A rod-like hexanuclear nickel cluster based on a bi(pyrazole-alcohol) ligand: structure, electrospray ionization mass spectrometry, magnetism and photocurrent response
Sheng, Kai; Ji, Bao-Qian; Feng, Lei; Su, Yan-Min; Jagodič, Marko; Jagličić, Zvonko; Sun, Di; New Journal of Chemistry 44 (2020) 7152–7157; doi:10.1039/D0NJ00959H

data_7059461
_publ_section_title
;
 A rod-like hexanuclear nickel cluster based on a bi(pyrazole-alcohol)
 ligand: structure, electrospray ionization mass spectrometry, magnetism
 and photocurrent response
;
_journal_issue                   17
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7152
_journal_page_last               7157
_journal_paper_doi               10.1039/D0NJ00959H
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C40 H64 N8 Ni6 O24, 4(C2 H6 O), 2(C2 H5 O)'
_chemical_formula_sum            'C52 H98 N8 Ni6 O30'
_chemical_formula_weight         1667.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-27 deposited with the CCDC.	2020-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.4801(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.039(3)
_cell_length_b                   12.0094(11)
_cell_length_c                   22.276(2)
_cell_measurement_reflns_used    4092
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.768
_cell_measurement_theta_min      2.225
_cell_volume                     7229.0(12)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23345
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         1.856
_exptl_absorpt_coefficient_mu    1.616
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10'
_exptl_crystal_colour            'clear yellowish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       block
_exptl_crystal_F_000             3496
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+21.5838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5453
_reflns_number_total             7379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00959h2.cif
_cod_data_source_block           p
_cod_depositor_comments
;Adding full bibliography for 7059461.cif.

 Adding full bibliography for 7059461.cif.
;
_cod_original_cell_volume        7229.0(11)
_cod_database_code               7059461
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.895
_exptl_absorpt_special_details
'The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.34133   26.749    8.343    9.630   89.989  110.974   89.992'
_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, All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O11(H11A,H11B)
2.b Rotating group:
 O12(H12A,H12B)
2.c Ternary CH refined with riding coordinates:
 C6(H6), C7(H7)
2.d Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C24(H24A,H24B)
2.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C26(H26)
2.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C12(H12C,H12D,H12E),
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C)
2.g Idealised tetrahedral OH refined as rotating group:
 O13(H13), O14(H14), O15(H15)
;
_shelx_res_checksum              19013
_olex2_submission_special_instructions 'No special instructions were received'