Synthesis, Spectroscopic and Structural Characterization of the First Mononuclear, Water Soluble Iron-Citrate Complex, (NH4)5Fe(C6H4O7)2.2H2O
M. Matzapetakis; C. P. Raptopoulou; A. Tsohos; V. Papaefthymiou; N. Moon; A. Salifoglou; Journal of the American Chemical Society 120 (1998) 13266–13267; doi:10.1021/ja9807035

data_4116912
_publ_section_title
;
 Synthesis, Spectroscopic and Structural Characterization of the First
 Mononuclear, Water Soluble Iron-Citrate Complex, (NH4)5Fe(C6H4O7)2.2H2O
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13266
_journal_page_last               13267
_journal_paper_doi               10.1021/ja9807035
_journal_volume                  120
_journal_year                    1998
_chemical_formula_analytical     '[(NH4)5Fe(C6H4O7)2]2H2O'
_chemical_formula_structural     '[(NH4)5Fe(citrate)2]2H2O'
_chemical_formula_sum            'C12 H32 Fe N5 O16'
_chemical_formula_weight         558.27
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.93(2)
_cell_angle_beta                 105.69(2)
_cell_angle_gamma                118.58(2)
_cell_formula_units_Z            1
_cell_length_a                   9.669(7)
_cell_length_b                   9.714(7)
_cell_length_c                   7.265(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.6
_cell_measurement_theta_min      6.5
_cell_volume                     568.3(7)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic package)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic package)'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic package)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device
'Crystal Logic Dual Goniometer diffractometer'
_diffrn_measurement_method       'theta-2theta scan'
_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  0.0096
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2192
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_meas      1.61
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             293
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.243(10)
_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_all   1.079
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_obs          0.0304
_refine_ls_shift/esd_max         0.046
_refine_ls_shift/esd_mean        0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+0.4719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0820
_refine_ls_wR_factor_obs         0.0816
_reflns_number_observed          1981
_reflns_number_total             2017
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9807035.cif
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+0.4719P] 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^)+(0.0217P)^2^+0.4719P] 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        568.2(7)
_cod_database_code               4116912