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_7715649
_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         'C45 H61 Li2 N Ni O5'
_chemical_formula_sum            'C45 H61 Li2 N Ni O5'
_chemical_formula_weight         768.53
_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             2023-10-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-17 deposited with the CCDC.	2024-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.5490(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.61066(4)
_cell_length_b                   10.14415(4)
_cell_length_c                   39.27151(16)
_cell_measurement_reflns_used    59561
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      80.6230
_cell_measurement_theta_min      4.4070
_cell_volume                     4213.72(3)
_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      173.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  19.00   0.50    0.80    --  -50.83  96.00 104.00  194
  2  \w     -7.00  78.00   0.50    0.80    --   50.83 -96.00  -4.00  170
  3  \w   -160.00 -84.00   0.50    3.40    --  -90.00 -96.00  -4.00  152
  4  \w    -79.00 -20.00   0.50    3.40    --  -90.00  96.00 104.00  118
  5  \w     42.00 105.00   0.50    3.40    --  111.50 -96.00  -4.00  126
  6  \w    106.00 178.00   0.50    3.40    --  111.50  96.00 104.00  144
  7  \w    -99.00 -44.00   0.50    0.80    --  -50.83   0.00 -90.00  110
  8  \w    -26.00  21.00   0.50    0.80    --  -50.83  19.00 -60.00   94
  9  \w    -43.00  20.00   0.50    0.80    --  -50.83  38.00  60.00  126
 10  \w    -43.00  20.00   0.50    0.80    --  -50.83  38.00 -90.00  126
 11  \w    -26.00  21.00   0.50    0.80    --  -50.83  19.00  30.00   94
 12  \w   -119.00 -73.00   0.50    0.80    --  -50.83-125.00  60.00   92
 13  \w   -119.00 -73.00   0.50    0.80    --  -50.83-125.00-180.00   92
 14  \w    -20.00  63.00   0.50    0.80    --   50.83 -57.00  60.00  166
 15  \w    -51.00 -18.00   0.50    3.40    --  -90.00  45.00  30.00   66
 16  \w    -51.00 -18.00   0.50    3.40    --  -90.00  45.00 -60.00   66
 17  \w   -138.00 -83.00   0.50    3.40    --  -90.00   0.00-120.00  110
 18  \w    104.00 178.00   0.50    3.40    --  111.50  45.00  90.00  148
 19  \w     41.00  71.00   0.50    3.40    --  111.50 -61.00   0.00   60
 20  \w     41.00  71.00   0.50    3.40    --  111.50 -61.00 -30.00   60
 21  \w     42.00 113.00   0.50    3.40    --  111.50-126.00   3.67  142
 22  \w     41.00 106.00   0.50    3.40    --  111.50 -94.00 150.00  130
 23  \w     41.00  71.00   0.50    3.40    --  111.50 -61.00 -90.00   60
 24  \w     41.00  71.00   0.50    3.40    --  111.50 -61.00 150.00   60
 25  \w     95.00 178.00   0.50    3.40    --  111.50 125.00  60.00  166
 26  \w    107.00 178.00   0.50    3.40    --  111.50  15.00  90.00  142
 27  \w     43.00 108.00   0.50    3.40    --  111.50-110.00  57.18  130
 28  \w     43.00 111.00   0.50    3.40    --  111.50-125.00-120.00  136
 29  \w     41.00 105.00   0.50    3.40    --  111.50 -77.00  60.00  128
 30  \w    107.00 178.00   0.50    3.40    --  111.50  15.00 -60.00  142
 31  \w     41.00  71.00   0.50    3.40    --  111.50 -61.00  60.00   60
 32  \w    107.00 178.00   0.50    3.40    --  111.50  15.00-150.00  142
 33  \w     92.00 178.00   0.50    3.40    --  111.50  77.00  90.00  172
 34  \w     44.00 111.00   0.50    3.40    --  111.50-125.00 -30.00  134
 35  \w     43.00  86.00   0.50    3.40    --  111.50-125.00  90.00   86
 36  \w     45.00 106.00   0.50    3.40    --  111.50-102.00 137.61  122
 37  \w     45.00  70.00   0.50    3.40    --  111.50 -61.00-120.00   50
 38  \w    136.00 163.00   0.50    3.40    --  111.50 125.00  30.00   54
 39  \w     99.00 170.00   0.50    3.40    --  111.50  61.00-120.00  142
 40  \w     46.00  72.00   0.50    3.40    --  111.50 -77.00   0.00   52
 41  \w    107.00 178.00   0.50    3.40    --  111.50  15.00-120.00  142
 42  \w     83.00 108.00   0.50    3.40    --  111.50-110.00  99.66   50
 43  \w     86.00 111.00   0.50    3.40    --  111.50-125.00 150.00   50
 44  \w     83.00 108.00   0.50    3.40    --  111.50-108.00 -15.26   50
 45  \w     47.00  81.00   0.50    3.40    --  111.50-125.00 150.00   68
 46  \w     42.00 101.00   0.50    3.40    --  111.50 -94.00-180.00  118
 47  \w     51.00 108.00   0.50    3.40    --  111.50-106.00  79.36  114
 48  \w     45.00 109.00   0.50    3.40    --  111.50-113.00 -80.83  128
 49  \w     77.00 103.00   0.50    3.40    --  111.50 -94.00-150.00   52
 50  \w     74.00 106.00   0.50    3.40    --  111.50 -94.00-120.00   64
 51  \w     98.00 176.00   0.50    3.40    --  111.50  61.00 -60.00  156
 52  \w     46.00  77.00   0.50    3.40    --  111.50-110.00  99.66   62
 53  \w     46.00  86.00   0.50    3.40    --  111.50-125.00 -90.00   80
 54  \w    108.00 173.00   0.50    3.40    --  111.50  30.00 120.00  130
 55  \w     63.00 118.00   0.50    3.40    --  111.50   0.00  90.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0362298000
_diffrn_orient_matrix_UB_12      -0.1120022000
_diffrn_orient_matrix_UB_13      -0.0238564000
_diffrn_orient_matrix_UB_21      0.0221152000
_diffrn_orient_matrix_UB_22      0.1017165000
_diffrn_orient_matrix_UB_23      -0.0280372000
_diffrn_orient_matrix_UB_31      0.1393310000
_diffrn_orient_matrix_UB_32      0.0129511000
_diffrn_orient_matrix_UB_33      0.0139164000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            87197
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.494
_diffrn_reflns_theta_min         2.257
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.467
_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    1.211
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         8616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0567P)^2^+2.0158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8185
_reflns_number_total             8616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00889h2.cif
_cod_data_source_block           23eh309_amb-1221
_cod_depositor_comments
'Adding full bibliography for 7715639--7715655.cif.'
_cod_database_code               7715649
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C180  H244  Li8  N4  Ni4  O20  '
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.795
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C26(H26A,H26B), C34(H34A,H34B), C36(H36A,H36B), C30(H30A,
 H30B), C38(H38A,H38B), C41(H41A,H41B), C33(H33A,H33B), C39(H39A,H39B),
 C29(H29A,H29B), C35(H35A,H35B), C40(H40A,H40B), C31(H31A,H31B), C42(H42A,H42B),
  C45(H45A,H45B), C32(H32A,H32B), C27(H27A,H27B), C43(H43A,H43B), C28(H28A,
 H28B), C44(H44A,H44B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C9(H9), C7(H7), C21(H21), C12(H12), C3(H3), C24(H24), C10(H10),
 C5(H5), C11(H11), C6(H6), C23(H23), C22(H22), C4(H4), C17(H17), C19(H19),
 C15(H15), C18(H18), C16(H16)
;
_shelx_res_checksum              93157
_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 1.187
_oxdiff_exptl_absorpt_empirical_full_min 0.876