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_7715650
_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         '2(C38 H44 Na2 Ni O3)'
_chemical_formula_sum            'C76 H88 Na4 Ni2 O6'
_chemical_formula_weight         1306.84
_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   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                106.7570(10)
_cell_angle_beta                 99.6030(10)
_cell_angle_gamma                92.9580(10)
_cell_formula_units_Z            2
_cell_length_a                   12.22970(10)
_cell_length_b                   13.7829(2)
_cell_length_c                   21.3400(2)
_cell_measurement_reflns_used    78765
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      33.6330
_cell_measurement_theta_min      2.2870
_cell_volume                     3377.09(7)
_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 0.995
_diffrn_measured_fraction_theta_max 0.997
_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    -68.00 -11.00   0.50    1.50    --  -13.54 121.00 137.00  114
  2  \w    -89.00 -30.00   0.50    1.50    --  -13.54 155.00 -65.00  118
  3  \w     -8.00  90.00   0.50    1.50    --   13.07  57.00-150.00  196
  4  \w    -16.00  83.00   0.50    1.50    --   13.07  77.00  90.00  198
  5  \w    -25.00  67.00   0.50    1.50    --  -13.54  19.00-150.00  184
  6  \w    -25.00  67.00   0.50    1.50    --  -13.54  19.00   0.00  184
  7  \w    -25.00  67.00   0.50    1.50    --  -13.54  19.00  90.00  184
  8  \w    -19.00  29.00   0.50    1.50    --  -13.54 -99.00-150.00   96
  9  \w    -42.00  56.00   0.50    1.50    --  -13.54  77.00-120.00  196
 10  \w    -80.00 -21.00   0.50    1.50    --  -13.54 139.00 -95.67  118
 11  \w    -82.00 -23.00   0.50    1.50    --  -13.54 142.00  50.98  118
 12  \w    -94.00   7.00   0.50    1.50    --  -13.54 -38.00 -90.00  202
 13  \w    -62.00  88.00   0.50    1.50    --   13.07   0.00-180.00  300
 14  \w    -19.00  29.00   0.50    1.50    --  -13.54 -99.00  30.00   96
 15  \w    -74.00 -17.00   0.50    1.50    --  -13.54 130.00 -47.70  114
 16  \w    -74.00 -17.00   0.50    1.50    --  -13.54 130.00 139.18  114
 17  \w    -80.00 -21.00   0.50    1.50    --  -13.54 139.00-142.30  118
 18  \w    -19.00  29.00   0.50    1.50    --  -13.54 -99.00-180.00   96
 19  \w    -74.00 -17.00   0.50    1.50    --  -13.54 130.00 106.23  114
 20  \w    -19.00  29.00   0.50    1.50    --  -13.54 -99.00  60.00   96
 21  \w    -82.00 -23.00   0.50    1.50    --  -13.54 142.00 -15.77  118
 22  \w    -79.00 -21.00   0.50    1.50    --  -13.54 138.00-174.09  116
 23  \w    -62.00  56.00   0.50    1.50    --   13.07   0.00-150.00  236
;
_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      0.0171670000
_diffrn_orient_matrix_UB_12      0.0478879000
_diffrn_orient_matrix_UB_13      -0.0033780000
_diffrn_orient_matrix_UB_21      0.0192781000
_diffrn_orient_matrix_UB_22      0.0192256000
_diffrn_orient_matrix_UB_23      0.0349541000
_diffrn_orient_matrix_UB_31      0.0532233000
_diffrn_orient_matrix_UB_32      -0.0160671000
_diffrn_orient_matrix_UB_33      -0.0041052000
_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  0.0484
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            204216
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.095
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.579
_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    1.285
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.339
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         20582
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0880P)^2^+2.1478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1613
_refine_ls_wR_factor_ref         0.1769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14532
_reflns_number_total             20582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00889h2.cif
_cod_data_source_block           23eh150_amb-1121
_cod_depositor_comments
'Adding full bibliography for 7715639--7715655.cif.'
_cod_original_cell_volume        3377.08(7)
_cod_database_code               7715650
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C152  H168  Na8  Ni4  O12  '
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.855
_reflns_odcompleteness_completeness 99.97
_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
2. Restrained distances
 O4-C65 \\sim O4-C65A
 with sigma of 0.02
 C66-C65 \\sim C66-C65A
 with sigma of 0.02
 O3-C38 \\sim O3A-C38
 with sigma of 0.02
 O3-C35 \\sim O3A-C35
 with sigma of 0.02
 O3-C38A \\sim O3A-C38A
 with sigma of 0.02
 O3-C35A \\sim O3A-C35A
 with sigma of 0.02
 Na2-O3 \\sim Na2-O3A
 with sigma of 0.02
 O3-C38A \\sim O3A-C38 \\sim O3-C35A \\sim O3A-C35
 with sigma of 0.02
 C36A-C35A \\sim C36-C35 \\sim C38A-C37A \\sim C38-C37
 with sigma of 0.02
 C37A-C36A \\sim C37-C36
 with sigma of 0.02
 O1-C30 \\sim O1-C30A
 with sigma of 0.02
 C30-C29 \\sim C30A-C29A
 with sigma of 0.02
 C29-C28 \\sim C29A-C28A
 with sigma of 0.02
 C28A-C27 \\sim C28-C27
 with sigma of 0.02
3. Rigid bond restraints
 O5, C69, C70, C71, C72
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O6, C76, C75, C74, C73
 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(C65) \\sim Ueq, Uanis(C65A) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
Uanis(C73) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C74) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C75) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O3) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C35A)
\\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq,
Uanis(C37A) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C38A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
Uanis(C30) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C28A)
\\sim Ueq, Uanis(C29A) \\sim Ueq, Uanis(C30A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Others
 Sof(C65A)=Sof(H65C)=Sof(H65D)=1-FVAR(1)
 Sof(C65)=Sof(H65A)=Sof(H65B)=FVAR(1)
 Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(O3A)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=1-FVAR(2)
 Sof(O3)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C35)=
 Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(2)
 Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=
 Sof(H30C)=Sof(H30D)=1-FVAR(3)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C68(H68A,H68B), C27(H27A,H27B), C73(H73B,H73A), C66(H66A,H66B), C67(H67A,
 H67B), C76(H76A,H76B), C32(H32A,H32B), C31(H31A,H31B), C75(H75A,H75B),
 C69(H69A,H69B), C74(H74A,H74B), C30(H30A,H30B), C65(H65A,H65B), C70(H70A,H70B),
  C28(H28A,H28B), C33(H33A,H33B), C71(H71A,H71B), C72(H72A,H72B), C34(H34A,
 H34B), C29(H29A,H29B), C37(H37A,H37B), C38(H38A,H38B), C35(H35A,H35B),
 C36(H36A,H36B), C65A(H65C,H65D), C38A(H38C,H38D), C35A(H35C,H35D), C36A(H36C,
 H36D), C37A(H37C,H37D), C28A(H28C,H28D), C29A(H29C,H29D), C30A(H30C,H30D)
6.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C57(H57), C41(H41), C40(H40), C16(H16), C6(H6), C3(H3), C25(H25),
 C12(H12), C60(H60), C2(H2), C44(H44), C17(H17), C4(H4), C22(H22), C18(H18),
 C50(H50), C56(H56), C5(H5), C42(H42), C54(H54), C43(H43), C55(H55), C8(H8),
 C46(H46), C24(H24), C11(H11), C23(H23), C49(H49), C61(H61), C63(H63), C48(H48),
  C62(H62), C10(H10), C9(H9), C47(H47)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23483
_shelx_fab_checksum              48854
_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 1.167
_oxdiff_exptl_absorpt_empirical_full_min 0.884