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_7715652
_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         'C37 H50 K2 Ni O7'
_chemical_formula_sum            'C37 H50 K2 Ni O7'
_chemical_formula_weight         743.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 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                 98.4080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.5914(4)
_cell_length_b                   15.6226(2)
_cell_length_c                   19.9575(3)
_cell_measurement_reflns_used    54386
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      33.5360
_cell_measurement_theta_min      2.3560
_cell_volume                     8201.8(2)
_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_temperature      100.15
_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    -36.00  51.00   0.50    1.00    --   13.22 -92.00  69.00  174
  2  \w    -51.00  40.00   0.50    1.00    --  -13.69  92.00-177.00  182
  3  \w    -35.00  23.00   0.50    1.00    --  -13.69 -92.00  69.00  116
  4  \w     -8.00  90.00   0.50    1.00    --   13.22  57.00   0.00  196
  5  \w     -8.00  90.00   0.50    1.00    --   13.22  57.00-150.00  196
  6  \w    -56.00  42.00   0.50    1.00    --   13.22 -77.00-120.00  196
  7  \w    -25.00  67.00   0.50    1.00    --  -13.69  19.00 -30.00  184
  8  \w    -18.00  54.00   0.50    1.00    --   13.22 -99.00 120.00  144
  9  \w    -18.00  54.00   0.50    1.00    --   13.22 -99.00 -30.00  144
 10  \w    -19.00  28.00   0.50    1.00    --  -13.69 -99.00-150.00   94
 11  \w    -19.00   6.00   0.50    1.00    --  -13.69 -99.00   0.00   50
 12  \w    -87.00 -42.00   0.50    1.00    --  -13.69-178.00  30.00   90
;
_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      0.0143450000
_diffrn_orient_matrix_UB_12      0.0336645000
_diffrn_orient_matrix_UB_13      0.0173423000
_diffrn_orient_matrix_UB_21      -0.0201474000
_diffrn_orient_matrix_UB_22      0.0083632000
_diffrn_orient_matrix_UB_23      0.0187638000
_diffrn_orient_matrix_UB_31      0.0107321000
_diffrn_orient_matrix_UB_32      -0.0292848000
_diffrn_orient_matrix_UB_33      0.0252679000
_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  0.0359
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            121855
_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         30.034
_diffrn_reflns_theta_min         2.167
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.795
_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    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.393
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.168
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         12004
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0513P)^2^+5.7371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10154
_reflns_number_total             12004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00889h2.cif
_cod_data_source_block           23eh192_amb-1150-dme
_cod_depositor_comments
'Adding full bibliography for 7715639--7715655.cif.'
_cod_database_code               7715652
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C312  H440  K16  Ni8  O60  '
_chemical_oxdiff_usercomment     AMB-1150_DME
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.766
_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
 O4-C30 \\sim O4A-C30A
 with sigma of 0.02
 O4-C31 \\sim O4A-C31A
 with sigma of 0.02
 C32-C31 \\sim C32A-C31A
 with sigma of 0.02
 O5-C32 \\sim O5A-C32A
 with sigma of 0.02
 O5-C33 \\sim O5A-C33A
 with sigma of 0.02
3. Rigid bond restraints
 C31A, O4A, C30A
 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(C30) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O4A)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C32A) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C33A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.01
5. Others
 Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(O4A)=Sof(C31A)=Sof(H31C)=
 Sof(H31D)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(O5A)=Sof(C33A)=Sof(H33D)=Sof(H33E)=
 Sof(H33F)=1-FVAR(1)
 Sof(O4)=Sof(O5)=Sof(C31)=Sof(H31B)=Sof(H31A)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C30)=Sof(H30B)=Sof(H30A)=Sof(H30C)=
 FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C27(H27A,H27B), C36(H36A,H36B), C35(H35A,H35B), C31(H31B,
 H31A), C32(H32A,H32B), C31A(H31C,H31D), C32A(H32C,H32D)
6.b Me refined with riding coordinates:
 C33(H33A,H33B,H33C), C30(H30B,H30A,H30C), C30A(H30D,H30E,H30F), C33A(H33D,
 H33E,H33F)
6.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C15(H15), C11(H11), C8(H8), C25(H25), C2(H2), C21(H21),
 C19(H19), C9(H9), C6(H6), C3(H3), C16(H16), C17(H17), C18(H18), C24(H24),
 C23(H23), C4(H4), C5(H5)
6.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C34(H34A,H34B,H34C), C37(H37A,H37B,
 H37C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90355
_shelx_fab_checksum              57827
_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 1.508
_oxdiff_exptl_absorpt_empirical_full_min 0.616