Hexa-, hepta- and dodeca-nuclear nickel(II) complexes of three Schiff-base ligands derived from 1,4-diformyl-2,3-dihydroxybenzene
Feltham, Humphrey L. C.; Clérac, Rodolphe; Brooker, Sally; Dalton Transactions  (2009) 2965–2973; doi:10.1039/b821782c

data_7030579
_publ_section_title
;
 Hexa-, hepta- and dodeca-nuclear nickel(II) complexes of three
 Schiff-base ligands derived from 1,4-diformyl-2,3-dihydroxybenzene
;
_journal_coden_ASTM              DTARAF
_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              2965
_journal_page_last               2973
_journal_paper_doi               10.1039/b821782c
_journal_year                    2009
_chemical_formula_sum            'C126.5 H105 N12 Ni12 O34'
_chemical_formula_weight         3041.75
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.269(5)
_cell_angle_beta                 73.420(5)
_cell_angle_gamma                66.534(5)
_cell_formula_units_Z            2
_cell_length_a                   19.330(3)
_cell_length_b                   19.357(3)
_cell_length_c                   22.798(3)
_cell_measurement_reflns_used    5578
_cell_measurement_temperature    92(2)
_cell_measurement_theta_max      28.86
_cell_measurement_theta_min      2.28
_cell_volume                     7499.5(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      92(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa Apex II area detector'
_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  0.1087
_diffrn_reflns_av_sigmaI/netI    0.1602
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54771
_diffrn_reflns_theta_full        22.46
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    1.539
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE (Bruker AXS Inc.)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         1.030
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         19426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1712
_refine_ls_R_factor_gt           0.1268
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1305P)^2^+130.5465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2979
_refine_ls_wR_factor_ref         0.3206
_reflns_number_gt                12798
_reflns_number_total             19426
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7001007
_cod_data_source_file            b821782c.txt
_cod_data_source_block           hf79sq
_cod_original_cell_volume        7499.4(17)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C126.50 H105 N12 Ni12 O34'
_cod_database_code               7030579