#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:52:29 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179676 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/28/4512834.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_4512834
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_absolute_configuration ad
_chemical_formula_moiety         'C52 H30 Fe3 N6 O10'
_chemical_formula_sum            'C52 H30 Fe3 N6 O10'
_chemical_formula_weight         1066.39
_space_group_IT_number           65
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2 2'
_symmetry_space_group_name_H-M   'C 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                   6.8353(16)
_cell_length_b                   32.355(4)
_cell_length_c                   16.8960(19)
_cell_measurement_reflns_used    1122
_cell_measurement_temperature    293
_cell_measurement_theta_max      24
_cell_measurement_theta_min      4
_cell_volume                     3736.7(11)
_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 0.983
_diffrn_measured_fraction_theta_max 0.872
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.098
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6623
_diffrn_reflns_theta_full        25.290
_diffrn_reflns_theta_max         29.407
_diffrn_reflns_theta_min         2.792
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    0.948
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.83
_refine_diff_density_min         -1.40
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0607
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1055
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1727
_refine_ls_R_factor_gt           0.0942
_refine_ls_shift/su_max          0.0000836
_refine_ls_shift/su_mean         0.0000069
_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: 
 3.21 -0.518 2.62 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0783
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0698
_reflns_limit_h_max              9
_reflns_limit_h_min              0
_reflns_limit_k_max              43
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                1402
_reflns_number_total             2554
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   1.09
_oxford_diffrn_Wilson_scale      92.38
_oxford_refine_ls_r_factor_ref   0.0656
_oxford_refine_ls_scale          0.2536(13)
_oxford_reflns_number_all        2530
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            cg501855k_si_005.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4512834--4512837.cif.'
_cod_original_cell_volume        3737(1)
_cod_original_sg_symbol_H-M      'C m m m '
_cod_database_code               4512834
#BEGIN Tags that were not found in dictionaries:
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE O   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
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
-x+1/2,-y+1/2,-z
x,-y,z
-x,y,-z
x+1/2,-y+1/2,z
-x+1/2,y+1/2,-z
-x,-y,z
x,y,-z
-x+1/2,-y+1/2,z
x+1/2,y+1/2,-z
x,-y,-z
-x,y,z
x+1/2,-y+1/2,-z
-x+1/2,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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Fe1 Fe 0.0000 0.5000 0.5000 0.0227 1.0000 Uani S T
N2 N 0.0000 0.4384(2) 0.5000 0.0276 1.0000 Uani S T
C3 C 0.0000 0.4125(2) 0.4356(4) 0.0380 1.0000 Uani S T
C4 C 0.0000 0.4255(2) 0.3563(4) 0.0348 1.0000 Uani S T
C5 C 0.0000 0.4659(2) 0.3326(4) 0.0320 1.0000 Uani S T
N6 N 0.0000 0.5000 0.3817(4) 0.0314 1.0000 Uani S T
C7 C 0.000000(7) 0.4794(2) 0.2512(4) 0.0495 1.0000 Uani S T
C8 C 0.0000 0.3922(2) 0.2940(4) 0.0445 1.0000 Uani S T
C9 C -0.1696(13) 0.3772(2) 0.2640(4) 0.0783 1.0000 Uani . .
C10 C -0.1709(12) 0.3475(2) 0.2051(4) 0.0762 1.0000 Uani . .
C11 C 0.0000 0.3327(2) 0.1744(4) 0.0364 1.0000 Uani S T
C12 C 0.0000 0.3010(2) 0.1097(4) 0.0352 1.0000 Uani S T
O13 O 0.1615(6) 0.28965(13) 0.0847(2) 0.0523 1.0000 Uani . .
Fe14 Fe 0.2500 0.2500 0.0000 0.0259 1.0000 Uani S T
O15 O 0.500000(7) 0.2778(2) 0.000000(7) 0.0296 1.0000 Uani S T
C16 C 0.000000(7) 0.3701(2) 0.4604(5) 0.0531 1.0000 Uani S T
N17 N 0.2897(13) 0.5000 0.5000 0.0310 1.0000 Uani S T
C1 C 0.3977(16) 0.5241(3) 0.5469(6) 0.0387 0.5000 Uani . .
H71 H 0.0000 0.4621 0.2067 0.0601 1.0000 Uiso RS .
H101 H -0.2878 0.3377 0.1861 0.0890 1.0000 Uiso R .
H91 H -0.2877 0.3867 0.2840 0.0932 1.0000 Uiso R .
H11 H 0.3146 0.5407 0.5787 0.0602 0.5000 Uiso R .
H161 H 0.0000 0.3462 0.4271 0.0626 1.0000 Uiso RS .
H151 H 0.5000 0.3074 0.0000 0.0371 1.0000 Uiso RS .
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
N6 10_556 Fe1 N2 2_566 90.00 yes
N6 10_556 Fe1 N17 2_566 90.00 yes
N2 2_566 Fe1 N17 2_566 90.00 yes
N6 10_556 Fe1 N2 . 90.00 yes
N2 2_566 Fe1 N2 . 180.00 yes
N17 2_566 Fe1 N2 . 90.00 yes
N6 10_556 Fe1 N6 . 180.00 yes
N2 2_566 Fe1 N6 . 90.00 yes
N17 2_566 Fe1 N6 . 90.00 yes
N2 . Fe1 N6 . 90.00 yes
N6 10_556 Fe1 N17 . 90.00 yes
N2 2_566 Fe1 N17 . 90.00 yes
N17 2_566 Fe1 N17 . 180.00 yes
N2 . Fe1 N17 . 90.00 yes
N6 . Fe1 N17 . 90.00 yes
C3 6_556 N2 Fe1 . 127.6(4) yes
C3 6_556 N2 C3 . 104.9(7) yes
Fe1 . N2 C3 . 127.6(4) yes
N2 . C3 C4 . 125.0(6) yes
N2 . C3 C16 . 110.5(6) yes
C4 . C3 C16 . 124.4(6) yes
C3 . C4 C5 . 124.4(6) yes
C3 . C4 C8 . 116.9(6) yes
C5 . C4 C8 . 118.6(6) yes
C4 . C5 N6 . 126.0(6) yes
C4 . C5 C7 . 124.6(6) yes
N6 . C5 C7 . 109.4(6) yes
C5 9_565 N6 C5 . 106.0(7) yes
C5 9_565 N6 Fe1 . 127.0(4) yes
C5 . N6 Fe1 . 127.0(4) yes
C5 . C7 C7 5_565 107.6(4) yes
C5 . C7 H71 . 125.6 no
C7 5_565 C7 H71 . 126.8 no
C4 . C8 C9 14_555 121.2(4) yes
C4 . C8 C9 . 121.2(4) yes
C9 14_555 C8 C9 . 117.5(8) yes
C8 . C9 C10 . 121.6(7) yes
C8 . C9 H91 . 119.3 no
C10 . C9 H91 . 119.1 no
C9 . C10 C11 . 120.8(7) yes
C9 . C10 H101 . 119.8 no
C11 . C10 H101 . 119.4 no
C10 . C11 C10 14_555 117.7(8) yes
C10 . C11 C12 . 121.1(4) yes
C10 14_555 C11 C12 . 121.1(4) yes
C11 . C12 O13 14_555 116.9(3) yes
C11 . C12 O13 . 116.9(3) yes
O13 14_555 C12 O13 . 126.2(7) yes
C12 . O13 Fe14 . 134.4(4) yes
O13 . Fe14 O13 4_555 179.994 yes
O13 . Fe14 O13 11_555 89.5(3) yes
O13 4_555 Fe14 O13 11_555 90.5(3) yes
O13 . Fe14 O13 10_555 90.5(3) yes
O13 4_555 Fe14 O13 10_555 89.5(3) yes
O13 11_555 Fe14 O13 10_555 179.994 yes
O13 . Fe14 O15 4_555 91.77(17) yes
O13 4_555 Fe14 O15 4_555 88.23(17) yes
O13 11_555 Fe14 O15 4_555 88.23(17) yes
O13 10_555 Fe14 O15 4_555 91.77(17) yes
O13 . Fe14 O15 . 88.23(17) yes
O13 4_555 Fe14 O15 . 91.77(17) yes
O13 11_555 Fe14 O15 . 91.77(17) yes
O13 10_555 Fe14 O15 . 88.23(17) yes
O15 4_555 Fe14 O15 . 179.994 yes
Fe14 15_555 O15 Fe14 . 124.5(4) yes
Fe14 15_555 O15 H151 . 117.8 no
Fe14 . O15 H151 . 117.8 no
C3 . C16 C16 6_556 107.0(4) yes
C3 . C16 H161 . 127.0 no
C16 6_556 C16 H161 . 126.0 no
C1 13_566 N17 C1 5_565 73.0(9) yes
C1 13_566 N17 C1 10_556 71.4(10) yes
C1 5_565 N17 C1 10_556 112.8(11) yes
C1 13_566 N17 Fe1 . 123.6(6) yes
C1 5_565 N17 Fe1 . 123.6(6) yes
C1 10_556 N17 Fe1 . 123.6(6) yes
C1 13_566 N17 C1 . 112.8(11) yes
C1 5_565 N17 C1 . 71.4(10) yes
C1 10_556 N17 C1 . 73.0(9) yes
Fe1 . N17 C1 . 123.6(6) yes
C1 5_565 C1 C1 10_556 90.00(2) yes
C1 5_565 C1 C1 14_655 90.00(4) yes
C1 10_556 C1 C1 14_655 90.00(5) yes
C1 5_565 C1 N17 . 54.3(5) yes
C1 10_556 C1 N17 . 53.5(5) yes
C1 14_655 C1 N17 . 123.6(6) yes
C1 5_565 C1 H11 . 124.6 no
C1 10_556 C1 H11 . 124.5 no
C1 14_655 C1 H11 . 126.7 no
N17 . C1 H11 . 109.7 no
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 N6 10_556 1.998(7) yes
Fe1 N2 2_566 1.992(8) yes
Fe1 N17 2_566 1.980(9) yes
Fe1 N2 . 1.992(8) yes
Fe1 N6 . 1.998(7) yes
Fe1 N17 . 1.980(9) yes
N2 C3 6_556 1.374(8) yes
N2 C3 . 1.374(8) yes
C3 C4 . 1.404(9) yes
C3 C16 . 1.434(10) yes
C4 C5 . 1.368(10) yes
C4 C8 . 1.505(9) yes
C5 N6 . 1.380(8) yes
C5 C7 . 1.443(9) yes
C7 C7 5_565 1.330(15) yes
C7 H71 . 0.939 no
C8 C9 14_555 1.356(8) yes
C8 C9 . 1.356(8) yes
C9 C10 . 1.383(8) yes
C9 H91 . 0.927 no
C10 C11 . 1.365(8) yes
C10 H101 . 0.917 no
C11 C12 . 1.499(9) yes
C12 O13 14_555 1.238(5) yes
C12 O13 . 1.238(5) yes
O13 Fe14 . 2.015(4) yes
Fe14 O15 4_555 1.931(3) yes
Fe14 O15 . 1.931(3) yes
O15 H151 . 0.957 no
C16 C16 6_556 1.338(16) yes
C16 H161 . 0.956 no
N17 C1 13_566 1.334(11) yes
N17 C1 5_565 1.334(11) yes
N17 C1 10_556 1.334(11) yes
N17 C1 . 1.334(11) yes
C1 C1 5_565 1.56(2) yes
C1 C1 10_556 1.59(2) yes
C1 C1 14_655 1.40(2) yes
C1 H11 . 0.950 no
#BEGIN Loops that were not found in dictionaries:
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
0 6 3 x
0 6 2 x
0 2 4 x
7 19 6 x
8 12 5 x
1 33 8 x
9 13 1 x
2 40 4 x
1 33 7 x
3 31 6 x
1 3 2 x
0 6 4 x
5 23 1 x
#END Loops that were not found in dictionaries
