Bis(4-carboxypyridinium) aquapentakis(isothiocyanato-κ<i>N</i>)iron(III) bis(pyridinium-4-carboxylate)
Li, Xiu-Ling; Lu, Zai-Sheng; Niu, De-Zhong; Acta Crystallographica Section E 63 (2007) m2640–m2640; doi:10.1107/S1600536807047460

data_2216180
_publ_section_title
;
 Bis(4-carboxypyridinium)
 aquapentakis(isothiocyanato-\k<i>N</i>)iron(III)
 bis(pyridinium-4-carboxylate)
;
_journal_coeditor_code           ZL2066
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2640
_journal_page_last               m2640
_journal_paper_doi               10.1107/S1600536807047460
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'(C6 H6 N O2)2 [Fe (N C S)5 (H2 O1)], 2C6 H5 N O2'
_chemical_formula_moiety
'2(C6 H6 N O2 +), C5 H2 Fe N5 O S5 2-, 2(C6 H5 N O2)'
_chemical_formula_sum            'C29 H24 Fe N9 O9 S5'
_chemical_formula_weight         858.72
_chemical_name_systematic
;
Bis(4-carboxypyridinium) aquapentakis(isothiocyanato-\k<i>N</i>)iron(III)
bis(pyridinium-4-carboxylate)
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8713(3)
_cell_length_b                   21.0882(3)
_cell_length_c                   11.9741(2)
_cell_measurement_reflns_used    6815
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      1.93
_cell_volume                     3755.18(11)
_computing_cell_refinement
'SMART (Siemens, 1996) and SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction
'SAINT (Siemens, 1996) and XPREP (Siemens, 1995)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_computing_publication_material  'SHELXTL (Bruker, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART CCD'
_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  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18247
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  0.8658
_exptl_absorpt_correction_T_min  0.7760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'purple red'
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.618
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0491
_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^)+(0.054P)^2^+5.0802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                2589
_reflns_number_total             3405
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2066.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 'Orthorhombic' changed to
'orthorhombic' 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               2216180
_cod_database_fobs_code          2216180