Tetranuclear Nickel(II) Complex with an Unsymmetrical Pentadentate Schiff-base Ligand Having a Defective Double-Cubane Core
MIKURIYA, Masahiro; TAKEUCHI, Masahiro; YOSHIOKA, Daisuke; X-ray Structure Analysis Online 33 (2017) 31–; doi:10.2116/xraystruct.33.31

data_1551573
_publ_section_title
;
 Tetranuclear Nickel(II) Complex with an Unsymmetrical Pentadentate
 Schiff-base Ligand Having a Defective Double-Cubane Core
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              31
_journal_paper_doi               10.2116/xraystruct.33.31
_journal_volume                  33
_journal_year                    2017
_chemical_formula_sum            'C34 H48 N4 Ni4 O10'
_chemical_formula_weight         907.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 112.214(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.154(3)
_cell_length_b                   11.821(3)
_cell_length_c                   15.945(4)
_cell_measurement_reflns_used    3819
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.378
_cell_measurement_theta_min      2.207
_cell_volume                     2120.8(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12433
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.378
_diffrn_reflns_theta_min         2.207
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.802
_exptl_absorpt_correction_T_max  0.614
_exptl_absorpt_correction_T_min  0.365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         5069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0588P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3516
_reflns_number_total             5069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            33_31_1.txt
_cod_data_source_block           nil11m_0m_sq
_cod_original_cell_volume        2120.9(9)
_cod_database_code               1551573
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.365
_shelx_estimated_absorpt_t_max   0.614
_shelx_res_checksum              37139
_shelx_hkl_checksum              87172
_shelx_fab_checksum              2998