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_7715644
_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         'C38 H52 N4 Na2 Ni'
_chemical_formula_sum            'C38 H52 N4 Na2 Ni'
_chemical_formula_weight         669.52
_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             2023-09-28
_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                 94.8440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5871(2)
_cell_length_b                   22.0003(3)
_cell_length_c                   16.2275(2)
_cell_measurement_reflns_used    37271
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.7360
_cell_measurement_theta_min      2.2290
_cell_volume                     3766.20(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      100.00(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 0.998
_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    -78.00 -20.00   0.50   10.00    --  -13.54 137.00  11.00  116
  2  \w    -75.00 -18.00   0.50   10.00    --  -13.54 133.00-166.00  114
  3  \w    -18.00  54.00   0.50   10.00    --   13.07 -99.00-120.00  144
  4  \w    -64.00  35.00   0.50   10.00    --   13.07 -57.00   0.00  198
  5  \w     -7.00  94.00   0.50   10.00    --   13.07  38.00 150.00  202
  6  \w    -19.00  29.00   0.50   10.00    --  -13.54 -99.00 120.00   96
  7  \w    -87.00 -42.00   0.50   10.00    --  -13.54-178.00-180.00   90
  8  \w    -19.00  29.00   0.50   10.00    --  -13.54 -99.00-120.00   96
  9  \w     -8.00  90.00   0.50   10.00    --   13.07  57.00  30.00  196
 10  \w    -18.00   7.00   0.50   10.00    --   13.07 -99.00   0.00   50
 11  \w    -18.00  54.00   0.50   10.00    --   13.07 -99.00 150.00  144
 12  \w    -87.00 -42.00   0.50   10.00    --  -13.54-178.00  30.00   90
 13  \w    -94.00   7.00   0.50   10.00    --  -13.54 -38.00-150.00  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      0.0228440000
_diffrn_orient_matrix_UB_12      -0.0302633000
_diffrn_orient_matrix_UB_13      -0.0014196000
_diffrn_orient_matrix_UB_21      0.0625124000
_diffrn_orient_matrix_UB_22      0.0111358000
_diffrn_orient_matrix_UB_23      -0.0022213000
_diffrn_orient_matrix_UB_31      0.0095762000
_diffrn_orient_matrix_UB_32      -0.0004145000
_diffrn_orient_matrix_UB_33      0.0437702000
_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  0.0436
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            114953
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.141
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         11482
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.9235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8371
_reflns_number_total             11482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00889h2.cif
_cod_data_source_block           23eh196_amb-1137-2
_cod_depositor_comments
'Adding full bibliography for 7715639--7715655.cif.'
_cod_database_code               7715644
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C152  H204  N16  Na8  Ni4  Mn1  '
_chemical_oxdiff_usercomment     AMB-1137-2
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.864
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-C18A \\sim N2-C18
 with sigma of 0.02
 N4-C24 \\sim N4-C24A
 with sigma of 0.02
 N4-C23A \\sim N4-C23
 with sigma of 0.02
 N1-C14A \\sim N1-C14
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C16A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C21A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18A) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C23A) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C24)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14A) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C16A)=Sof(H16C)=Sof(H16D)=1-FVAR(1)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=FVAR(1)
 Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=1-FVAR(2)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22B)=Sof(H22A)=FVAR(2)
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(3)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(3)
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=1-FVAR(4)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=
 FVAR(4)
 Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(5)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(5)
5.a Ternary CH refined with riding coordinates:
 C25(H25), C26(H26), C27(H27)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C21(H21A,H21B), C22(H22B,H22A), C16(H16A,H16B), C15A(H15C,
 H15D), C16A(H16C,H16D), C22A(H22C,H22D), C21A(H21C,H21D)
5.c Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C13(H13B,H13C,H13A), C24(H24A,H24B,H24C), C23(H23A,H23B,
 H23C), C18(H18A,H18B,H18C), C18A(H18D,H18E,H18F), C24A(H24D,H24E,H24F),
 C23A(H23D,H23E,H23F), C14A(H14D,H14E,H14F)
5.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C37(H37), C12(H12), C10(H10), C11(H11), C2(H2), C30(H30),
 C35(H35), C28(H28), C6(H6), C32(H32), C34(H34), C4(H4), C5(H5), C3(H3),
 C33(H33)
5.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              95515
_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 1.188
_oxdiff_exptl_absorpt_empirical_full_min 0.759