O,N-Coordinated o-iminobenzoquinone and o-iminobenzosemiquinonato(1‒) ligands in complexes of Ni(ii), Co(iii) and Fe(iii)
Sik Min, Kil; Weyhermüller, Thomas; Wieghardt, Karl; Dalton Transactions  (2003) 1126–; doi:10.1039/b211698g

data_7012530
_publ_section_title
;
 O,N-Coordinated o-iminobenzoquinone and o-iminobenzosemiquinonato(1--)
 ligands in complexes of Ni(ii), Co(iii) and Fe(iii)
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1126
_journal_paper_doi               10.1039/b211698g
_journal_year                    2003
_chemical_formula_analytical
'[C26 H40 N5 O1 Fe]2+, 2 (CLO4)-, 0.5 CH3OH, 0.5 H2O'
_chemical_formula_sum            'C26.5 H46 Cl2 Fe N5 O10'
_chemical_formula_weight         721.43
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 113.60(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.8198(3)
_cell_length_b                   21.0452(6)
_cell_length_c                   20.6800(6)
_cell_measurement_reflns_used    142490
_cell_measurement_temperature    100(2)
_cell_volume                     6708.0(6)
_computing_cell_refinement       'DENZO, Nonius Collect Software'
_computing_data_collection       'DENZO, Nonius Collect Software'
_computing_data_reduction        'DENZO, Nonius Collect Software'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius Kappa-CCD'
_diffrn_measurement_method       '554 images at 1 deg. in \w and 30 sec.'
_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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            82667
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         3.39
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_type   'not corrected'
_exptl_crystal_colour            'deep blue'
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.36
_refine_diff_density_max         1.341
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         21139
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.081
_refine_ls_restrained_S_obs      1.097
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_obs          0.0603
_refine_ls_shift/esd_max         -0.383
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+10.4200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1595
_refine_ls_wR_factor_obs         0.1465
_reflns_number_observed          17467
_reflns_number_total             21218
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b211698g.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+10.4200P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+10.4200P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6708.0(3)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C26.50 H46 Cl2 Fe N5 O10'
_cod_database_code               7012530