02
 C58-C57 \\sim C58A-C57A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C54A) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C53)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62A) \\sim Ueq, Uanis(C62)
\\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.01
Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C57A) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C58A) \\sim Ueq, Uanis(C59) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
4. Others
 Sof(D53C)=Sof(D53D)=Sof(D55C)=Sof(D55D)=Sof(C54A)=Sof(D54C)=Sof(D54D)=1-FVAR(1)
 Sof(D53A)=Sof(D53B)=Sof(D55A)=Sof(D55B)=Sof(C54)=Sof(D54A)=Sof(D54B)=FVAR(1)
 Sof(D63C)=Sof(D63D)=Sof(D61C)=Sof(D61D)=Sof(C62A)=Sof(D62C)=Sof(D62D)=1-FVAR(2)
 Sof(D63A)=Sof(D63B)=Sof(D61A)=Sof(D61B)=Sof(C62)=Sof(D62A)=Sof(D62B)=FVAR(2)
 Sof(D59C)=Sof(D59D)=Sof(D56C)=Sof(D56D)=Sof(C58A)=Sof(D58C)=Sof(D58D)=
 Sof(C57A)=Sof(D57C)=Sof(D57D)=1-FVAR(3)
 Sof(D59A)=Sof(D59B)=Sof(D56A)=Sof(D56B)=Sof(C58)=Sof(D58A)=Sof(D58B)=Sof(C57)=
 Sof(D57A)=Sof(D57B)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C52(D52A,D52B), C53(D53A,D53B), C53(D53C,D53D), C63(D63A,D63B), C63(D63C,
 D63D), C61(D61A,D61B), C61(D61C,D61D), C60(D60A,D60B), C55(D55A,D55B),
 C55(D55C,D55D), C59(D59A,D59B), C59(D59C,D59D), C56(D56A,D56B), C56(D56C,D56D),
  C62(D62A,D62B), C54(D54A,D54B), C54A(D54C,D54D), C62A(D62C,D62D), C58(D58A,
 D58B), C57(D57A,D57B), C58A(D58C,D58D), C57A(D57C,D57D)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C17(H17), C39(H39), C33(H33), C27(H27), C9(H9), C23(H23), C45(H45),
 C47(H47), C35(H35), C51(H51), C21(H21), C18(H18), C38(H38), C41(H41), C19(H19),
  C32(H32), C8(H8), C43(H43), C6(H6), C7(H7), C37(H37), C36(H36), C31(H31),
 C44(H44), C20(H20), C48(H48), C49(H49), C15(H15), C50(H50), C11(H11), C26(H26),
  C29(H29), C42(H42), C24(H24), C30(H30), C25(H25), C13(H13), C14(H14), C12(H12)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              43248
_shelx_fab_checksum              15744
_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 1.191
_oxdiff_exptl_absorpt_empirical_full_min 0.895