#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:52:29 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179676 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/28/4512835.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_4512835
loop_
_publ_author_name
'Fateeva, Alexandra'
'Clarisse, Jade'
'Pilet, Guillaume'
'Grenèche, Jean-Marc'
'Nouar, Farid'
'Abeykoon, Brian K.'
'Guegan, Frédéric'
'Goutaudier, Christelle'
'Luneau, Dominique'
'Warren, John E.'
'Rosseinsky, Matthew J.'
'Devic, Thomas'
_publ_section_title
;
 Iron and Porphyrin Metal--Organic Frameworks: Insight into Structural
 Diversity, Stability, and Porosity
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1819
_journal_paper_doi               10.1021/cg501855k
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C56 H32 Fe3 N8 O8'
_chemical_formula_sum            'C56 H32 Fe3 N8 O8'
_chemical_formula_weight         1112.44
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   16.6770(7)
_cell_length_b                   16.6770(7)
_cell_length_c                   16.5322(13)
_cell_measurement_reflns_used    1903
_cell_measurement_temperature    293
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     4598.0(5)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6805
_diffrn_reflns_theta_full        25.197
_diffrn_reflns_theta_max         29.299
_diffrn_reflns_theta_min         2.996
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.205
_refine_diff_density_max         0.84
_refine_diff_density_min         -0.48
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9257
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         887
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1386
_refine_ls_R_factor_gt           0.1020
_refine_ls_shift/su_max          0.0001614
_refine_ls_shift/su_mean         0.0000119
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 16.1 13.6 10.9 6.87 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1591
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.0997
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              21
_reflns_limit_k_min              1
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                1050
_reflns_number_total             1577
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   2.33
_oxford_diffrn_Wilson_scale      2.04
_oxford_refine_ls_r_factor_ref   0.0954
_oxford_refine_ls_scale          1.523(13)
_oxford_reflns_number_all        1570
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            cg501855k_si_004.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4512834--4512837.cif.'
_cod_original_sg_symbol_H-M      'I 4/m m m '
_cod_database_code               4512835
#BEGIN Tags that were not found in dictionaries:
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.010000 = C(15) TO N(16) 
END                                                                             
;
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z+1/2
-x+1/2,-y+1/2,-z+1/2
x,y,-z
-x,-y,z
x+1/2,y+1/2,-z+1/2
-x+1/2,-y+1/2,z+1/2
y,x,-z
-y,-x,z
y+1/2,x+1/2,-z+1/2
-y+1/2,-x+1/2,z+1/2
y,x,z
-y,-x,-z
y+1/2,x+1/2,z+1/2
-y+1/2,-x+1/2,-z+1/2
y,-x,-z
-y,x,z
y+1/2,-x+1/2,-z+1/2
-y+1/2,x+1/2,z+1/2
x,-y,-z
-x,y,z
x+1/2,-y+1/2,-z+1/2
-x+1/2,y+1/2,z+1/2
y,-x,z
-y,x,-z
y+1/2,-x+1/2,z+1/2
-y+1/2,x+1/2,-z+1/2
-x,y,-z
x,-y,z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Fe1 Fe 1.0000 1.0000 0.5000 0.0304 1.0000 Uani S T
N2 N 1.0000 0.8805(4) 0.5000 0.0322 1.0000 Uani S T
C3 C 0.9351(4) 0.8309(3) 0.5000 0.0432 1.0000 Uani S T
C4 C 0.9602(4) 0.7478(4) 0.5000 0.0630 1.0000 Uani S T
C5 C 0.8553(4) 0.8553(4) 0.5000 0.0451 1.0000 Uani S T
C6 C 0.7909(4) 0.7909(4) 0.5000 0.0545 1.0000 Uani S T
C7 C 0.7617(4) 0.7617(4) 0.4302(6) 0.0817 1.0000 Uani S T
C8 C 0.7030(4) 0.7030(4) 0.4294(6) 0.0758 1.0000 Uani S T
C9 C 0.6749(4) 0.6749(4) 0.5000 0.0524 1.0000 Uani S T
C10 C 0.6097(4) 0.6097(4) 0.5000 0.0514 1.0000 Uani S T
O11 O 0.5854(2) 0.5854(2) 0.4336(4) 0.0634 1.0000 Uani S T
Fe2 Fe 0.5000 0.5000 0.41633(12) 0.0356 1.0000 Uani S T
N13 N 0.5000 0.5000 0.2902(7) 0.0474 1.0000 Uani S T
C14 C 0.5484(6) 0.5484(6) 0.2462(12) 0.0839 0.5000 Uani S T
C15 C 0.5472(7) 0.5472(7) 0.1632(12) 0.0609 0.5000 Uani S TU
N16 N 0.5000 0.5000 0.1186(8) 0.0402 1.0000 Uani S TU
H81 H 0.6827 0.6827 0.3811 0.0922 1.0000 Uiso . .
H141 H 0.5841 0.5841 0.2730 0.0995 0.5000 Uiso . .
H151 H 0.5827 0.5827 0.1336 0.0702 0.5000 Uiso . .
H71 H 0.7821 0.7821 0.3808 0.0975 1.0000 Uiso . .
H41 H 0.9258 0.7017 0.5000 0.0745 1.0000 Uiso . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805
1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 2_776 Fe1 N2 14_776 90.00(2) yes
N2 2_776 Fe1 N2 17_576 90.00(2) yes
N2 14_776 Fe1 N2 17_576 179.994 yes
N2 2_776 Fe1 N2 . 179.994 yes
N2 14_776 Fe1 N2 . 90.00(2) yes
N2 17_576 Fe1 N2 . 90.00(2) yes
C3 22_755 N2 Fe1 . 127.4(3) yes
C3 22_755 N2 C3 . 105.1(7) yes
Fe1 . N2 C3 . 127.4(3) yes
N2 . C3 C4 . 110.6(5) yes
N2 . C3 C5 . 125.6(6) yes
C4 . C3 C5 . 123.8(6) yes
C3 . C4 C4 22_755 106.8(4) yes
C3 . C4 H41 . 126.6 no
C4 22_755 C4 H41 . 126.6 no
C3 . C5 C3 9_556 124.0(8) yes
C3 . C5 C6 . 118.0(4) yes
C3 9_556 C5 C6 . 118.0(4) yes
C5 . C6 C7 5_556 120.8(5) yes
C5 . C6 C7 . 120.8(5) yes
C7 5_556 C6 C7 . 118.4(10) yes
C6 . C7 C8 . 121.3(9) yes
C6 . C7 H71 . 118.6 no
C8 . C7 H71 . 120.0 no
C7 . C8 C9 . 119.2(9) yes
C7 . C8 H81 . 121.5 no
C9 . C8 H81 . 119.4 no
C8 . C9 C8 5_556 120.7(11) yes
C8 . C9 C10 . 119.7(6) yes
C8 5_556 C9 C10 . 119.7(6) yes
C9 . C10 O11 5_556 117.6(5) yes
C9 . C10 O11 . 117.6(5) yes
O11 5_556 C10 O11 . 124.9(10) yes
C10 . O11 Fe2 . 125.6(6) yes
Fe2 21_566 Fe2 O11 18_655 81.93(18) yes
Fe2 21_566 Fe2 O11 30_565 81.93(18) yes
O11 18_655 Fe2 O11 30_565 163.9(4) yes
Fe2 21_566 Fe2 N13 . 179.994 yes
O11 18_655 Fe2 N13 . 98.07(18) yes
O11 30_565 Fe2 N13 . 98.07(18) yes
Fe2 21_566 Fe2 O11 . 81.93(18) yes
O11 18_655 Fe2 O11 . 88.87(6) yes
O11 30_565 Fe2 O11 . 88.87(6) yes
N13 . Fe2 O11 . 98.07(18) yes
Fe2 . N13 C14 22_655 122.5(9) yes
Fe2 . N13 C14 25_565 122.5(9) yes
C14 22_655 N13 C14 25_565 115.0(18) yes
Fe2 . N13 C14 6_665 122.5(9) yes
C14 22_655 N13 C14 6_665 73.2(9) yes
C14 25_565 N13 C14 6_665 73.2(9) yes
Fe2 . N13 C14 . 122.5(9) yes
C14 22_655 N13 C14 . 73.2(9) yes
C14 25_565 N13 C14 . 73.2(9) yes
C14 6_665 N13 C14 . 115.0(18) yes
C14 25_565 C14 C14 18_655 90.00(2) yes
C14 25_565 C14 N13 . 53.4(4) yes
C14 18_655 C14 N13 . 53.4(4) yes
C14 25_565 C14 C15 . 89.2(6) yes
C14 18_655 C14 C15 . 89.2(6) yes
N13 . C14 C15 . 121.3(14) yes
C14 25_565 C14 H141 . 128.7 no
C14 18_655 C14 H141 . 128.7 no
N13 . C14 H141 . 119.7 no
C15 . C14 H141 . 119.0 no
C15 25_565 C15 C15 18_655 90.00(2) yes
C15 25_565 C15 C14 . 90.8(6) yes
C15 18_655 C15 C14 . 90.8(6) yes
C15 25_565 C15 N16 . 53.9(4) yes
C15 18_655 C15 N16 . 53.9(4) yes
C14 . C15 N16 . 124.7(14) yes
C15 25_565 C15 H151 . 127.6 no
C15 18_655 C15 H151 . 127.6 no
C14 . C15 H151 . 119.2 no
N16 . C15 H151 . 116.1 no
C15 10_665 N16 C15 18_655 72.2(8) yes
C15 10_665 N16 C15 25_565 72.2(8) yes
C15 18_655 N16 C15 25_565 112.9(17) yes
C15 10_665 N16 C15 . 112.9(17) yes
C15 18_655 N16 C15 . 72.2(8) yes
C15 25_565 N16 C15 . 72.2(8) yes
C15 10_665 N16 Fe1 3_444 123.5(9) yes
C15 18_655 N16 Fe1 3_444 123.5(9) yes
C15 25_565 N16 Fe1 3_444 123.5(9) yes
C15 . N16 Fe1 3_444 123.5(9) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 N2 2_776 1.992(6) yes
Fe1 N2 14_776 1.992(6) yes
Fe1 N2 17_576 1.992(6) yes
Fe1 N2 . 1.992(6) yes
N2 C3 22_755 1.363(7) yes
N2 C3 . 1.363(7) yes
C3 C4 . 1.446(9) yes
C3 C5 . 1.392(7) yes
C4 C4 22_755 1.328(15) yes
C4 H41 . 0.960 no
C5 C6 . 1.519(12) yes
C6 C7 5_556 1.344(10) yes
C6 C7 . 1.344(10) yes
C7 C8 . 1.384(12) yes
C7 H71 . 0.948 no
C8 C9 . 1.342(10) yes
C8 H81 . 0.932 no
C9 C10 . 1.537(15) yes
C10 O11 5_556 1.238(7) yes
C10 O11 . 1.238(7) yes
O11 Fe2 . 2.035(5) yes
Fe2 Fe2 21_566 2.767(4) yes
Fe2 N13 . 2.086(12) yes
N13 C14 22_655 1.353(17) yes
N13 C14 25_565 1.353(17) yes
N13 C14 6_665 1.353(17) yes
N13 C14 . 1.353(17) yes
C14 C14 25_565 1.614(19) yes
C14 C14 18_655 1.614(19) yes
C14 C15 . 1.37(3) yes
C14 H141 . 0.951 no
C15 C15 25_565 1.58(2) yes
C15 C15 18_655 1.58(2) yes
C15 N16 . 1.34(2) yes
C15 H151 . 0.970 no
