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#$Date: 2025-08-20 17:12:52 +0300 (Wed, 20 Aug 2025) $
#$Revision: 301832 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/10/88/4108835.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_4108835
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 Cr N6), 6(H2 O), H2 O'
_chemical_formula_sum            'C54 H74 Cr2 N24 O7'
_chemical_formula_weight         1275.37
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 91.702(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.1142(4)
_cell_length_b                   21.4319(13)
_cell_length_c                   20.9403(13)
_cell_measurement_reflns_used    2735
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      2.72
_cell_volume                     3191.4(3)
_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 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0889
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20747
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_T_max  0.9798
_exptl_absorpt_correction_T_min  0.9412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6630
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0757P)²+2.5725P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1825
_reflns_number_gt                4466
_reflns_number_total             6630
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja806916t_si_005.cif
_cod_data_source_block           e1154a
_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               4108835
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 1.2262(5) 0.31427(18) 0.69532(17) 0.0197(8) Uani 1 1 d .
N1 N 1.3726(4) 0.32055(17) 0.65886(16) 0.0300(8) Uani 1 1 d .
H1 H 1.3675 0.3050 0.6200 0.036 Uiso 1 1 calc R
C2 C 1.5441(6) 0.3528(2) 0.6813(2) 0.0425(12) Uani 1 1 d .
H2A H 1.6054 0.3726 0.6446 0.051 Uiso 1 1 calc R
H2B H 1.6331 0.3222 0.7007 0.051 Uiso 1 1 calc R
C3 C 1.4996(6) 0.4008(2) 0.7288(2) 0.0445(12) Uani 1 1 d .
H3A H 1.4344 0.4360 0.7070 0.053 Uiso 1 1 calc R
H3B H 1.6181 0.4169 0.7484 0.053 Uiso 1 1 calc R
C4 C 1.3776(5) 0.3759(2) 0.78028(19) 0.0280(9) Uani 1 1 d .
H4A H 1.4531 0.3487 0.8093 0.034 Uiso 1 1 calc R
H4B H 1.3286 0.4110 0.8056 0.034 Uiso 1 1 calc R
N2 N 1.2204(4) 0.34033(15) 0.75181(14) 0.0215(7) Uani 1 1 d .
H2 H 1.1174 0.3363 0.7737 0.026 Uiso 1 1 calc R
C5 C 1.0636(4) 0.27665(18) 0.67157(17) 0.0199(8) Uani 1 1 d .
C6 C 0.9882(4) 0.28637(18) 0.60982(17) 0.0212(8) Uani 1 1 d .
H6 H 1.0411 0.3172 0.5831 0.025 Uiso 1 1 calc R
C7 C 0.8365(4) 0.25108(19) 0.58758(17) 0.0215(8) Uani 1 1 d .
H7 H 0.7850 0.2577 0.5458 0.026 Uiso 1 1 calc R
C8 C 0.7600(4) 0.20573(18) 0.62712(17) 0.0208(8) Uani 1 1 d .
C9 C 0.8353(5) 0.19589(18) 0.68854(18) 0.0218(8) Uani 1 1 d .
H9 H 0.7839 0.1646 0.7150 0.026 Uiso 1 1 calc R
C10 C 0.9861(5) 0.23199(18) 0.71115(18) 0.0219(8) Uani 1 1 d .
H10 H 1.0357 0.2261 0.7533 0.026 Uiso 1 1 calc R
C11 C 0.5986(4) 0.16699(18) 0.60440(18) 0.0210(8) Uani 1 1 d .
N3 N 0.5905(4) 0.14716(15) 0.54484(14) 0.0225(7) Uani 1 1 d .
H3 H 0.6876 0.1541 0.5208 0.027 Uiso 1 1 calc R
C12 C 0.4273(5) 0.1140(2) 0.51660(19) 0.0282(9) Uani 1 1 d .
H12A H 0.4553 0.0688 0.5142 0.034 Uiso 1 1 calc R
H12B H 0.4014 0.1294 0.4726 0.034 Uiso 1 1 calc R
C13 C 0.2560(5) 0.1241(2) 0.55652(19) 0.0286(9) Uani 1 1 d .
H13A H 0.1547 0.0952 0.5424 0.034 Uiso 1 1 calc R
H13B H 0.2096 0.1674 0.5505 0.034 Uiso 1 1 calc R
C14 C 0.3048(5) 0.11311(19) 0.62670(19) 0.0249(9) Uani 1 1 d .
H14A H 0.1960 0.1238 0.6530 0.030 Uiso 1 1 calc R
H14B H 0.3363 0.0686 0.6339 0.030 Uiso 1 1 calc R
N4 N 0.4672(4) 0.15265(15) 0.64500(15) 0.0241(7) Uani 1 1 d .
H4 H 0.4767 0.1672 0.6843 0.029 Uiso 1 1 calc R
C15 C 0.2905(5) 0.00562(18) 0.90772(18) 0.0210(8) Uani 1 1 d .
N5 N 0.4435(4) -0.02752(15) 0.91767(15) 0.0251(7) Uani 1 1 d .
H5 H 0.4503 -0.0526 0.9510 0.030 Uiso 1 1 calc R
C16 C 0.6038(5) -0.0243(2) 0.8752(2) 0.0360(11) Uani 1 1 d .
H16A H 0.6710 -0.0647 0.8757 0.043 Uiso 1 1 calc R
H16B H 0.6926 0.0084 0.8906 0.043 Uiso 1 1 calc R
C17 C 0.5360(6) -0.0094(2) 0.8087(2) 0.0360(11) Uani 1 1 d .
H17A H 0.4657 -0.0455 0.7907 0.043 Uiso 1 1 calc R
H17B H 0.6450 -0.0014 0.7816 0.043 Uiso 1 1 calc R
C18 C 0.4098(5) 0.0474(2) 0.80862(19) 0.0296(9) Uani 1 1 d .
H18A H 0.4859 0.0851 0.8180 0.036 Uiso 1 1 calc R
H18B H 0.3487 0.0525 0.7659 0.036 Uiso 1 1 calc R
N6 N 0.2665(4) 0.04024(15) 0.85663(14) 0.0227(7) Uani 1 1 d .
H6A H 0.1591 0.0601 0.8509 0.027 Uiso 1 1 calc R
C19 C 0.1401(4) 0.00291(18) 0.95531(17) 0.0190(8) Uani 1 1 d .
C20 C 0.0854(5) -0.05450(18) 0.97979(17) 0.0210(8) Uani 1 1 d .
H20 H 0.1441 -0.0917 0.9659 0.025 Uiso 1 1 calc R
C21 C 0.0549(4) 0.05758(18) 0.97547(18) 0.0211(8) Uani 1 1 d .
H21 H 0.0922 0.0967 0.9588 0.025 Uiso 1 1 calc R
Cr1 Cr 0.67148(7) 0.22131(3) 0.89704(3) 0.01747(17) Uani 1 1 d .
C22 C 0.8427(5) 0.15447(19) 0.85636(17) 0.0223(8) Uani 1 1 d .
N7 N 0.9300(5) 0.11619(17) 0.83301(17) 0.0329(8) Uani 1 1 d .
C23 C 0.5020(5) 0.21360(17) 0.81549(18) 0.0197(8) Uani 1 1 d .
N8 N 0.4198(4) 0.20695(16) 0.76737(16) 0.0274(8) Uani 1 1 d .
C24 C 0.5337(5) 0.15086(18) 0.94464(18) 0.0210(8) Uani 1 1 d .
N9 N 0.4780(4) 0.11141(16) 0.97660(16) 0.0263(7) Uani 1 1 d .
C25 C 0.4884(5) 0.28747(18) 0.93252(17) 0.0217(8) Uani 1 1 d .
N10 N 0.3877(4) 0.32551(16) 0.95009(16) 0.0289(8) Uani 1 1 d .
C26 C 0.8386(5) 0.22312(18) 0.98011(18) 0.0213(8) Uani 1 1 d .
N11 N 0.9134(4) 0.21900(16) 1.02915(16) 0.0263(7) Uani 1 1 d .
C27 C 0.8196(5) 0.29433(19) 0.85621(18) 0.0238(8) Uani 1 1 d .
N12 N 0.8967(5) 0.33572(17) 0.83381(17) 0.0344(9) Uani 1 1 d .
O1 O 0.9806(4) 0.46575(15) 0.86505(16) 0.0383(8) Uani 1 1 d D
O2 O 0.3080(4) 0.45507(15) 0.94098(16) 0.0372(7) Uani 1 1 d D
O3 O 0.9742(11) 0.0335(4) 0.7158(4) 0.058(2) Uani 0.50 1 d PD
O4 O 0.8368(5) 0.01372(18) 0.57500(19) 0.0499(9) Uani 1 1 d D
H1A H 0.889(5) 0.480(2) 0.883(2) 0.048 Uiso 1 1 d D
H1B H 0.951(7) 0.4297(12) 0.856(2) 0.048 Uiso 1 1 d D
H2C H 0.330(7) 0.4170(10) 0.942(2) 0.050 Uiso 1 1 d D
H2D H 0.213(4) 0.459(2) 0.919(2) 0.050 Uiso 1 1 d D
H4C H 0.939(4) -0.003(2) 0.569(3) 0.054 Uiso 1 1 d D
H4D H 0.823(7) 0.030(2) 0.5402(14) 0.054 Uiso 1 1 d D
H3C H 0.868(9) 0.019(6) 0.722(7) 0.087 Uiso 0.50 1 d PD
H3D H 0.937(18) 0.063(4) 0.738(6) 0.087 Uiso 0.50 1 d PD
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'
Cr Cr 0.3209 0.6236 '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
N2 C1 N1 121.8(3) .
N2 C1 C5 119.3(3) .
N1 C1 C5 118.9(3) .
C1 N1 C2 121.8(3) .
C1 N1 H1 119.1 .
C2 N1 H1 119.1 .
N1 C2 C3 110.6(3) .
N1 C2 H2A 109.5 .
C3 C2 H2A 109.5 .
N1 C2 H2B 109.5 .
C3 C2 H2B 109.5 .
H2A C2 H2B 108.1 .
C2 C3 C4 112.2(4) .
C2 C3 H3A 109.2 .
C4 C3 H3A 109.2 .
C2 C3 H3B 109.2 .
C4 C3 H3B 109.2 .
H3A C3 H3B 107.9 .
N2 C4 C3 110.0(3) .
N2 C4 H4A 109.7 .
C3 C4 H4A 109.7 .
N2 C4 H4B 109.7 .
C3 C4 H4B 109.7 .
H4A C4 H4B 108.2 .
C1 N2 C4 123.0(3) .
C1 N2 H2 118.5 .
C4 N2 H2 118.5 .
C10 C5 C6 120.3(3) .
C10 C5 C1 119.5(3) .
C6 C5 C1 120.1(3) .
C7 C6 C5 120.1(3) .
C7 C6 H6 119.9 .
C5 C6 H6 119.9 .
C6 C7 C8 119.6(3) .
C6 C7 H7 120.2 .
C8 C7 H7 120.2 .
C9 C8 C7 120.4(3) .
C9 C8 C11 118.9(3) .
C7 C8 C11 120.7(3) .
C10 C9 C8 120.0(3) .
C10 C9 H9 120.0 .
C8 C9 H9 120.0 .
C5 C10 C9 119.6(3) .
C5 C10 H10 120.2 .
C9 C10 H10 120.2 .
N3 C11 N4 121.6(3) .
N3 C11 C8 119.7(3) .
N4 C11 C8 118.7(3) .
C11 N3 C12 123.2(3) .
C11 N3 H3 118.4 .
C12 N3 H3 118.4 .
N3 C12 C13 110.3(3) .
N3 C12 H12A 109.6 .
C13 C12 H12A 109.6 .
N3 C12 H12B 109.6 .
C13 C12 H12B 109.6 .
H12A C12 H12B 108.1 .
C12 C13 C14 110.3(3) .
C12 C13 H13A 109.6 .
C14 C13 H13A 109.6 .
C12 C13 H13B 109.6 .
C14 C13 H13B 109.6 .
H13A C13 H13B 108.1 .
N4 C14 C13 108.5(3) .
N4 C14 H14A 110.0 .
C13 C14 H14A 110.0 .
N4 C14 H14B 110.0 .
C13 C14 H14B 110.0 .
H14A C14 H14B 108.4 .
C11 N4 C14 122.1(3) .
C11 N4 H4 118.9 .
C14 N4 H4 118.9 .
N6 C15 N5 121.6(3) .
N6 C15 C19 119.4(3) .
N5 C15 C19 118.9(3) .
C15 N5 C16 122.3(3) .
C15 N5 H5 118.9 .
C16 N5 H5 118.9 .
N5 C16 C17 109.8(3) .
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 .
C16 C17 C18 110.4(4) .
C16 C17 H17A 109.6 .
C18 C17 H17A 109.6 .
C16 C17 H17B 109.6 .
C18 C17 H17B 109.6 .
H17A C17 H17B 108.1 .
N6 C18 C17 110.0(3) .
N6 C18 H18A 109.7 .
C17 C18 H18A 109.7 .
N6 C18 H18B 109.7 .
C17 C18 H18B 109.7 .
H18A C18 H18B 108.2 .
C15 N6 C18 123.0(3) .
C15 N6 H6A 118.5 .
C18 N6 H6A 118.5 .
C21 C19 C20 120.2(3) .
C21 C19 C15 120.0(3) .
C20 C19 C15 119.8(3) .
C21 C20 C19 120.3(3) 3_557
C21 C20 H20 119.9 3_557
C19 C20 H20 119.9 .
C20 C21 C19 119.5(3) 3_557
C20 C21 H21 120.2 3_557
C19 C21 H21 120.2 .
C23 Cr1 C24 93.81(14) .
C23 Cr1 C25 89.62(14) .
C24 Cr1 C25 90.85(14) .
C23 Cr1 C26 176.37(15) .
C24 Cr1 C26 82.99(14) .
C25 Cr1 C26 92.13(14) .
C23 Cr1 C22 86.62(14) .
C24 Cr1 C22 89.22(14) .
C25 Cr1 C22 176.24(14) .
C26 Cr1 C22 91.61(14) .
C23 Cr1 C27 90.62(14) .
C24 Cr1 C27 175.40(15) .
C25 Cr1 C27 87.95(14) .
C26 Cr1 C27 92.62(15) .
C22 Cr1 C27 92.27(15) .
N7 C22 Cr1 176.9(3) .
N8 C23 Cr1 174.2(3) .
N9 C24 Cr1 170.8(3) .
N10 C25 Cr1 177.4(3) .
N11 C26 Cr1 171.0(3) .
N12 C27 Cr1 178.0(3) .
H1A O1 H1B 105(5) .
H2C O2 H2D 105(5) .
H3C O3 H3D 84(10) .
H4C O4 H4D 98(5) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.310(5) .
C1 N1 1.317(4) .
C1 C5 1.484(5) .
N1 C2 1.467(5) .
N1 H1 0.8800 .
C2 C3 1.470(6) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.502(6) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 N2 1.466(5) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
N2 H2 0.8800 .
C5 C10 1.391(5) .
C5 C6 1.400(5) .
C6 C7 1.387(5) .
C6 H6 0.9500 .
C7 C8 1.398(5) .
C7 H7 0.9500 .
C8 C9 1.395(5) .
C8 C11 1.484(5) .
C9 C10 1.394(5) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C11 N3 1.317(5) .
C11 N4 1.318(4) .
N3 C12 1.471(5) .
N3 H3 0.8800 .
C12 C13 1.513(5) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C14 1.518(5) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 N4 1.474(4) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
N4 H4 0.8800 .
C15 N6 1.309(5) .
C15 N5 1.311(4) .
C15 C19 1.485(4) .
N5 C16 1.468(4) .
N5 H5 0.8800 .
C16 C17 1.495(6) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.512(6) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 N6 1.461(4) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
N6 H6A 0.8800 .
C19 C21 1.391(5) .
C19 C20 1.393(5) .
C20 C21 1.390(5) 3_557
C20 H20 0.9500 .
C21 C20 1.390(5) 3_557
C21 H21 0.9500 .
Cr1 C23 2.068(4) .
Cr1 C24 2.072(4) .
Cr1 C25 2.078(4) .
Cr1 C26 2.078(4) .
Cr1 C22 2.079(4) .
Cr1 C27 2.084(4) .
C22 N7 1.147(5) .
C23 N8 1.159(5) .
C24 N9 1.156(5) .
C25 N10 1.153(5) .
C26 N11 1.146(5) .
C27 N12 1.150(5) .
O1 H1A 0.828(19) .
O1 H1B 0.821(19) .
O2 H2C 0.831(19) .
O2 H2D 0.814(19) .
O3 H3C 0.83(2) .
O3 H3D 0.83(2) .
O4 H4C 0.825(19) .
O4 H4D 0.813(19) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139117532
