#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:51:47 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179543 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/12/4501215.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_4501215
loop_
_publ_author_name
'Gao, Qiang'
'Wang, Xiqu'
'Conato, Marlon T.'
'Makarenko, Tatyana'
'Jacobson, Allan J.'
_publ_section_title
;
 Microporous, Homochiral Structures Containing Iron Oxo-Clusters Supported
 by Antimony(III) Tartrate Scaffolds
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4632
_journal_paper_doi               10.1021/cg200899w
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C54 H101 Fe14 K3 N2 O116 Sb12'
_chemical_formula_weight         4994.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           182
_symmetry_space_group_name_Hall  'P 6c 2c'
_symmetry_space_group_name_H-M   'P 63 2 2'
_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                   19.0892(9)
_cell_length_b                   19.0892(9)
_cell_length_c                   24.5573(12)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.79
_cell_volume                     7749.7(6)
_computing_cell_refinement       Bruker-ApexII
_computing_data_collection       Bruker-ApexII
_computing_data_reduction        Bruker-ApexII
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Bruker-ApexII
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  Bruker-ApexII
_diffrn_measurement_method       'narrow frame'
_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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            48072
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    3.508
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             4798
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.930
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.603
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_coef       0.00123(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    constrain
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         6335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.215
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0789P)²+4.4050P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                5547
_reflns_number_total             6335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200899w_si_002.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P6322
_cod_database_code               4501215
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
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
Sb1 Sb 0.64525(3) 0.42961(3) 0.56707(2) 0.03146(13) Uani 1 1 d .
Sb2 Sb 0.55242(3) 0.32232(3) 0.32028(2) 0.03853(15) Uani 1 1 d .
Fe1 Fe 0.54093(6) 0.40779(6) 0.44217(5) 0.0406(3) Uani 1 1 d .
Fe2 Fe 0.48096(5) 0.21689(5) 0.44407(4) 0.0308(2) Uani 1 1 d .
Fe3 Fe 0.6667 0.3333 0.44348(7) 0.0270(3) Uani 1 3 d S
K1 K 0.36918(13) 0.0000 0.5000 0.0527(7) Uani 1 2 d S
O1 O 0.6667 0.3333 0.5754(3) 0.0291(16) Uani 1 3 d S
O2 O 0.6667 0.3333 0.3126(4) 0.042(2) Uani 1 3 d S
O3 O 0.6525(3) 0.4221(3) 0.48630(19) 0.0312(10) Uani 1 1 d .
O4 O 0.5637(3) 0.3153(3) 0.4000(2) 0.0351(11) Uani 1 1 d .
O5 O 0.5551(3) 0.4751(3) 0.5403(3) 0.0546(16) Uani 1 1 d .
O6 O 0.4277(3) 0.4423(3) 0.5588(2) 0.0420(12) Uani 1 1 d .
O7 O 0.5335(3) 0.3337(3) 0.5742(2) 0.0371(11) Uani 1 1 d .
O8 O 0.4067(3) 0.1566(3) 0.5070(2) 0.0430(13) Uani 1 1 d .
O9 O 0.3355(4) 0.1660(4) 0.5757(3) 0.072(2) Uani 1 1 d .
O10 O 0.4600(3) 0.3001(3) 0.4736(2) 0.0363(11) Uani 1 1 d .
O11 O 0.4764(4) 0.3808(4) 0.3430(3) 0.0564(16) Uani 1 1 d .
O12 O 0.4703(4) 0.4909(5) 0.3246(3) 0.077(2) Uani 1 1 d .
O13 O 0.6273(3) 0.4430(3) 0.3141(3) 0.0476(13) Uani 1 1 d .
O14 O 0.7812(3) 0.5980(3) 0.3820(2) 0.0474(14) Uani 1 1 d .
O15 O 0.7533(5) 0.6584(5) 0.3155(3) 0.087(3) Uani 1 1 d .
O16 O 0.6353(3) 0.5155(3) 0.4161(2) 0.0367(11) Uani 1 1 d .
O17W O 0.2556(9) 0.0002(7) 0.5780(7) 0.081(5) Uani 0.50 1 d P
O18W O 0.3056(15) 0.2627(13) 0.3857(13) 0.091(10) Uani 0.30 1 d P
C1 C 0.6008(5) 0.4994(5) 0.3192(4) 0.049(2) Uani 1 1 d .
H1 H 0.6132 0.5308 0.2855 0.059 Uiso 1 1 calc R
C2 C 0.5061(5) 0.4546(6) 0.3292(4) 0.050(2) Uani 1 1 d .
C3 C 0.7314(5) 0.6099(5) 0.3526(4) 0.051(2) Uani 1 1 d .
C4 C 0.3811(4) 0.1959(5) 0.5368(3) 0.0446(18) Uani 1 1 d .
C5 C 0.6426(5) 0.5570(4) 0.3666(3) 0.0412(17) Uani 1 1 d .
H5 H 0.6185 0.5915 0.3714 0.049 Uiso 1 1 calc R
C6 C 0.4128(4) 0.2840(4) 0.5204(3) 0.0394(17) Uani 1 1 d .
H6 H 0.3672 0.2925 0.5128 0.047 Uiso 1 1 calc R
C7 C 0.4632(4) 0.3389(4) 0.5672(3) 0.0361(14) Uani 1 1 d .
H7 H 0.4311 0.3205 0.6007 0.043 Uiso 1 1 calc R
C8 C 0.4827(4) 0.4263(4) 0.5550(3) 0.0385(16) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
K K 0.2009 0.2494 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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'
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
O3 Sb1 O7 95.8(2) . .
O3 Sb1 O1 89.0(3) . .
O7 Sb1 O1 76.94(14) . .
O3 Sb1 O5 80.8(2) . .
O7 Sb1 O5 74.01(19) . .
O1 Sb1 O5 147.95(16) . .
O4 Sb2 O13 96.4(2) . .
O4 Sb2 O2 87.3(3) . .
O13 Sb2 O2 76.73(16) . .
O4 Sb2 O11 84.8(2) . .
O13 Sb2 O11 73.9(2) . .
O2 Sb2 O11 148.49(18) . .
O10 Fe1 O16 171.9(2) . .
O10 Fe1 O6 83.62(19) . 9_556
O16 Fe1 O6 103.52(19) . 9_556
O10 Fe1 O4 74.19(18) . .
O16 Fe1 O4 102.95(19) . .
O6 Fe1 O4 132.34(19) 9_556 .
O10 Fe1 O3 97.74(19) . .
O16 Fe1 O3 74.20(18) . .
O6 Fe1 O3 148.5(2) 9_556 .
O4 Fe1 O3 77.27(17) . .
O10 Fe1 K1 131.21(15) . 5_665
O16 Fe1 K1 48.94(15) . 5_665
O6 Fe1 K1 75.89(14) 9_556 5_665
O4 Fe1 K1 148.12(12) . 5_665
O3 Fe1 K1 79.90(12) . 5_665
O10 Fe2 O16 171.2(2) . 3_655
O10 Fe2 O14 96.6(2) . 3_655
O16 Fe2 O14 79.1(2) 3_655 3_655
O10 Fe2 O3 104.6(2) . 3_655
O16 Fe2 O3 80.92(19) 3_655 3_655
O14 Fe2 O3 157.2(2) 3_655 3_655
O10 Fe2 O8 79.0(2) . .
O16 Fe2 O8 94.2(2) 3_655 .
O14 Fe2 O8 101.4(3) 3_655 .
O3 Fe2 O8 91.0(2) 3_655 .
O10 Fe2 O4 80.2(2) . .
O16 Fe2 O4 107.3(2) 3_655 .
O14 Fe2 O4 90.2(2) 3_655 .
O3 Fe2 O4 85.29(19) 3_655 .
O8 Fe2 O4 157.2(2) . .
O4 Fe3 O4 96.61(19) 3_655 5_665
O4 Fe3 O4 96.61(19) 3_655 .
O4 Fe3 O4 96.61(19) 5_665 .
O4 Fe3 O3 81.51(17) 3_655 5_665
O4 Fe3 O3 84.31(18) 5_665 5_665
O4 Fe3 O3 178.00(18) . 5_665
O4 Fe3 O3 84.31(18) 3_655 3_655
O4 Fe3 O3 178.00(18) 5_665 3_655
O4 Fe3 O3 81.51(17) . 3_655
O3 Fe3 O3 97.60(16) 5_665 3_655
O4 Fe3 O3 178.00(18) 3_655 .
O4 Fe3 O3 81.51(17) 5_665 .
O4 Fe3 O3 84.31(18) . .
O3 Fe3 O3 97.60(16) 5_665 .
O3 Fe3 O3 97.60(16) 3_655 .
O8 K1 O8 146.6(2) 7_556 .
O8 K1 O5 135.31(17) 7_556 3_655
O8 K1 O5 75.47(16) . 3_655
O8 K1 O5 75.47(16) 7_556 8_656
O8 K1 O5 135.31(17) . 8_656
O5 K1 O5 73.5(3) 3_655 8_656
O8 K1 O17W 75.0(3) 7_556 7_556
O8 K1 O17W 80.1(3) . 7_556
O5 K1 O17W 147.0(3) 3_655 7_556
O5 K1 O17W 111.3(4) 8_656 7_556
O8 K1 O17W 80.1(3) 7_556 .
O8 K1 O17W 75.0(3) . .
O5 K1 O17W 111.3(4) 3_655 .
O5 K1 O17W 147.0(3) 8_656 .
O17W K1 O17W 82.9(7) 7_556 .
O8 K1 O16 132.69(15) 7_556 3_655
O8 K1 O16 61.40(14) . 3_655
O5 K1 O16 69.70(17) 3_655 3_655
O5 K1 O16 77.95(16) 8_656 3_655
O17W K1 O16 79.2(3) 7_556 3_655
O17W K1 O16 135.0(3) . 3_655
O8 K1 O16 61.40(14) 7_556 8_656
O8 K1 O16 132.69(15) . 8_656
O5 K1 O16 77.95(16) 3_655 8_656
O5 K1 O16 69.70(17) 8_656 8_656
O17W K1 O16 135.0(3) 7_556 8_656
O17W K1 O16 79.2(3) . 8_656
O16 K1 O16 139.40(19) 3_655 8_656
O8 K1 Fe2 30.12(11) 7_556 7_556
O8 K1 Fe2 150.98(12) . 7_556
O5 K1 Fe2 107.82(13) 3_655 7_556
O5 K1 Fe2 70.57(12) 8_656 7_556
O17W K1 Fe2 104.4(2) 7_556 7_556
O17W K1 Fe2 77.1(2) . 7_556
O16 K1 Fe2 147.45(10) 3_655 7_556
O16 K1 Fe2 31.30(9) 8_656 7_556
O8 K1 Fe1 136.29(13) 7_556 3_655
O8 K1 Fe1 73.09(11) . 3_655
O5 K1 Fe1 42.30(14) 3_655 3_655
O5 K1 Fe1 62.30(12) 8_656 3_655
O17W K1 Fe1 109.1(3) 7_556 3_655
O17W K1 Fe1 143.1(3) . 3_655
O16 K1 Fe1 30.38(9) 3_655 3_655
O16 K1 Fe1 109.93(11) 8_656 3_655
Fe2 K1 Fe1 129.25(6) 7_556 3_655
O8 K1 Fe1 73.09(11) 7_556 8_656
O8 K1 Fe1 136.29(13) . 8_656
O5 K1 Fe1 62.30(12) 3_655 8_656
O5 K1 Fe1 42.30(14) 8_656 8_656
O17W K1 Fe1 143.1(3) 7_556 8_656
O17W K1 Fe1 109.1(3) . 8_656
O16 K1 Fe1 109.93(11) 3_655 8_656
O16 K1 Fe1 30.38(9) 8_656 8_656
Fe2 K1 Fe1 48.88(2) 7_556 8_656
Fe1 K1 Fe1 82.50(6) 3_655 8_656
Sb1 O1 Sb1 119.05(8) 5_665 3_655
Sb1 O1 Sb1 119.05(8) 5_665 .
Sb1 O1 Sb1 119.05(8) 3_655 .
Sb2 O2 Sb2 119.19(8) 3_655 5_665
Sb2 O2 Sb2 119.19(8) 3_655 .
Sb2 O2 Sb2 119.19(8) 5_665 .
Sb1 O3 Fe2 119.6(2) . 5_665
Sb1 O3 Fe3 126.1(2) . .
Fe2 O3 Fe3 96.88(19) 5_665 .
Sb1 O3 Fe1 112.7(2) . .
Fe2 O3 Fe1 97.30(18) 5_665 .
Fe3 O3 Fe1 98.81(18) . .
Sb2 O4 Fe2 121.5(2) . .
Sb2 O4 Fe3 127.8(3) . .
Fe2 O4 Fe3 96.3(2) . .
Sb2 O4 Fe1 109.2(2) . .
Fe2 O4 Fe1 96.4(2) . .
Fe3 O4 Fe1 99.6(2) . .
C8 O5 Sb1 111.9(5) . .
C8 O5 K1 133.1(5) . 5_665
Sb1 O5 K1 114.1(2) . 5_665
C8 O6 Fe1 141.1(5) . 9_556
C7 O7 Sb1 122.8(4) . .
C4 O8 Fe2 117.4(5) . .
C4 O8 K1 134.5(5) . .
Fe2 O8 K1 107.6(2) . .
C6 O10 Fe2 119.8(4) . .
C6 O10 Fe1 128.5(4) . .
Fe2 O10 Fe1 108.8(2) . .
C2 O11 Sb2 115.7(5) . .
C1 O13 Sb2 123.1(5) . .
C3 O14 Fe2 118.3(5) . 5_665
C5 O16 Fe2 116.7(4) . 5_665
C5 O16 Fe1 128.4(4) . .
Fe2 O16 Fe1 105.9(2) 5_665 .
C5 O16 K1 101.9(4) . 5_665
Fe2 O16 K1 96.67(19) 5_665 5_665
Fe1 O16 K1 100.68(19) . 5_665
O13 C1 C5 111.2(6) . .
O13 C1 C2 110.6(6) . .
C5 C1 C2 108.4(7) . .
O12 C2 O11 126.8(9) . .
O12 C2 C1 120.0(8) . .
O11 C2 C1 113.2(7) . .
O15 C3 O14 123.1(8) . .
O15 C3 C5 121.5(8) . .
O14 C3 C5 115.4(7) . .
O9 C4 O8 123.6(7) . .
O9 C4 C6 121.2(7) . .
O8 C4 C6 115.3(6) . .
O16 C5 C3 109.3(6) . .
O16 C5 C1 112.4(6) . .
C3 C5 C1 108.4(7) . .
O10 C6 C7 110.7(5) . .
O10 C6 C4 108.5(6) . .
C7 C6 C4 108.8(7) . .
O7 C7 C6 109.8(6) . .
O7 C7 C8 112.2(6) . .
C6 C7 C8 108.8(6) . .
O6 C8 O5 125.9(7) . .
O6 C8 C7 118.4(7) . .
O5 C8 C7 115.6(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 O3 1.999(5) .
Sb1 O7 2.007(5) .
Sb1 O1 2.0827(9) .
Sb1 O5 2.376(5) .
Sb2 O4 1.981(5) .
Sb2 O13 2.020(5) .
Sb2 O2 2.0923(10) .
Sb2 O11 2.298(6) .
Fe1 O10 2.008(5) .
Fe1 O16 2.045(5) .
Fe1 O6 2.099(5) 9_556
Fe1 O4 2.269(5) .
Fe1 O3 2.281(5) .
Fe1 K1 3.973(2) 5_665
Fe2 O10 1.961(5) .
Fe2 O16 2.009(5) 3_655
Fe2 O14 2.010(5) 3_655
Fe2 O3 2.022(4) 3_655
Fe2 O8 2.022(5) .
Fe2 O4 2.056(5) .
Fe3 O4 2.109(5) 3_655
Fe3 O4 2.109(5) 5_665
Fe3 O4 2.109(5) .
Fe3 O3 2.124(5) 5_665
Fe3 O3 2.124(5) 3_655
Fe3 O3 2.124(5) .
K1 O8 2.709(5) 7_556
K1 O8 2.709(5) .
K1 O5 2.757(6) 3_655
K1 O5 2.757(6) 8_656
K1 O17W 2.894(14) 7_556
K1 O17W 2.894(14) .
K1 O16 3.048(5) 3_655
K1 O16 3.048(5) 8_656
K1 Fe2 3.8402(9) 7_556
K1 Fe1 3.973(2) 3_655
K1 Fe1 3.973(2) 8_656
O1 Sb1 2.0827(9) 5_665
O1 Sb1 2.0827(9) 3_655
O2 Sb2 2.0923(10) 3_655
O2 Sb2 2.0923(10) 5_665
O3 Fe2 2.022(4) 5_665
O5 C8 1.274(9) .
O5 K1 2.757(6) 5_665
O6 C8 1.235(8) .
O6 Fe1 2.099(5) 9_556
O7 C7 1.406(8) .
O8 C4 1.306(9) .
O9 C4 1.223(9) .
O10 C6 1.396(9) .
O11 C2 1.273(10) .
O12 C2 1.197(10) .
O13 C1 1.407(10) .
O14 C3 1.302(10) .
O14 Fe2 2.010(5) 5_665
O15 C3 1.213(10) .
O16 C5 1.420(9) .
O16 Fe2 2.009(5) 5_665
O16 K1 3.048(5) 5_665
C1 C5 1.524(12) .
C1 C2 1.585(11) .
C3 C5 1.516(11) .
C4 C6 1.530(10) .
C6 C7 1.529(10) .
C7 C8 1.546(10) .
