#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:04:36 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178834 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/88/4108836.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_4108836
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         '1.5(C14 H20 N4 O2), C6 Cr N6'
_chemical_formula_sum            'C27 H30 Cr N12 O3'
_chemical_formula_weight         622.63
_chemical_name_systematic
;
 ?
;
_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                 93.909(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2526(9)
_cell_length_b                   19.894(3)
_cell_length_c                   20.773(3)
_cell_measurement_reflns_used    760
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.00
_cell_volume                     2990.2(7)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1707
_diffrn_reflns_av_sigmaI/netI    0.3620
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18562
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.9661
_exptl_absorpt_correction_T_min  0.9418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.2541
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0383P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.2139
_reflns_number_gt                1997
_reflns_number_total             6852
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja806916t_si_006.cif
_cod_data_source_block           e937a
_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               4108836
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7547(10) 0.1620(4) 0.2268(4) 0.0161(19) Uani 1 1 d . . .
N1 N 0.7429(8) 0.1303(3) 0.2827(3) 0.0170(16) Uani 1 1 d . . .
H1 H 0.6380 0.1324 0.3015 0.020 Uiso 1 1 calc R . .
C2 C 0.8966(10) 0.0918(4) 0.3146(4) 0.021(2) Uani 1 1 d . . .
H2A H 0.8472 0.0528 0.3375 0.026 Uiso 1 1 calc R . .
H2B H 0.9657 0.1206 0.3468 0.026 Uiso 1 1 calc R . .
C3 C 1.0246(10) 0.0677(4) 0.2652(4) 0.019(2) Uani 1 1 d . . .
H3 H 1.1432 0.0526 0.2881 0.023 Uiso 1 1 calc R . .
O1 O 0.9396(7) 0.0115(3) 0.2323(3) 0.0319(16) Uani 1 1 d . . .
H1A H 1.0169 -0.0076 0.2102 0.048 Uiso 1 1 calc R . .
C4 C 1.0661(9) 0.1218(4) 0.2179(4) 0.023(2) Uani 1 1 d . . .
H4A H 1.1514 0.1550 0.2395 0.027 Uiso 1 1 calc R . .
H4B H 1.1291 0.1017 0.1818 0.027 Uiso 1 1 calc R . .
N2 N 0.8980(8) 0.1566(3) 0.1922(3) 0.0194(17) Uani 1 1 d . . .
H2 H 0.8938 0.1739 0.1531 0.023 Uiso 1 1 calc R . .
C5 C 0.5963(9) 0.2058(4) 0.2024(3) 0.0148(18) Uani 1 1 d . . .
C6 C 0.5283(9) 0.2048(4) 0.1385(3) 0.0171(19) Uani 1 1 d . . .
H6 H 0.5797 0.1748 0.1090 0.021 Uiso 1 1 calc R . .
C7 C 0.3849(9) 0.2476(4) 0.1172(3) 0.017 Uani 1 1 d . . .
H7 H 0.3388 0.2467 0.0733 0.020 Uiso 1 1 calc R . .
C8 C 0.3092(9) 0.2917(4) 0.1601(3) 0.0156(19) Uani 1 1 d . . .
C9 C 0.3782(9) 0.2943(4) 0.2248(4) 0.0182(19) Uani 1 1 d . . .
H9 H 0.3284 0.3253 0.2538 0.022 Uiso 1 1 calc R . .
C10 C 0.5202(9) 0.2511(4) 0.2461(3) 0.0218(19) Uani 1 1 d . . .
H10 H 0.5662 0.2519 0.2900 0.026 Uiso 1 1 calc R . .
C11 C 0.1548(10) 0.3379(4) 0.1377(4) 0.018(2) Uani 1 1 d . . .
N3 N 0.1678(8) 0.3733(3) 0.0860(3) 0.0191(17) Uani 1 1 d . . .
H3A H 0.2693 0.3698 0.0653 0.023 Uiso 1 1 calc R . .
C12 C 0.0219(10) 0.4188(4) 0.0600(3) 0.024(2) Uani 1 1 d . . .
H12A H -0.0554 0.3956 0.0258 0.029 Uiso 1 1 calc R . .
H12B H 0.0784 0.4586 0.0407 0.029 Uiso 1 1 calc R . .
C13 C -0.0976(11) 0.4411(4) 0.1130(4) 0.025(2) Uani 1 1 d . . .
H13 H -0.2085 0.4658 0.0940 0.030 Uiso 1 1 calc R . .
O2 O 0.0021(7) 0.4823(3) 0.1599(2) 0.0277(15) Uani 1 1 d . . .
H2C H 0.0469 0.5155 0.1415 0.042 Uiso 1 1 calc R . .
C14 C -0.1569(10) 0.3805(4) 0.1488(4) 0.021(2) Uani 1 1 d . . .
H14A H -0.2283 0.3946 0.1855 0.025 Uiso 1 1 calc R . .
H14B H -0.2374 0.3519 0.1198 0.025 Uiso 1 1 calc R . .
N4 N 0.0087(8) 0.3419(3) 0.1731(3) 0.0206(17) Uani 1 1 d . . .
H4 H 0.0103 0.3216 0.2108 0.025 Uiso 1 1 calc R . .
C15 C 0.7037(10) 0.9850(4) 0.0825(4) 0.0177(19) Uani 1 1 d . . .
N5 N 0.7167(8) 0.9366(3) 0.1247(3) 0.0175(16) Uani 1 1 d . A .
H5 H 0.8123 0.9094 0.1245 0.021 Uiso 1 1 calc R . .
C16 C 0.5795(11) 0.9248(5) 0.1731(4) 0.0370(12) Uani 1 1 d . . .
C17 C 0.407(4) 0.9591(16) 0.1551(14) 0.0370(12) Uani 0.37(2) 1 d P A 1
C17A C 0.479(2) 0.9885(9) 0.1811(8) 0.0370(12) Uani 0.63(2) 1 d P A 2
O3 O 0.3148(7) 0.9696(3) 0.2180(3) 0.0370(12) Uani 1 1 d . . .
C18 C 0.4123(11) 1.0239(5) 0.1245(4) 0.0370(12) Uani 1 1 d . . .
N6 N 0.5628(8) 1.0263(3) 0.0796(3) 0.0266(18) Uani 1 1 d . A .
H6A H 0.5570 1.0573 0.0493 0.032 Uiso 1 1 calc R . .
C19 C 0.8537(10) 0.9921(4) 0.0386(3) 0.0142(19) Uani 1 1 d . . .
C20 C 0.9211(10) 0.9383(4) 0.0076(3) 0.020(2) Uani 1 1 d . . .
H20 H 0.8664 0.8953 0.0121 0.024 Uiso 1 1 calc R . .
C21 C 0.9303(10) 1.0542(4) 0.0305(3) 0.0177(19) Uani 1 1 d . . .
H21 H 0.8817 1.0922 0.0512 0.021 Uiso 1 1 calc R . .
Cr1 Cr 0.28356(17) 0.74224(6) 0.06625(6) 0.0163(3) Uani 1 1 d . . .
C22 C 0.1285(9) 0.7542(4) -0.0209(3) 0.020(2) Uani 1 1 d . . .
N7 N 0.0602(8) 0.7709(3) -0.0698(3) 0.0246(18) Uani 1 1 d . . .
C23 C 0.4498(11) 0.6700(4) 0.0226(4) 0.021(2) Uani 1 1 d . . .
N8 N 0.5305(10) 0.6318(4) -0.0053(3) 0.040(2) Uani 1 1 d . . .
C24 C 0.1323(10) 0.6615(5) 0.1016(3) 0.023(2) Uani 1 1 d . . .
N9 N 0.0570(9) 0.6166(4) 0.1234(3) 0.0278(19) Uani 1 1 d . . .
C25 C 0.4399(9) 0.7499(4) 0.1526(4) 0.0185(19) Uani 1 1 d . . .
N10 N 0.5136(8) 0.7635(4) 0.2028(3) 0.0242(18) Uani 1 1 d . . .
C26 C 0.1153(11) 0.8124(5) 0.1054(4) 0.0253(14) Uani 1 1 d . . .
N11 N 0.0262(9) 0.8516(3) 0.1291(3) 0.0253(14) Uani 1 1 d . . .
C27 C 0.4347(10) 0.8219(4) 0.0308(3) 0.0157(19) Uani 1 1 d . . .
N12 N 0.5021(8) 0.8678(4) 0.0084(3) 0.0258(18) 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'
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
_geom_angle_site_symmetry_3
N2 C1 N1 122.8(7) . .
N2 C1 C5 118.7(7) . .
N1 C1 C5 118.5(7) . .
C1 N1 C2 123.3(6) . .
C1 N1 H1 118.4 . .
C2 N1 H1 118.4 . .
N1 C2 C3 109.9(6) . .
N1 C2 H2A 109.7 . .
C3 C2 H2A 109.7 . .
N1 C2 H2B 109.7 . .
C3 C2 H2B 109.7 . .
H2A C2 H2B 108.2 . .
O1 C3 C4 110.4(6) . .
O1 C3 C2 108.0(6) . .
C4 C3 C2 112.1(6) . .
O1 C3 H3 108.8 . .
C4 C3 H3 108.8 . .
C2 C3 H3 108.8 . .
C3 O1 H1A 109.5 . .
N2 C4 C3 112.1(6) . .
N2 C4 H4A 109.2 . .
C3 C4 H4A 109.2 . .
N2 C4 H4B 109.2 . .
C3 C4 H4B 109.2 . .
H4A C4 H4B 107.9 . .
C1 N2 C4 120.6(6) . .
C1 N2 H2 119.7 . .
C4 N2 H2 119.7 . .
C6 C5 C10 119.7(7) . .
C6 C5 C1 121.9(7) . .
C10 C5 C1 118.3(6) . .
C5 C6 C7 120.3(7) . .
C5 C6 H6 119.8 . .
C7 C6 H6 119.8 . .
C8 C7 C6 120.1(7) . .
C8 C7 H7 120.0 . .
C6 C7 H7 120.0 . .
C7 C8 C9 120.5(7) . .
C7 C8 C11 120.5(7) . .
C9 C8 C11 119.0(7) . .
C10 C9 C8 119.3(7) . .
C10 C9 H9 120.3 . .
C8 C9 H9 120.3 . .
C9 C10 C5 120.1(7) . .
C9 C10 H10 120.0 . .
C5 C10 H10 120.0 . .
N3 C11 N4 122.2(7) . .
N3 C11 C8 119.8(7) . .
N4 C11 C8 118.0(7) . .
C11 N3 C12 123.3(6) . .
C11 N3 H3A 118.3 . .
C12 N3 H3A 118.3 . .
N3 C12 C13 110.4(6) . .
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 . .
O2 C13 C14 105.8(6) . .
O2 C13 C12 112.0(6) . .
C14 C13 C12 108.9(7) . .
O2 C13 H13 110.0 . .
C14 C13 H13 110.0 . .
C12 C13 H13 110.0 . .
C13 O2 H2C 109.5 . .
N4 C14 C13 109.4(6) . .
N4 C14 H14A 109.8 . .
C13 C14 H14A 109.8 . .
N4 C14 H14B 109.8 . .
C13 C14 H14B 109.8 . .
H14A C14 H14B 108.2 . .
C11 N4 C14 119.9(7) . .
C11 N4 H4 120.0 . .
C14 N4 H4 120.0 . .
N5 C15 N6 121.1(7) . .
N5 C15 C19 117.8(7) . .
N6 C15 C19 121.1(7) . .
C15 N5 C16 123.6(7) . .
C15 N5 H5 118.2 . .
C16 N5 H5 118.2 . .
C17A C16 N5 107.5(8) . .
C17A C16 C17 37.0(12) . .
N5 C16 C17 111.1(11) . .
C18 C17 C16 119(2) . .
C18 C17 O3 106.5(19) . .
C16 C17 O3 105.3(18) . .
C18 C17A C16 118.2(13) . .
C18 C17A O3 108.0(12) . .
C16 C17A O3 104.9(11) . .
C17A O3 C17 35.8(11) . .
C17 C18 C17A 37.9(12) . .
C17 C18 N6 110.6(11) . .
C17A C18 N6 108.2(8) . .
C15 N6 C18 123.8(7) . .
C15 N6 H6A 118.1 . .
C18 N6 H6A 118.1 . .
C20 C19 C21 119.5(7) . .
C20 C19 C15 121.5(8) . .
C21 C19 C15 119.0(8) . .
C19 C20 C21 120.3(8) . 3_775
C19 C20 H20 119.9 . .
C21 C20 H20 119.9 3_775 .
C19 C21 C20 120.3(7) . 3_775
C19 C21 H21 119.9 . .
C20 C21 H21 119.9 3_775 .
C25 Cr1 C26 84.9(3) . .
C25 Cr1 C22 169.2(3) . .
C26 Cr1 C22 88.1(3) . .
C25 Cr1 C27 88.8(3) . .
C26 Cr1 C27 88.0(3) . .
C22 Cr1 C27 82.7(3) . .
C25 Cr1 C24 91.3(3) . .
C26 Cr1 C24 92.4(3) . .
C22 Cr1 C24 97.3(3) . .
C27 Cr1 C24 179.6(3) . .
C25 Cr1 C23 97.3(3) . .
C26 Cr1 C23 177.8(3) . .
C22 Cr1 C23 89.7(3) . .
C27 Cr1 C23 92.1(3) . .
C24 Cr1 C23 87.5(3) . .
N7 C22 Cr1 168.1(7) . .
N8 C23 Cr1 174.5(8) . .
N9 C24 Cr1 176.4(7) . .
N10 C25 Cr1 169.5(7) . .
N11 C26 Cr1 177.5(7) . .
N12 C27 Cr1 173.3(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.308(8) .
C1 N1 1.329(8) .
C1 C5 1.503(10) .
N1 C2 1.473(8) .
N1 H1 0.8800 .
C2 C3 1.508(9) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 O1 1.428(8) .
C3 C4 1.502(10) .
C3 H3 1.0000 .
O1 H1A 0.8400 .
C4 N2 1.471(8) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
N2 H2 0.8800 .
C5 C6 1.385(9) .
C5 C10 1.417(9) .
C6 C7 1.393(9) .
C6 H6 0.9500 .
C7 C8 1.390(9) .
C7 H7 0.9500 .
C8 C9 1.404(9) .
C8 C11 1.498(10) .
C9 C10 1.391(10) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C11 N3 1.291(9) .
C11 N4 1.333(8) .
N3 C12 1.468(9) .
N3 H3A 0.8800 .
C12 C13 1.513(9) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 O2 1.432(8) .
C13 C14 1.495(10) .
C13 H13 1.0000 .
O2 H2C 0.8400 .
C14 N4 1.484(9) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
N4 H4 0.8800 .
C15 N5 1.300(9) .
C15 N6 1.311(9) .
C15 C19 1.474(9) .
N5 C16 1.480(9) .
N5 H5 0.8800 .
C16 C17A 1.477(17) .
C16 C17 1.45(3) .
C17 C18 1.44(3) .
C17 O3 1.52(2) .
C17A C18 1.426(17) .
C17A O3 1.505(14) .
C18 N6 1.483(9) .
N6 H6A 0.8800 .
C19 C20 1.356(10) .
C19 C21 1.369(10) .
C20 C21 1.389(9) 3_775
C20 H20 0.9500 .
C21 C20 1.389(9) 3_775
C21 H21 0.9500 .
Cr1 C25 2.062(8) .
Cr1 C26 2.057(8) .
Cr1 C22 2.080(7) .
Cr1 C27 2.088(8) .
Cr1 C24 2.106(9) .
Cr1 C23 2.118(9) .
C22 N7 1.147(8) .
C23 N8 1.141(9) .
C24 N9 1.154(9) .
C25 N10 1.170(8) .
C26 N11 1.146(9) .
C27 N12 1.151(9) .
