Cation-Bonding and Protonation of the Fe4-Square Cluster
Hou, Yu; Rodriguez, Mark A.; Nyman, May; Crystal Growth & Design 12 (2012) 1422–; doi:10.1021/cg2015397

data_4505545
_publ_section_title
;
 Cation-Bonding and Protonation of the Fe4-Square Cluster
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1422
_journal_paper_doi               10.1021/cg2015397
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C26 H33 Fe4 La N4 O36'
_chemical_formula_weight         1339.87
_chemical_name_common            'lanthanum iron(4) dioxo di-HPDTA diacetate'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 99.440(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.074(3)
_cell_length_b                   11.1217(14)
_cell_length_c                   21.507(3)
_cell_measurement_reflns_used    1232
_cell_measurement_temperature    150(2)
_cell_volume                     4972.5(12)
_computing_cell_refinement       'SMART 5.054 (Bruker, 1998)'
_computing_data_collection       'SMART 5.054 (Bruker, 1998)'
_computing_data_reduction        'SAINT 6.02 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL 5.1  (Bruker, 1998)'
_computing_publication_material  'SHELXTL 5.1  (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL 5.1  (Bruker, 1998'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
'0.5 degree frames measured for 1 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  'Si 1 1 1 and 3 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41228
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_sigmaI/netI    0.0943
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            51760
_diffrn_reflns_theta_full        30.90
_diffrn_reflns_theta_max         30.90
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    2.086
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_correction_T_min  0.9401
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker 2000'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flake
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.607
_refine_diff_density_min         -2.049
_refine_diff_density_rms         0.270
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         14379
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0821
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1482P)^2^+26.4901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2154
_refine_ls_wR_factor_ref         0.2343
_reflns_number_gt                10445
_reflns_number_total             14379
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2015397_si_005.cif
_cod_data_source_block           0888_cc
_cod_original_cell_volume        4972.5(11)
_cod_original_sg_symbol_Hall     'C 2yc'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4505545