Synthesis and Structural, Spectroscopic, and Magnetic Characterization of (NH4)[Fe3(μ3-OH)(H2L)3(HL)3] (H3L = Orotic Acid) Presenting Two Novel Metal-Binding Modes of the Orotate Ligand: The Case of a Spin-Frustrated System
Catherine P. Raptopoulou; Vaslis Tangoulis; Vassilis Psycharis; Inorganic Chemistry 39 (2000) 4452–4459; doi:10.1021/ic9914084

data_4321423
_publ_section_title
;
 Synthesis and Structural, Spectroscopic, and Magnetic Characterization of
 (NH4)[Fe3(\m3-OH)(H2L)3(HL)3] (H3L = Orotic Acid) Presenting Two Novel
 Metal-Binding Modes of the Orotate Ligand: The Case of a Spin-Frustrated
 System
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4452
_journal_page_last               4459
_journal_paper_doi               10.1021/ic9914084
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         (NH4)[Fe3(OH)(C5H3N2O4)3(C5H2N2O4)3].7.75H2O
_chemical_formula_sum            'C30 H35.5 Fe3 N13 O32.75'
_chemical_formula_weight         1269.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           hexagonal
_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                   14.813(7)
_cell_length_b                   14.813(7)
_cell_length_c                   15.084(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      11.6
_cell_measurement_theta_min      5.5
_cell_volume                     2866(2)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic package, C.E.Strouse 1994)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic package, C.E.Strouse 1994)'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic package, C.E.Strouse 1994)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Crystal Logic Dual Goniometer diffractometer'
_diffrn_measurement_method       'theta-2theta scans'
_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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6610
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        -1.3
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_meas      1.45
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             1293
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1067P)^2^+4.3732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1755
_refine_ls_wR_factor_ref         0.1908
_reflns_number_gt                2700
_reflns_number_total             3383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9914084.cif
_cod_data_source_block           she98
_cod_original_cell_volume        2867(2)
_cod_database_code               4321423