#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:04:36 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178834 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/88/4108838.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_4108838
loop_
_publ_author_name
'Pierre Dechambenoit'
'Sylvie Ferlay'
'Nathalie Kyritsakas'
'Mir Wais Hosseini'
_publ_section_title
;
 Molecular Tectonics: Control of Reversible Water Release in Porous
 Charge-Assisted H-Bonded Networks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17106
_journal_page_last               17113
_journal_paper_doi               10.1021/ja806916t
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         '3(C14 H20 N4), 2(C6 Fe N6)'
_chemical_formula_sum            'C54 H60 Fe2 N24'
_chemical_formula_weight         1156.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.987(2)
_cell_angle_beta                 89.044(3)
_cell_angle_gamma                83.821(2)
_cell_formula_units_Z            1
_cell_length_a                   7.2138(6)
_cell_length_b                   12.1706(11)
_cell_length_c                   17.3090(16)
_cell_measurement_reflns_used    1722
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.14
_cell_measurement_theta_min      2.84
_cell_volume                     1505.0(2)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0824
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10289
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.9684
_exptl_absorpt_correction_T_min  0.9481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0487
_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                4018
_reflns_number_total             6335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja806916t_si_008.cif
_cod_data_source_block           e990a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4108838
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
C1 C 0.8298(3) 0.8456(2) 1.00089(15) 0.0239(7) Uani 1 1 d .
N1 N 0.8302(3) 0.75016(18) 1.04267(12) 0.0267(6) Uani 1 1 d .
H1 H 0.7268 0.7347 1.0670 0.032 Uiso 1 1 calc R
C2 C 0.9952(4) 0.6678(2) 1.05081(16) 0.0341(8) Uani 1 1 d .
H2A H 0.9559 0.5921 1.0562 0.041 Uiso 1 1 calc R
H2B H 1.0648 0.6784 1.0979 0.041 Uiso 1 1 calc R
C3 C 1.1199(4) 0.6815(2) 0.97968(17) 0.0400(9) Uani 1 1 d .
H3A H 1.0592 0.6572 0.9342 0.048 Uiso 1 1 calc R
H3B H 1.2399 0.6347 0.9883 0.048 Uiso 1 1 calc R
C4 C 1.1549(3) 0.8018(2) 0.96411(17) 0.0334(8) Uani 1 1 d .
H4A H 1.2313 0.8232 1.0062 0.040 Uiso 1 1 calc R
H4B H 1.2243 0.8122 0.9146 0.040 Uiso 1 1 calc R
N2 N 0.9766(3) 0.87178(18) 0.95976(12) 0.0261(6) Uani 1 1 d .
H2 H 0.9670 0.9333 0.9287 0.031 Uiso 1 1 calc R
C5 C 0.6589(3) 0.9252(2) 1.00011(15) 0.0211(7) Uani 1 1 d .
C6 C 0.5758(3) 0.9520(2) 1.07051(15) 0.0219(7) Uani 1 1 d .
H6 H 0.6274 0.9194 1.1183 0.026 Uiso 1 1 calc R
C7 C 0.4171(3) 1.0269(2) 1.06941(16) 0.0237(7) Uani 1 1 d .
H7 H 0.3595 1.0456 1.1169 0.028 Uiso 1 1 calc R
C8 C 0.7928(3) 0.0779(2) 0.40223(15) 0.0186(6) Uani 1 1 d .
N3 N 0.9344(3) 0.11495(17) 0.43493(12) 0.0239(6) Uani 1 1 d .
H3 H 0.9319 0.1197 0.4854 0.029 Uiso 1 1 calc R
C9 C 1.0960(3) 0.1485(2) 0.39029(16) 0.0349(8) Uani 1 1 d .
H9A H 1.1921 0.0843 0.3884 0.042 Uiso 1 1 calc R
H9B H 1.1507 0.2071 0.4158 0.042 Uiso 1 1 calc R
C10 C 1.0372(4) 0.1915(2) 0.30923(16) 0.0341(8) Uani 1 1 d .
H10A H 1.1491 0.2036 0.2770 0.041 Uiso 1 1 calc R
H10B H 0.9599 0.2637 0.3106 0.041 Uiso 1 1 calc R
C11 C 0.9268(4) 0.1100(2) 0.27330(16) 0.0296(7) Uani 1 1 d .
H11A H 0.8705 0.1449 0.2241 0.036 Uiso 1 1 calc R
H11B H 1.0110 0.0438 0.2614 0.036 Uiso 1 1 calc R
N4 N 0.7791(3) 0.07650(17) 0.32704(12) 0.0222(5) Uani 1 1 d .
H4 H 0.6781 0.0548 0.3080 0.027 Uiso 1 1 calc R
C12 C 0.6408(3) 0.0371(2) 0.45287(15) 0.0182(6) Uani 1 1 d .
C13 C 0.5629(3) 0.1018(2) 0.50995(14) 0.0206(6) Uani 1 1 d .
H13 H 0.6070 0.1712 0.5166 0.025 Uiso 1 1 calc R
C14 C 0.4204(3) 0.0650(2) 0.55739(15) 0.0202(6) Uani 1 1 d .
H14 H 0.3657 0.1090 0.5962 0.024 Uiso 1 1 calc R
C15 C 0.2847(3) 0.5516(2) 0.60047(16) 0.0204(6) Uani 1 1 d .
N5 N 0.2687(3) 0.52981(18) 0.67560(12) 0.0234(6) Uani 1 1 d .
H5 H 0.1665 0.5031 0.6939 0.028 Uiso 1 1 calc R
C16 C 0.4123(3) 0.5476(2) 0.73076(16) 0.0285(7) Uani 1 1 d .
H16A H 0.4963 0.4783 0.7416 0.034 Uiso 1 1 calc R
H16B H 0.3529 0.5681 0.7802 0.034 Uiso 1 1 calc R
C17 C 0.5241(4) 0.6396(2) 0.69717(16) 0.0331(8) Uani 1 1 d .
H17A H 0.4464 0.7119 0.6966 0.040 Uiso 1 1 calc R
H17B H 0.6343 0.6428 0.7299 0.040 Uiso 1 1 calc R
C18 C 0.5866(3) 0.6182(2) 0.61535(16) 0.0355(8) Uani 1 1 d .
H18A H 0.6445 0.6831 0.5912 0.043 Uiso 1 1 calc R
H18B H 0.6813 0.5529 0.6169 0.043 Uiso 1 1 calc R
N6 N 0.4294(3) 0.59844(18) 0.56906(13) 0.0272(6) Uani 1 1 d .
H6A H 0.4301 0.6180 0.5189 0.033 Uiso 1 1 calc R
C19 C 0.1372(3) 0.5248(2) 0.54859(15) 0.0198(6) Uani 1 1 d .
C20 C 0.0724(3) 0.4209(2) 0.55804(15) 0.0206(7) Uani 1 1 d .
H20 H 0.1221 0.3671 0.5975 0.025 Uiso 1 1 calc R
C21 C 0.0654(3) 0.6035(2) 0.49065(15) 0.0217(7) Uani 1 1 d .
H21 H 0.1109 0.6742 0.4844 0.026 Uiso 1 1 calc R
Fe2 Fe 0.74332(5) 0.22100(4) 0.73719(2) 0.02124(11) Uani 1 1 d .
C22 C 0.5808(4) 0.2764(2) 0.81956(16) 0.0242(7) Uani 1 1 d .
N7 N 0.4889(3) 0.30923(19) 0.86942(14) 0.0369(7) Uani 1 1 d .
C23 C 0.8745(3) 0.3523(2) 0.74004(15) 0.0219(7) Uani 1 1 d .
N8 N 0.9491(3) 0.4319(2) 0.74119(13) 0.0327(6) Uani 1 1 d .
C24 C 0.5934(3) 0.2977(2) 0.65250(16) 0.0214(7) Uani 1 1 d .
N9 N 0.5188(3) 0.34008(19) 0.59716(13) 0.0274(6) Uani 1 1 d .
C25 C 0.8995(3) 0.1670(2) 0.65345(16) 0.0205(7) Uani 1 1 d .
N10 N 0.9789(3) 0.13826(18) 0.59875(13) 0.0263(6) Uani 1 1 d .
C26 C 0.6109(3) 0.0899(2) 0.73519(15) 0.0223(7) Uani 1 1 d .
N11 N 0.5370(3) 0.0106(2) 0.73451(13) 0.0314(6) Uani 1 1 d .
C27 C 0.8996(3) 0.1350(2) 0.81669(15) 0.0208(7) Uani 1 1 d .
N12 N 0.9824(3) 0.07842(19) 0.86346(13) 0.0276(6) 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
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 '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
N2 C1 N1 121.7(2) . .
N2 C1 C5 119.6(2) . .
N1 C1 C5 118.7(2) . .
C1 N1 C2 123.2(2) . .
C1 N1 H1 118.4 . .
C2 N1 H1 118.4 . .
N1 C2 C3 109.4(2) . .
N1 C2 H2A 109.8 . .
C3 C2 H2A 109.8 . .
N1 C2 H2B 109.8 . .
C3 C2 H2B 109.8 . .
H2A C2 H2B 108.3 . .
C2 C3 C4 109.8(2) . .
C2 C3 H3A 109.7 . .
C4 C3 H3A 109.7 . .
C2 C3 H3B 109.7 . .
C4 C3 H3B 109.7 . .
H3A C3 H3B 108.2 . .
N2 C4 C3 109.5(2) . .
N2 C4 H4A 109.8 . .
C3 C4 H4A 109.8 . .
N2 C4 H4B 109.8 . .
C3 C4 H4B 109.8 . .
H4A C4 H4B 108.2 . .
C1 N2 C4 122.1(2) . .
C1 N2 H2 119.0 . .
C4 N2 H2 119.0 . .
C7 C5 C6 120.3(2) 2_677 .
C7 C5 C1 120.6(2) 2_677 .
C6 C5 C1 119.2(2) . .
C7 C6 C5 118.9(2) . .
C7 C6 H6 120.5 . .
C5 C6 H6 120.5 . .
C6 C7 C5 120.8(2) . 2_677
C6 C7 H7 119.6 . .
C5 C7 H7 119.6 2_677 .
N4 C8 N3 122.6(2) . .
N4 C8 C12 118.8(2) . .
N3 C8 C12 118.7(2) . .
C8 N3 C9 122.3(2) . .
C8 N3 H3 118.9 . .
C9 N3 H3 118.9 . .
N3 C9 C10 109.7(2) . .
N3 C9 H9A 109.7 . .
C10 C9 H9A 109.7 . .
N3 C9 H9B 109.7 . .
C10 C9 H9B 109.7 . .
H9A C9 H9B 108.2 . .
C9 C10 C11 110.7(2) . .
C9 C10 H10A 109.5 . .
C11 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
C11 C10 H10B 109.5 . .
H10A C10 H10B 108.1 . .
N4 C11 C10 110.0(2) . .
N4 C11 H11A 109.7 . .
C10 C11 H11A 109.7 . .
N4 C11 H11B 109.7 . .
C10 C11 H11B 109.7 . .
H11A C11 H11B 108.2 . .
C8 N4 C11 122.2(2) . .
C8 N4 H4 118.9 . .
C11 N4 H4 118.9 . .
C14 C12 C13 121.0(2) 2_656 .
C14 C12 C8 119.6(2) 2_656 .
C13 C12 C8 119.4(2) . .
C12 C13 C14 120.0(2) . .
C12 C13 H13 120.0 . .
C14 C13 H13 120.0 . .
C12 C14 C13 119.0(2) 2_656 .
C12 C14 H14 120.5 2_656 .
C13 C14 H14 120.5 . .
N5 C15 N6 121.7(2) . .
N5 C15 C19 119.7(2) . .
N6 C15 C19 118.7(2) . .
C15 N5 C16 123.3(2) . .
C15 N5 H5 118.3 . .
C16 N5 H5 118.3 . .
N5 C16 C17 109.7(2) . .
N5 C16 H16A 109.7 . .
C17 C16 H16A 109.7 . .
N5 C16 H16B 109.7 . .
C17 C16 H16B 109.7 . .
H16A C16 H16B 108.2 . .
C18 C17 C16 109.8(2) . .
C18 C17 H17A 109.7 . .
C16 C17 H17A 109.7 . .
C18 C17 H17B 109.7 . .
C16 C17 H17B 109.7 . .
H17A C17 H17B 108.2 . .
N6 C18 C17 110.6(2) . .
N6 C18 H18A 109.5 . .
C17 C18 H18A 109.5 . .
N6 C18 H18B 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 108.1 . .
C15 N6 C18 121.7(2) . .
C15 N6 H6A 119.1 . .
C18 N6 H6A 119.1 . .
C21 C19 C20 120.4(2) . .
C21 C19 C15 119.9(3) . .
C20 C19 C15 119.7(3) . .
C21 C20 C19 119.4(3) 2_566 .
C21 C20 H20 120.3 2_566 .
C19 C20 H20 120.3 . .
C19 C21 C20 120.2(3) . 2_566
C19 C21 H21 119.9 . .
C20 C21 H21 119.9 2_566 .
C25 Fe2 C24 83.19(11) . .
C25 Fe2 C23 92.35(11) . .
C24 Fe2 C23 88.79(11) . .
C25 Fe2 C22 178.51(12) . .
C24 Fe2 C22 95.38(11) . .
C23 Fe2 C22 88.04(10) . .
C25 Fe2 C26 88.15(11) . .
C24 Fe2 C26 91.35(11) . .
C23 Fe2 C26 179.49(12) . .
C22 Fe2 C26 91.45(11) . .
C25 Fe2 C27 92.89(10) . .
C24 Fe2 C27 175.48(12) . .
C23 Fe2 C27 93.63(11) . .
C22 Fe2 C27 88.52(11) . .
C26 Fe2 C27 86.27(11) . .
N7 C22 Fe2 178.2(3) . .
N8 C23 Fe2 178.5(3) . .
N9 C24 Fe2 173.1(2) . .
N10 C25 Fe2 173.5(2) . .
N11 C26 Fe2 178.1(2) . .
N12 C27 Fe2 174.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.318(3) .
C1 N1 1.313(3) .
C1 C5 1.484(3) .
N1 C2 1.471(3) .
N1 H1 0.8800 .
C2 C3 1.520(3) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.512(4) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 N2 1.464(3) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
N2 H2 0.8800 .
C5 C7 1.385(3) 2_677
C5 C6 1.398(3) .
C6 C7 1.383(3) .
C6 H6 0.9500 .
C7 C5 1.385(3) 2_677
C7 H7 0.9500 .
C8 N4 1.308(3) .
C8 N3 1.316(3) .
C8 C12 1.492(3) .
N3 C9 1.463(3) .
N3 H3 0.8800 .
C9 C10 1.505(4) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.516(3) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 N4 1.470(3) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
N4 H4 0.8800 .
C12 C14 1.388(3) 2_656
C12 C13 1.391(3) .
C13 C14 1.393(3) .
C13 H13 0.9500 .
C14 C12 1.388(3) 2_656
C14 H14 0.9500 .
C15 N5 1.310(3) .
C15 N6 1.329(3) .
C15 C19 1.484(3) .
N5 C16 1.466(3) .
N5 H5 0.8800 .
C16 C17 1.519(3) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.515(3) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 N6 1.452(3) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
N6 H6A 0.8800 .
C19 C21 1.391(3) .
C19 C20 1.391(3) .
C20 C21 1.386(3) 2_566
C20 H20 0.9500 .
C21 C20 1.386(3) 2_566
C21 H21 0.9500 .
Fe2 C25 1.938(3) .
Fe2 C24 1.946(3) .
Fe2 C23 1.947(3) .
Fe2 C22 1.950(3) .
Fe2 C26 1.949(3) .
Fe2 C27 1.951(3) .
C22 N7 1.152(3) .
C23 N8 1.160(3) .
C24 N9 1.159(3) .
C25 N10 1.159(3) .
C26 N11 1.152(3) .
C27 N12 1.147(3) .
