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_7043238
_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         'C68 H80 Ni4 O24'
_chemical_formula_sum            'C68 H80 Ni4 O24'
_chemical_formula_weight         1516.16
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-06-04 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.54(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.105(3)
_cell_length_b                   25.712(5)
_cell_length_c                   16.804(3)
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      1.449
_cell_volume                     6952(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BLU-ICE (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 0.947
_diffrn_measured_fraction_theta_max 0.938
_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  0.0788
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            112825
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.449
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    1.145
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       needle
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.00513(18)
_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   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     890
_refine_ls_number_reflns         14970
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0610P)^2^+9.8500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10951
_reflns_number_total             14970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01757j2.cif
_cod_data_source_block           Ni4
_cod_database_code               7043238
_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
2. Restrained distances
 O23-H23
 0.85 with sigma of 0.01
 O17-H17
 0.85 with sigma of 0.01
 O24-H24
 0.85 with sigma of 0.01
 O22-H22
 0.85 with sigma of 0.01
 C67-H23
 1.891831 with sigma of 0.02
 Ni4-H23
 2.675256 with sigma of 0.02
 C61-H17
 1.882386 with sigma of 0.02
 Ni1-H17
 2.657736 with sigma of 0.02
 C68-H24
 1.888604 with sigma of 0.02
 Ni2-H24
 2.673646 with sigma of 0.02
 C66-H22
 1.851453 with sigma of 0.02
 Ni3-H22
 2.640382 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C24(H24A,H24B), C39(H39A,H39B), C54(H54A,H54B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15),
 C19(H19), C20(H20), C21(H21), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C34(H34), C35(H35), C36(H36), C41(H41), C42(H42), C43(H43), C44(H44),
 C45(H45), C49(H49), C50(H50), C51(H51), C56(H56), C57(H57), C58(H58), C59(H59),
  C60(H60)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C31(H31A,H31B,H31C), C46(H46A,H46B,
 H46C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,
 H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C68(H68A,H68B,H68C)
;
_shelx_res_checksum              52626
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'