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_7030578
_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            'C48.5 H81 N4 Ni6 O26'
_chemical_formula_weight         1488.43
_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                81.176(2)
_cell_angle_beta                 77.741(2)
_cell_angle_gamma                74.981(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0545(6)
_cell_length_b                   13.1060(6)
_cell_length_c                   22.7396(11)
_cell_measurement_reflns_used    5223
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      25.748
_cell_measurement_theta_min      2.1905
_cell_volume                     3092.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      91(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Kappa Apex II area detector'
_diffrn_measurement_method       '\f and \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  0.0850
_diffrn_reflns_av_sigmaI/netI    0.1173
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40197
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    1.872
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE (Bruker AXS Inc.)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         12544
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0772
_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^)+(0.0336P)^2^+13.4223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1678
_reflns_number_gt                8429
_reflns_number_total             12544
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7001006
_cod_data_source_file            b821782c.txt
_cod_data_source_block           hf30
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C48.50 H81 N4 Ni6 O26'
_cod_database_code               7030578