Syntheses, Structures and Magnetic Properties of Tetranuclear Cubane-type and Heptanuclear Wheel-type Nickel(II) Complexes with 3-Methoxysalicylic Acid Derivatives
Kobayashi, Fumiya; Ohtani, Ryo; Teraoka, Saki; Kosaka, Wataru; Miyasaka, Hitoshi; Zhang, Yingjie; Lindoy, Leonard F.; Hayami, Shinya; Nakamura, Masaaki; Dalton Trans.  (2017) –; doi:10.1039/C7DT01757J

data_7043239
_publ_section_title
;
 Syntheses, Structures and Magnetic Properties of Tetranuclear Cubane-type
 and Heptanuclear Wheel-type Nickel(II) Complexes with 3-Methoxysalicylic
 Acid Derivatives
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01757J
_journal_year                    2017
_chemical_formula_moiety         '1(C108 H120 N12 Ni7 O24), 2(Cl), 0.25(H2 O)'
_chemical_formula_sum            'C108 H120.5 Cl2 N12 Ni7 O24.25'
_chemical_formula_weight         2456.48
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-04 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4.00008
_cell_length_a                   22.615(3)
_cell_length_b                   22.615(3)
_cell_length_c                   22.615(3)
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.478
_cell_measurement_theta_min      2.014
_cell_volume                     11566(3)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ADSC Quantum Detector'
_diffrn_measurement_method       '\p  scans'
_diffrn_radiation_type
'silicon double crystal monochromated synchrotron'
_diffrn_radiation_wavelength     0.71074
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            181274
_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         27.475
_diffrn_reflns_theta_min         2.014
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       needle
_exptl_crystal_F_000             5106
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.166
_refine_diff_density_min         -1.525
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0049(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         4427
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0678
_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^)+(0.1256P)^2^+11.6427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.2084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3505
_reflns_number_total             4427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01757j2.cif
_cod_data_source_block           Ni7
_cod_original_cell_volume        11566(4)
_cod_original_formula_sum        'C108 H120.50 Cl2 N12 Ni7 O24.25'
_cod_database_code               7043239
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C12, C17, C16, C15, C14, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C12 \\sim C17 \\sim C16 \\sim C15 \\sim C14 \\sim C13: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(O4) = Uanis(C18)
4. Others
 Fixed Sof: O1W(0.04167)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C4(H4), C5(H5), C6(H6), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              9211
_olex2_submission_special_instructions 'No special instructions were received'