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#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100722.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_1100722
loop_
_publ_author_name
'Andrea C. Sudik'
'Adrien P. Côté'
'Omar M. Yaghi'
_publ_contact_author_address
; 

department of chemistry 

university of michigan 

930 n. university ave. 

ann arbor, mi 48109-1055 

united states of america 

;
_publ_contact_author_email       oyaghi@umich.edu
_publ_contact_author_name        'professor omar m. yaghi'
_publ_section_title
;

Metal-Organic Frameworks Based on Trigonal Prismatic Building Blocks and

the New "acs" Topology

;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2998
_journal_page_last               3000
_journal_paper_doi               10.1021/ic050064g
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '(C33 H15 Fe3 N3 O16), (Cl4 Fe), O'
_chemical_formula_sum            'C33 H15 Cl4 Fe4 N3 O17'
_chemical_formula_weight         1090.61
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           190
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_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                   12.531(3)
_cell_length_b                   12.531(3)
_cell_length_c                   18.476(11)
_cell_measurement_reflns_used    715
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      1.88
_cell_volume                     2512.5(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1441
_diffrn_reflns_av_sigmaI/netI    0.1009
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11323
_diffrn_reflns_theta_full        25.15
_diffrn_reflns_theta_max         25.15
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.407
_exptl_absorpt_correction_T_max  0.9498
_exptl_absorpt_correction_T_min  0.9433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-58'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.042
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(10)
_refine_ls_extinction_coef       0.015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.260
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1543
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.260
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.1044
_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/[σ²(Fo²)+(0.1172P)²+5.2365P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2454
_refine_ls_wR_factor_ref         0.2550
_reflns_number_gt                1292
_reflns_number_total             1543
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050064gsi20050115_040515_2.cif
_cod_data_source_block           MOF-235
_cod_original_cell_volume        2512.6(17)
_cod_original_sg_symbol_Hall     P-6c-2c
_cod_database_code               1100722
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.7270(2) 1.2195(2) 0.7500 0.0233(6) Uani 1 2 d S . .
O1 O 0.6667 1.3333 0.7500 0.018(4) Uani 1 6 d S . .
O2 O 0.8499(8) 1.3019(7) 0.6692(4) 0.034(2) Uani 1 1 d . . .
O3 O 0.7800(11) 1.0882(12) 0.7500 0.047(3) Uani 1 2 d S . .
O4 O 0.6106(8) 1.1159(8) 0.6719(5) 0.042(2) Uani 1 1 d . . .
C1 C 0.716(3) 0.982(3) 0.7500 0.21(3) Uani 1 2 d S . .
H1 H 0.6321 0.9569 0.7500 0.255 Uiso 1 2 calc SR . .
N1 N 0.738(2) 0.893(2) 0.7500 0.119(10) Uani 1 2 d SD . .
C3 C 0.5160(11) 1.1110(13) 0.6423(8) 0.046(3) Uani 1 1 d . . .
C4 C 0.5680(13) 1.0240(18) 0.5353(7) 0.064(5) Uani 1 1 d . . .
H4 H 0.6384 1.0371 0.5598 0.03(3) Uiso 1 1 calc R . .
C5 C 0.4835(12) 1.0521(13) 0.5685(7) 0.047(4) Uani 1 1 d . . .
C6 C 0.3754(11) 1.0259(11) 0.5325(6) 0.041(3) Uani 1 1 d . . .
H6 H 0.3204 1.0452 0.5545 0.050 Uiso 1 1 calc R . .
C7 C 0.805(6) 0.896(5) 0.692(3) 0.16(3) Uani 0.50 1 d P . .
C8 C 0.643(5) 0.767(3) 0.7500 0.30(4) Uani 1 2 d SD . .
O1W O 0.3333 0.6667 0.594(6) 0.22(4) Uani 0.50 3 d SP . .
Fe2 Fe 0.0000 1.0000 0.5000 0.099(3) Uani 1 6 d S . .
Cl1 Cl -0.1618(12) 1.0000 0.5000 0.051(4) Uani 0.333 2 d SP . .
Cl2 Cl -0.1453(17) 0.9805(19) 0.574(2) 0.31(2) Uani 0.50 1 d P . .
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'
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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
O1 Fe1 O4 93.0(2) . 4_556 ?
O1 Fe1 O4 93.0(2) . . ?
O4 Fe1 O4 92.3(6) 4_556 . ?
O1 Fe1 O2 95.9(2) . 4_556 ?
O4 Fe1 O2 85.5(4) 4_556 4_556 ?
O4 Fe1 O2 170.9(3) . 4_556 ?
O1 Fe1 O2 95.9(2) . . ?
O4 Fe1 O2 170.9(3) 4_556 . ?
O4 Fe1 O2 85.4(4) . . ?
O2 Fe1 O2 95.4(5) 4_556 . ?
O1 Fe1 O3 176.3(4) . . ?
O4 Fe1 O3 84.5(3) 4_556 . ?
O4 Fe1 O3 84.5(3) . . ?
O2 Fe1 O3 86.6(3) 4_556 . ?
O2 Fe1 O3 86.6(3) . . ?
Fe1 O1 Fe1 120.000(2) 3_575 . ?
Fe1 O1 Fe1 120.0 3_575 2_775 ?
Fe1 O1 Fe1 120.001(1) . 2_775 ?
C3 O2 Fe1 129.4(8) 2_775 . ?
C1 O3 Fe1 126.8(17) . . ?
C3 O4 Fe1 134.2(8) . . ?
O3 C1 N1 132(3) . . ?
O3 C1 H1 114.0 . . ?
N1 C1 H1 114.0 . . ?
C1 N1 C7 113(2) . . ?
C1 N1 C7 113(2) . 4_556 ?
C7 N1 C7 105(6) . 4_556 ?
C1 N1 C8 123(3) . . ?
C7 N1 C8 101(3) . . ?
C7 N1 C8 101(3) 4_556 . ?
O2 C3 O4 125.4(12) 3_575 . ?
O2 C3 C5 119.3(12) 3_575 . ?
O4 C3 C5 115.3(12) . . ?
C4 C4 C5 118.9(8) 8_676 . ?
C4 C4 H4 120.6 8_676 . ?
C5 C4 H4 120.6 . . ?
C6 C5 C4 119.8(12) . . ?
C6 C5 C3 122.7(12) . . ?
C4 C5 C3 117.5(12) . . ?
C6 C6 C5 121.2(8) 8_676 . ?
C6 C6 H6 119.4 8_676 . ?
C5 C6 H6 119.4 . . ?
Cl1 Fe2 Cl1 119.998(1) 3_575 1_455 ?
Cl1 Fe2 Cl1 120.001(6) 3_575 2_665 ?
Cl1 Fe2 Cl1 120.001(10) 1_455 2_665 ?
Cl2 Cl1 Cl2 153(2) 8_676 . ?
Cl2 Cl1 Fe2 76.6(11) 8_676 1_655 ?
Cl2 Cl1 Fe2 76.6(11) . 1_655 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.920(2) . ?
Fe1 O4 2.001(9) 4_556 ?
Fe1 O4 2.001(9) . ?
Fe1 O2 2.019(8) 4_556 ?
Fe1 O2 2.019(8) . ?
Fe1 O3 2.059(13) . ?
O1 Fe1 1.920(2) 3_575 ?
O1 Fe1 1.920(2) 2_775 ?
O2 C3 1.235(16) 2_775 ?
O3 C1 1.16(3) . ?
O4 C3 1.278(15) . ?
C1 N1 1.27(3) . ?
C1 H1 0.9300 . ?
N1 C7 1.36(4) . ?
N1 C7 1.36(4) 4_556 ?
N1 C8 1.43(2) . ?
C3 O2 1.235(16) 3_575 ?
C3 C5 1.507(18) . ?
C4 C4 1.41(3) 8_676 ?
C4 C5 1.412(19) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(17) . ?
C6 C6 1.33(2) 8_676 ?
C6 H6 0.9300 . ?
Fe2 Cl1 2.028(16) . ?
Fe2 Cl1 2.028(16) . ?
Fe2 Cl1 2.028(16) . ?
Fe2 Cl2 2.19(2) . ?
Fe2 Cl2 2.19(2) . ?
Fe2 Cl2 2.19(2) . ?
Fe2 Cl2 2.19(2) . ?
Fe2 Cl2 2.19(2) . ?
Fe2 Cl2 2.19(2) . ?
Cl1 Fe2 2.028(16) . ?
Cl2 Fe2 2.19(2) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Fe1 O1 Fe1 -46.3(3) 4_556 . . 3_575 ?
O4 Fe1 O1 Fe1 46.3(3) . . . 3_575 ?
O2 Fe1 O1 Fe1 -132.0(3) 4_556 . . 3_575 ?
O2 Fe1 O1 Fe1 132.0(3) . . . 3_575 ?
O4 Fe1 O1 Fe1 133.7(3) 4_556 . . 2_775 ?
O4 Fe1 O1 Fe1 -133.7(3) . . . 2_775 ?
O2 Fe1 O1 Fe1 48.0(3) 4_556 . . 2_775 ?
O2 Fe1 O1 Fe1 -48.0(3) . . . 2_775 ?
O1 Fe1 O2 C3 13.9(12) . . . 2_775 ?
O4 Fe1 O2 C3 106.4(12) . . . 2_775 ?
O2 Fe1 O2 C3 -82.7(12) 4_556 . . 2_775 ?
O3 Fe1 O2 C3 -168.9(12) . . . 2_775 ?
O4 Fe1 O3 C1 46.5(3) 4_556 . . . ?
O4 Fe1 O3 C1 -46.5(3) . . . . ?
O2 Fe1 O3 C1 132.2(3) 4_556 . . . ?
O2 Fe1 O3 C1 -132.2(3) . . . . ?
O1 Fe1 O4 C3 -11.8(13) . . . . ?
O4 Fe1 O4 C3 81.2(13) 4_556 . . . ?
O2 Fe1 O4 C3 -107.5(13) . . . . ?
O3 Fe1 O4 C3 165.5(13) . . . . ?
Fe1 O3 C1 N1 180.0 . . . . ?
O3 C1 N1 C7 -59(4) . . . . ?
O3 C1 N1 C7 59(4) . . . 4_556 ?
O3 C1 N1 C8 180.0 . . . . ?
Fe1 O4 C3 O2 -21(2) . . . 3_575 ?
Fe1 O4 C3 C5 158.7(9) . . . . ?
C4 C4 C5 C6 3(3) 8_676 . . . ?
C4 C4 C5 C3 -176(2) 8_676 . . . ?
O2 C3 C5 C6 -8(2) 3_575 . . . ?
O4 C3 C5 C6 172.1(13) . . . . ?
O2 C3 C5 C4 171.5(15) 3_575 . . . ?
O4 C3 C5 C4 -8(2) . . . . ?
C4 C5 C6 C6 0(3) . . . 8_676 ?
C3 C5 C6 C6 179.9(15) . . . 8_676 ?
Cl2 Cl1 Cl2 Fe2 0.00(2) 8_676 . . 1_655 ?
