#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:38:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179590 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/55/4505544.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4505544
loop_
_publ_author_name
'Hou, Yu'
'Rodriguez, Mark A.'
'Nyman, May'
_publ_section_title
;
 Cation-Bonding and Protonation of the Fe4-Square Cluster
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1422
_journal_paper_doi               10.1021/cg2015397
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C52 H66 Fe8 Mg2 N8 Na2 O72'
_chemical_formula_weight         2496.53
_chemical_name_common            'sodium magnesium iron(4) di-HPDTA diacetate'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 98.5510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   11.0430(9)
_cell_length_b                   20.5133(16)
_cell_length_c                   11.2959(9)
_cell_measurement_reflns_used    237
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     2530.4(3)
_computing_cell_refinement       '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      188(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21601
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.250
_exptl_absorpt_correction_T_max  0.8831
_exptl_absorpt_correction_T_min  0.7891
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker 2000'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.413
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5950
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0737
_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/[σ²(Fo²)+(0.1601P)²+8.0027P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2401
_refine_ls_wR_factor_ref         0.2494
_reflns_number_gt                5091
_reflns_number_total             5950
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2015397_si_004.cif
_cod_data_source_block           11oc051_mgfe4
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4505544
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.38119(6) 0.16472(3) 0.71544(6) 0.0258(2) Uani 1 1 d .
Fe2 Fe 0.71210(6) 0.16699(3) 0.82763(5) 0.0232(2) Uani 1 1 d .
O1 O 0.5449(3) 0.12489(15) 0.7852(3) 0.0269(6) Uani 1 1 d .
O2 O 0.7426(3) 0.14916(17) 0.6578(3) 0.0333(7) Uani 1 1 d .
O3 O 0.4230(4) 0.14896(18) 0.5507(3) 0.0378(8) Uani 1 1 d .
N1 N 0.3329(4) 0.06139(19) 0.6892(4) 0.0321(8) Uani 1 1 d .
N2 N 0.7729(3) 0.06538(17) 0.8416(3) 0.0272(7) Uani 1 1 d .
O4 O 0.7233(4) 0.14709(17) 1.0062(3) 0.0377(8) Uani 1 1 d .
O5 O 0.2989(4) 0.14268(19) 0.8584(4) 0.0447(9) Uani 1 1 d .
Mg1 Mg 0.6650(4) 0.2500 0.3204(2) 0.0555(8) Uani 1 2 d S
Na1 Na 0.3412(4) 0.2500 0.3947(3) 0.0526(8) Uani 1 2 d S
O6 O 0.4327(5) 0.2500 0.7520(5) 0.0375(11) Uani 1 2 d SD
H6 H 0.514(2) 0.2500 0.780(7) 0.03(2) Uiso 1 2 d SD
O7 O 0.6502(5) 0.2500 0.8257(5) 0.0392(11) Uani 1 2 d S
O8 O 0.8403(5) 0.0896(2) 0.5400(4) 0.0531(11) Uani 1 1 d .
C1 C 0.8385(5) 0.0517(2) 0.7393(5) 0.0367(10) Uani 1 1 d .
H1A H 0.8190 0.0078 0.7103 0.044 Uiso 1 1 calc R
H1B H 0.9261 0.0538 0.7660 0.044 Uiso 1 1 calc R
C2 C 0.5547(4) 0.0583(2) 0.7567(4) 0.0306(9) Uani 1 1 d .
H2 H 0.5721 0.0548 0.6743 0.037 Uiso 1 1 calc .
C3 C 0.6588(4) 0.0267(2) 0.8396(4) 0.0319(9) Uani 1 1 d .
H3A H 0.6378 0.0240 0.9198 0.038 Uiso 1 1 calc R
H3B H 0.6719 -0.0173 0.8124 0.038 Uiso 1 1 calc R
C4 C 0.2166(5) 0.0531(3) 0.7371(6) 0.0450(13) Uani 1 1 d .
H4A H 0.2066 0.0079 0.7589 0.054 Uiso 1 1 calc R
H4B H 0.1483 0.0651 0.6767 0.054 Uiso 1 1 calc R
C5 C 0.8038(5) 0.1004(2) 0.6369(4) 0.0361(10) Uani 1 1 d .
O9 O 0.8895(3) 0.19548(16) 0.8639(4) 0.0379(8) Uani 1 1 d .
O1W O 0.6484(7) 0.2500 0.4991(5) 0.0582(17) Uani 1 2 d S
O10 O 0.2122(3) 0.19571(19) 0.6355(4) 0.0476(10) Uani 1 1 d .
O11 O 0.4334(5) 0.0795(2) 0.4035(4) 0.0614(12) Uani 1 1 d .
O12 O 0.8425(6) 0.0970(2) 1.1572(4) 0.0653(14) Uani 1 1 d .
O2W O 0.7945(6) 0.1755(2) 0.3455(4) 0.0667(14) Uani 1 1 d .
C6 C 0.8519(5) 0.0597(2) 0.9590(4) 0.0362(10) Uani 1 1 d .
H6A H 0.9352 0.0719 0.9512 0.043 Uiso 1 1 calc R
H6B H 0.8526 0.0149 0.9866 0.043 Uiso 1 1 calc R
O3W O 0.6819(8) 0.2500 0.1447(5) 0.067(2) Uani 1 2 d S
C7 C 0.4026(5) 0.0939(3) 0.4997(5) 0.0414(11) Uani 1 1 d .
O4W O 0.5244(6) 0.1797(3) 0.2855(4) 0.0739(16) Uani 1 1 d .
C8 C 0.1596(7) 0.2500 0.6216(6) 0.0373(15) Uani 1 2 d S
C9 C 0.3273(5) 0.0457(3) 0.5604(5) 0.0438(12) Uani 1 1 d .
H9A H 0.2428 0.0470 0.5218 0.053 Uiso 1 1 calc R
H9B H 0.3582 0.0020 0.5520 0.053 Uiso 1 1 calc R
C10 C 0.9409(6) 0.2500 0.8826(6) 0.0320(13) Uani 1 2 d S
O13 O 0.1470(5) 0.0847(2) 0.9177(6) 0.0739(17) Uani 1 1 d .
C11 C 0.8037(6) 0.1039(2) 1.0490(4) 0.0412(12) Uani 1 1 d .
C12 C 0.2186(5) 0.0962(3) 0.8459(6) 0.0481(14) Uani 1 1 d .
C13 C 0.4334(4) 0.0247(2) 0.7641(5) 0.0356(10) Uani 1 1 d .
H13A H 0.4358 -0.0198 0.7355 0.043 Uiso 1 1 calc R
H13B H 0.4187 0.0236 0.8466 0.043 Uiso 1 1 calc R
C14 C 1.0752(8) 0.2500 0.9292(11) 0.057(2) Uani 1 2 d S
H14A H 1.1043 0.2059 0.9373 0.086 Uiso 0.50 1 calc PR
H14B H 1.0891 0.2712 1.0058 0.086 Uiso 0.50 1 calc PR
H14C H 1.1183 0.2729 0.8742 0.086 Uiso 0.50 1 calc PR
C15 C 0.0236(8) 0.2500 0.5825(10) 0.059(2) Uani 1 2 d S
H15A H 0.0052 0.2705 0.5055 0.089 Uiso 0.50 1 calc PR
H15B H -0.0156 0.2736 0.6397 0.089 Uiso 0.50 1 calc PR
H15C H -0.0059 0.2059 0.5774 0.089 Uiso 0.50 1 calc PR
O5W O 0.4794(9) 0.1179(5) 0.0664(7) 0.132(3) Uani 1 1 d .
O6W O 0.0330(9) 0.0413(6) 0.4520(11) 0.158(4) Uani 1 1 d .
O7W O 0.1365(19) 0.1557(10) 0.3298(17) 0.267(9) Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O6 Fe1 O3 104.6(2) . .
O6 Fe1 O5 101.0(2) . .
O3 Fe1 O5 153.88(17) . .
O6 Fe1 O1 93.81(17) . .
O3 Fe1 O1 88.89(14) . .
O5 Fe1 O1 94.60(15) . .
O6 Fe1 O10 91.98(18) . .
O3 Fe1 O10 87.79(17) . .
O5 Fe1 O10 86.16(18) . .
O1 Fe1 O10 173.89(14) . .
O6 Fe1 N1 174.12(19) . .
O3 Fe1 N1 78.70(15) . .
O5 Fe1 N1 76.27(16) . .
O1 Fe1 N1 81.28(14) . .
O10 Fe1 N1 93.04(16) . .
O7 Fe2 O9 94.70(18) . .
O7 Fe2 O1 93.90(17) . .
O9 Fe2 O1 171.16(13) . .
O7 Fe2 O2 105.7(2) . .
O9 Fe2 O2 87.24(15) . .
O1 Fe2 O2 88.45(13) . .
O7 Fe2 O4 99.5(2) . .
O9 Fe2 O4 86.75(16) . .
O1 Fe2 O4 93.88(14) . .
O2 Fe2 O4 154.53(15) . .
O7 Fe2 N2 174.4(2) . .
O9 Fe2 N2 89.02(14) . .
O1 Fe2 N2 82.57(13) . .
O2 Fe2 N2 78.72(14) . .
O4 Fe2 N2 76.45(14) . .
C2 O1 Fe2 111.6(3) . .
C2 O1 Fe1 113.3(3) . .
Fe2 O1 Fe1 130.23(16) . .
C5 O2 Fe2 119.5(3) . .
C7 O3 Fe1 120.8(3) . .
C7 O3 Na1 110.9(3) . .
Fe1 O3 Na1 111.65(17) . .
C4 N1 C9 115.0(4) . .
C4 N1 C13 110.4(4) . .
C9 N1 C13 111.4(4) . .
C4 N1 Fe1 105.6(3) . .
C9 N1 Fe1 108.4(3) . .
C13 N1 Fe1 105.3(3) . .
C1 N2 C6 113.1(4) . .
C1 N2 C3 113.5(4) . .
C6 N2 C3 110.9(4) . .
C1 N2 Fe2 107.8(3) . .
C6 N2 Fe2 105.9(3) . .
C3 N2 Fe2 104.9(3) . .
C11 O4 Fe2 116.2(3) . .
C12 O5 Fe1 117.3(4) . .
O3W Mg1 O1W 179.8(4) . .
O3W Mg1 O2W 88.4(2) . .
O1W Mg1 O2W 91.5(2) . .
O3W Mg1 O2W 88.4(2) . 4_565
O1W Mg1 O2W 91.5(2) . 4_565
O2W Mg1 O2W 94.3(4) . 4_565
O3W Mg1 O4W 89.4(3) . .
O1W Mg1 O4W 90.8(2) . .
O2W Mg1 O4W 89.8(2) . .
O2W Mg1 O4W 175.3(3) 4_565 .
O3W Mg1 O4W 89.4(2) . 4_565
O1W Mg1 O4W 90.8(2) . 4_565
O2W Mg1 O4W 175.3(3) . 4_565
O2W Mg1 O4W 89.8(2) 4_565 4_565
O4W Mg1 O4W 86.1(4) . 4_565
O3W Mg1 Na1 116.4(3) . .
O1W Mg1 Na1 63.8(2) . .
O2W Mg1 Na1 128.37(18) . .
O2W Mg1 Na1 128.37(18) 4_565 .
O4W Mg1 Na1 49.49(19) . .
O4W Mg1 Na1 49.5(2) 4_565 .
O3 Na1 O3 96.31(19) . 4_565
O3 Na1 O4W 117.23(19) . 4_565
O3 Na1 O4W 73.64(14) 4_565 4_565
O3 Na1 O4W 73.64(14) . .
O3 Na1 O4W 117.23(19) 4_565 .
O4W Na1 O4W 59.5(2) 4_565 .
O3 Na1 O7W 80.5(4) . .
O3 Na1 O7W 143.3(4) 4_565 .
O4W Na1 O7W 140.1(4) 4_565 .
O4W Na1 O7W 97.1(4) . .
O3 Na1 O7W 143.3(4) . 4_565
O3 Na1 O7W 80.5(4) 4_565 4_565
O4W Na1 O7W 97.1(4) 4_565 4_565
O4W Na1 O7W 140.1(4) . 4_565
O7W Na1 O7W 80.9(8) . 4_565
O3 Na1 Mg1 84.96(12) . .
O3 Na1 Mg1 84.96(12) 4_565 .
O4W Na1 Mg1 33.56(12) 4_565 .
O4W Na1 Mg1 33.56(12) . .
O7W Na1 Mg1 130.6(4) . .
O7W Na1 Mg1 130.6(4) 4_565 .
Fe1 O6 Fe1 139.1(3) . 4_565
Fe2 O7 Fe2 136.4(3) . 4_565
N2 C1 C5 111.6(4) . .
O1 C2 C3 110.5(4) . .
O1 C2 C13 109.1(4) . .
C3 C2 C13 111.5(4) . .
N2 C3 C2 110.1(4) . .
N1 C4 C12 108.9(4) . .
O8 C5 O2 124.3(5) . .
O8 C5 C1 118.2(5) . .
O2 C5 C1 117.5(4) . .
C10 O9 Fe2 133.5(3) . .
C8 O10 Fe1 134.8(4) . .
N2 C6 C11 109.5(4) . .
O11 C7 O3 124.3(5) . .
O11 C7 C9 119.1(5) . .
O3 C7 C9 116.4(5) . .
Mg1 O4W Na1 97.0(2) . .
O10 C8 O10 125.1(7) . 4_565
O10 C8 C15 117.4(3) . .
O10 C8 C15 117.4(3) 4_565 .
N1 C9 C7 110.9(4) . .
O9 C10 O9 125.5(6) . 4_565
O9 C10 C14 117.2(3) . .
O9 C10 C14 117.2(3) 4_565 .
O12 C11 O4 124.2(5) . .
O12 C11 C6 119.2(5) . .
O4 C11 C6 116.7(4) . .
O13 C12 O5 124.1(6) . .
O13 C12 C4 119.4(6) . .
O5 C12 C4 116.5(4) . .
N1 C13 C2 109.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O6 1.8669(18) .
Fe1 O3 2.009(4) .
Fe1 O5 2.019(4) .
Fe1 O1 2.033(3) .
Fe1 O10 2.050(4) .
Fe1 N1 2.195(4) .
Fe2 O7 1.834(2) .
Fe2 O9 2.027(4) .
Fe2 O1 2.030(3) .
Fe2 O2 2.030(3) .
Fe2 O4 2.044(3) .
Fe2 N2 2.188(4) .
O1 C2 1.412(5) .
O2 C5 1.250(6) .
O3 C7 1.272(7) .
O3 Na1 2.782(4) .
N1 C4 1.476(6) .
N1 C9 1.482(7) .
N1 C13 1.494(6) .
N2 C1 1.479(6) .
N2 C6 1.480(6) .
N2 C3 1.487(6) .
O4 C11 1.297(7) .
O5 C12 1.296(7) .
Mg1 O3W 2.021(6) .
Mg1 O1W 2.053(6) .
Mg1 O2W 2.084(6) .
Mg1 O2W 2.084(6) 4_565
Mg1 O4W 2.112(6) .
Mg1 O4W 2.112(6) 4_565
Mg1 Na1 3.792(5) .
Na1 O3 2.782(4) 4_565
Na1 O4W 2.904(7) 4_565
Na1 O4W 2.904(7) .
Na1 O7W 2.98(2) .
Na1 O7W 2.98(2) 4_565
O6 Fe1 1.8669(18) 4_565
O7 Fe2 1.834(2) 4_565
O8 C5 1.241(6) .
C1 C5 1.534(7) .
C2 C3 1.516(6) .
C2 C13 1.519(6) .
C4 C12 1.510(9) .
O9 C10 1.258(5) .
O10 C8 1.255(5) .
O11 C7 1.222(7) .
O12 C11 1.242(6) .
C6 C11 1.516(7) .
C7 C9 1.520(8) .
C8 O10 1.255(5) 4_565
C8 C15 1.502(11) .
C10 O9 1.258(4) 4_565
C10 C14 1.498(10) .
O13 C12 1.237(7) .
