Synthetic, structural, electrochemical and solvent extraction studies of neutral trinuclear Co(ii), Ni(ii), Cu(ii) and Zn(ii) metallocycles and tetrahedral tetranuclear Fe(iii) species incorporating 1,4-aryl-linked bis-β-diketonato ligands
Clegg, Jack K.; Bray, David J.; Gloe, Kerstin; Gloe, Karsten; Jolliffe, Katrina A.; Lawrance, Geoffrey A.; Lindoy, Leonard F.; Meehan, George V.; Wenzel, Marco; Dalton Transactions  (2008) 1331–1340; doi:10.1039/b716653b

data_7003488
_publ_section_title
;
 Synthetic, structural, electrochemical and solvent extraction studies
 of neutral trinuclear Co(ii), Ni(ii), Cu(ii) and Zn(ii) metallocycles
 and tetrahedral tetranuclear Fe(iii) species incorporating
 1,4-aryl-linked bis-\b-diketonato ligands
;
_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              1331
_journal_page_last               1340
_journal_paper_doi               10.1039/b716653b
_journal_year                    2008
_chemical_formula_moiety         '(C90 H102 N6 Ni3 O12), 3.5(C5 H5 N)'
_chemical_formula_sum            'C107.5 H119.5 N9.5 Ni3 O12'
_chemical_formula_weight         1912.76
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                104.688(8)
_cell_angle_beta                 93.275(8)
_cell_angle_gamma                98.843(7)
_cell_formula_units_Z            2
_cell_length_a                   8.9493(10)
_cell_length_b                   23.585(3)
_cell_length_c                   26.145(3)
_cell_measurement_reflns_used    3927
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.026
_cell_measurement_theta_min      2.34
_cell_volume                     5247.9(11)
_computing_cell_refinement       'SAINT (Bruker-Nonius, 2003)'
_computing_data_collection       'APEX (Bruker-Nonius, 2003)'
_computing_data_reduction
'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)'
_computing_molecular_graphics
;ORTEP-3 (Farrugia, 1997)
WINGX-32 (Farrugia, 1999)
;
_computing_publication_material  'enCIFer 1.1 (CCDC, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  APEXII-FR591
_diffrn_measurement_method       \w+\f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2848
_diffrn_reflns_av_sigmaI/netI    0.1526
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            127447
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         1.37
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2022
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.930
_refine_diff_density_min         -1.526
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.0032(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1048
_refine_ls_number_reflns         12860
_refine_ls_number_restraints     783
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1943
_refine_ls_R_factor_gt           0.0913
_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^)+(0.1690P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2253
_refine_ls_wR_factor_ref         0.2723
_reflns_number_gt                6417
_reflns_number_total             12860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b716653b.txt
_cod_data_source_block           lj222sad
_cod_depositor_comments
;
The following automatic conversions were performed:
data name '_symmetry_intl_tables_number' replaced with
'_symmetry_Int_Tables_number' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_cell_volume        5247.8(11)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C107.50 H119.50 N9.50 Ni3 O12'
_cod_database_code               7003488