Hemi{tris(picolinic acid-κ^2^<i>N</i>,<i>O</i>)iron(II)/tris(picolinato-κ^2^<i>N</i>,<i>O</i>)iron(II)} hemi(tetrafluoroborate)
Onggo, Djulia; Martak, Fatimah; Ismunandar; Yamin, Bohari M.; Ng, Seik Weng; Acta Crystallographica Section E 62 (2006) m1112–m1113; doi:10.1107/S1600536806014000

data_2208804
_publ_section_title
;Hemi{tris(picolinic
 acid-\k^2^<i>N</i>,<i>O</i>)iron(II)/tris(picolinato-\k^2^<i>N</i>,<i>O</i>)iron(II)}
 hemi(tetrafluoroborate)
;
_journal_coeditor_code           BT2049
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1112
_journal_page_last               m1113
_journal_paper_doi               10.1107/S1600536806014000
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'[Fe (C6 H4 N O2) (C6 H4.5 N O2) (C6 H5 N O2)] (B F4)0.5'
_chemical_formula_moiety
'[Fe (C6 H4 N O2) (C6 H4.5 N O2) (C6 H5 N O2)] 0.5+, 0.5B F4 -'
_chemical_formula_sum            'C18 H13.5 B0.5 F2 Fe N3 O6'
_chemical_formula_weight         467.07
_chemical_name_systematic
;
Hemi{tris(picolinic acid-\k^2^<i>N</i>,<i>O</i>)iron(II)/tris(picolinato-
\k^2^<i>N</i>,<i>O</i>)iron(II)} hemi(tetrafluoroborate)
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_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            2
_cell_length_a                   13.564(2)
_cell_length_b                   13.564
_cell_length_c                   6.0108(9)
_cell_measurement_reflns_used    724
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.4
_cell_measurement_theta_min      3.0
_cell_volume                     957.7(2)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Bruker APEX area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.062
_diffrn_reflns_av_sigmaI/netI    0.046
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4988
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.7
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.21
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1128
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.21
_refine_ls_R_factor_all          0.071
_refine_ls_R_factor_gt           0.065
_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^)+(0.0655P)^2^+1.2441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.151
_refine_ls_wR_factor_ref         0.154
_reflns_number_gt                1055
_reflns_number_total             1128
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2049.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2208804
_cod_database_fobs_code          2208804