Structural Variation from Heterometallic Heptanuclear, Heptanuclear to Cubane Clusters Based on 2-hydroxy-3-ethoxy-benzaldehyde: Effects of pH and Temperature
zhang, shu hua; Zhao, Ru-Xiao; li, gui; ZHANG, hai yang; Zhang, Chun Lian; Muller, Gilles; RSC Adv.  (2014) –; doi:10.1039/C4RA09687H

data_7218416
_publ_section_title
;
 Structural Variation from Heterometallic Heptanuclear, Heptanuclear to
 Cubane Clusters Based on 2-hydroxy-3-ethoxy-benzaldehyde: Effects of pH
 and Temperature
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA09687H
_journal_year                    2014
_chemical_formula_moiety         'C60 H72 Ni7 O24, 2(Cl O4) '
_chemical_formula_sum            'C60 H72 Cl2 Ni7 O32'
_chemical_formula_weight         1786.95
_space_group_IT_number           147
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   14.6487(7)
_cell_length_b                   14.6487(7)
_cell_length_c                   9.6629(5)
_cell_measurement_reflns_used    1423
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.478
_cell_measurement_theta_min      3.833
_cell_volume                     1795.71(15)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3860
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         3.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.956
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2124
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+3.0726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                1602
_reflns_number_total             2128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra09687h2.cif
_cod_data_source_block           ni2
_cod_original_cell_volume        1795.7(2)
_cod_database_code               7218416