#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:04:36 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178834 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/88/4108832.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_4108832
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)'
_chemical_formula_sum            'C54 H60 Cr2 N24'
_chemical_formula_weight         1149.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 106.777(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.2563(3)
_cell_length_b                   20.5934(9)
_cell_length_c                   21.5442(9)
_cell_measurement_reflns_used    1856
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.07
_cell_measurement_theta_min      2.98
_cell_volume                     3082.4(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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0713
_diffrn_reflns_av_sigmaI/netI    0.0949
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24667
_diffrn_reflns_theta_full        29.16
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.9839
_exptl_absorpt_correction_T_min  0.9565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         8424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0576
_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)+(0.0631P)²+0.6646P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1578
_reflns_number_gt                4778
_reflns_number_total             8424
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja806916t_si_002.cif
_cod_data_source_block           e1026a
_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               4108832
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 -0.0396(3) 0.81960(12) 0.70015(13) 0.0220(5) Uani 1 1 d .
N1 N 0.0241(3) 0.84741(10) 0.75673(11) 0.0253(5) Uani 1 1 d .
H1 H 0.1474 0.8441 0.7776 0.030 Uiso 1 1 calc R
C2 C -0.0996(4) 0.88393(14) 0.78721(14) 0.0293(6) Uani 1 1 d .
H2A H -0.0251 0.9196 0.8138 0.035 Uiso 1 1 calc R
H2B H -0.1460 0.8549 0.8161 0.035 Uiso 1 1 calc R
C3 C -0.2702(4) 0.91184(14) 0.73547(16) 0.0347(7) Uani 1 1 d .
H3A H -0.2262 0.9474 0.7122 0.042 Uiso 1 1 calc R
H3B H -0.3646 0.9300 0.7560 0.042 Uiso 1 1 calc R
C4 C -0.3648(4) 0.85892(15) 0.68782(15) 0.0338(7) Uani 1 1 d .
H4A H -0.4287 0.8273 0.7094 0.041 Uiso 1 1 calc R
H4B H -0.4640 0.8783 0.6509 0.041 Uiso 1 1 calc R
N2 N -0.2205(3) 0.82564(11) 0.66408(11) 0.0262(5) Uani 1 1 d .
H2 H -0.2549 0.8091 0.6247 0.031 Uiso 1 1 calc R
C5 C 0.0941(3) 0.78041(12) 0.67426(13) 0.0222(5) Uani 1 1 d .
C6 C 0.2102(3) 0.73362(12) 0.71418(13) 0.0237(5) Uani 1 1 d .
H6 H 0.2048 0.7273 0.7573 0.028 Uiso 1 1 calc R
C7 C 0.3341(4) 0.69638(12) 0.68974(14) 0.0250(6) Uani 1 1 d .
H7 H 0.4132 0.6644 0.7164 0.030 Uiso 1 1 calc R
C8 C 0.3426(4) 0.70568(12) 0.62704(13) 0.0229(5) Uani 1 1 d .
C9 C 0.2260(4) 0.75273(13) 0.58708(14) 0.0245(6) Uani 1 1 d .
H9 H 0.2323 0.7593 0.5441 0.029 Uiso 1 1 calc R
C10 C 0.1015(4) 0.78951(13) 0.61118(13) 0.0238(5) Uani 1 1 d .
H10 H 0.0210 0.8211 0.5843 0.029 Uiso 1 1 calc R
C11 C 0.4752(4) 0.66661(12) 0.60083(13) 0.0246(6) Uani 1 1 d .
N3 N 0.6548(3) 0.65881(11) 0.63669(12) 0.0285(5) Uani 1 1 d .
H3 H 0.6897 0.6742 0.6765 0.034 Uiso 1 1 calc R
C12 C 0.7980(4) 0.62525(16) 0.61241(16) 0.0397(8) Uani 1 1 d .
H12A H 0.8948 0.6042 0.6489 0.048 Uiso 1 1 calc R
H12B H 0.8653 0.6570 0.5922 0.048 Uiso 1 1 calc R
C13 C 0.7006(5) 0.57463(16) 0.56315(17) 0.0433(8) Uani 1 1 d .
H13A H 0.6520 0.5390 0.5850 0.052 Uiso 1 1 calc R
H13B H 0.7945 0.5561 0.5426 0.052 Uiso 1 1 calc R
C14 C 0.5347(4) 0.60512(14) 0.51178(15) 0.0346(7) Uani 1 1 d .
H14A H 0.5850 0.6352 0.4847 0.041 Uiso 1 1 calc R
H14B H 0.4590 0.5709 0.4833 0.041 Uiso 1 1 calc R
N4 N 0.4106(3) 0.64086(11) 0.54326(12) 0.0281(5) Uani 1 1 d .
H4 H 0.2877 0.6450 0.5224 0.034 Uiso 1 1 calc R
C15 C 0.1220(3) 0.50714(12) 0.90974(13) 0.0219(5) Uani 1 1 d .
N5 N -0.0174(3) 0.47203(10) 0.92083(12) 0.0284(5) Uani 1 1 d .
H5 H 0.0100 0.4452 0.9541 0.034 Uiso 1 1 calc R
C16 C -0.2153(4) 0.47637(15) 0.87959(16) 0.0368(8) Uani 1 1 d .
H16A H -0.2857 0.5092 0.8974 0.044 Uiso 1 1 calc R
H16B H -0.2800 0.4340 0.8791 0.044 Uiso 1 1 calc R
C17 C -0.2212(4) 0.49466(15) 0.81217(16) 0.0394(7) Uani 1 1 d .
H17A H -0.3556 0.5042 0.7869 0.047 Uiso 1 1 calc R
H17B H -0.1749 0.4578 0.7912 0.047 Uiso 1 1 calc R
C18 C -0.0971(4) 0.55356(13) 0.81213(14) 0.0321(7) Uani 1 1 d .
H18A H -0.0836 0.5603 0.7682 0.039 Uiso 1 1 calc R
H18B H -0.1591 0.5926 0.8240 0.039 Uiso 1 1 calc R
N6 N 0.0938(3) 0.54450(10) 0.85866(11) 0.0248(5) Uani 1 1 d .
H6A H 0.1929 0.5649 0.8520 0.030 Uiso 1 1 calc R
C19 C 0.3179(3) 0.50347(12) 0.95661(12) 0.0207(5) Uani 1 1 d .
C20 C 0.3984(4) 0.44323(12) 0.97802(13) 0.0228(5) Uani 1 1 d .
H20 H 0.3281 0.4046 0.9630 0.027 Uiso 1 1 calc R
C21 C 0.5816(4) 0.43969(12) 1.02135(13) 0.0225(5) Uani 1 1 d .
H21 H 0.6378 0.3987 1.0358 0.027 Uiso 1 1 calc R
Cr1 Cr 0.71077(6) 0.731577(19) 0.89902(2) 0.02151(12) Uani 1 1 d .
C22 C 0.9133(4) 0.80303(13) 0.93896(14) 0.0278(6) Uani 1 1 d .
N7 N 1.0210(4) 0.84273(12) 0.96256(14) 0.0410(7) Uani 1 1 d .
C23 C 0.8997(4) 0.65898(12) 0.94445(13) 0.0228(5) Uani 1 1 d .
N8 N 0.9911(3) 0.61787(11) 0.97447(12) 0.0280(5) Uani 1 1 d .
C24 C 0.6315(3) 0.72985(12) 0.98435(13) 0.0230(5) Uani 1 1 d .
N9 N 0.6075(3) 0.72375(11) 1.03430(12) 0.0294(5) Uani 1 1 d .
C25 C 0.5085(4) 0.65976(13) 0.85934(13) 0.0260(6) Uani 1 1 d .
N10 N 0.4026(4) 0.61908(12) 0.83686(12) 0.0355(6) Uani 1 1 d .
C26 C 0.5206(4) 0.80530(13) 0.85635(14) 0.0282(6) Uani 1 1 d .
N11 N 0.4201(3) 0.84622(12) 0.83124(14) 0.0379(6) Uani 1 1 d .
C27 C 0.7918(4) 0.72242(12) 0.81440(14) 0.0240(6) Uani 1 1 d .
N12 N 0.8188(3) 0.71226(11) 0.76536(12) 0.0297(5) 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'
Cr Cr 0.3209 0.6236 '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
N1 C1 N2 122.1(2) . .
N1 C1 C5 119.6(2) . .
N2 C1 C5 118.3(2) . .
C1 N1 C2 123.1(2) . .
C1 N1 H1 118.4 . .
C2 N1 H1 118.4 . .
N1 C2 C3 109.9(2) . .
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 . .
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 110.1(2) . .
N2 C4 H4A 109.6 . .
C3 C4 H4A 109.6 . .
N2 C4 H4B 109.6 . .
C3 C4 H4B 109.6 . .
H4A C4 H4B 108.2 . .
C1 N2 C4 121.8(2) . .
C1 N2 H2 119.1 . .
C4 N2 H2 119.1 . .
C10 C5 C6 120.5(2) . .
C10 C5 C1 120.5(2) . .
C6 C5 C1 119.0(2) . .
C7 C6 C5 119.0(3) . .
C7 C6 H6 120.5 . .
C5 C6 H6 120.5 . .
C8 C7 C6 120.5(2) . .
C8 C7 H7 119.7 . .
C6 C7 H7 119.7 . .
C7 C8 C9 120.3(2) . .
C7 C8 C11 120.8(2) . .
C9 C8 C11 118.8(2) . .
C10 C9 C8 119.2(3) . .
C10 C9 H9 120.4 . .
C8 C9 H9 120.4 . .
C5 C10 C9 120.3(2) . .
C5 C10 H10 119.8 . .
C9 C10 H10 119.8 . .
N4 C11 N3 122.0(2) . .
N4 C11 C8 119.2(2) . .
N3 C11 C8 118.8(2) . .
C11 N3 C12 122.1(2) . .
C11 N3 H3 119.0 . .
C12 N3 H3 119.0 . .
N3 C12 C13 109.9(2) . .
N3 C12 H12A 109.7 . .
C13 C12 H12A 109.7 . .
N3 C12 H12B 109.7 . .
C13 C12 H12B 109.7 . .
H12A C12 H12B 108.2 . .
C12 C13 C14 109.8(3) . .
C12 C13 H13A 109.7 . .
C14 C13 H13A 109.7 . .
C12 C13 H13B 109.7 . .
C14 C13 H13B 109.7 . .
H13A C13 H13B 108.2 . .
N4 C14 C13 109.5(2) . .
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 122.8(2) . .
C11 N4 H4 118.6 . .
C14 N4 H4 118.6 . .
N6 C15 N5 122.1(2) . .
N6 C15 C19 119.1(2) . .
N5 C15 C19 118.7(2) . .
C15 N5 C16 121.9(2) . .
C15 N5 H5 119.1 . .
C16 N5 H5 119.1 . .
N5 C16 C17 110.9(2) . .
N5 C16 H16A 109.5 . .
C17 C16 H16A 109.5 . .
N5 C16 H16B 109.5 . .
C17 C16 H16B 109.5 . .
H16A C16 H16B 108.1 . .
C16 C17 C18 110.7(3) . .
C16 C17 H17A 109.5 . .
C18 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
C18 C17 H17B 109.5 . .
H17A C17 H17B 108.1 . .
N6 C18 C17 110.0(2) . .
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 122.4(2) . .
C15 N6 H6A 118.8 . .
C18 N6 H6A 118.8 . .
C21 C19 C20 120.6(2) 3_667 .
C21 C19 C15 119.6(2) 3_667 .
C20 C19 C15 119.8(2) . .
C21 C20 C19 119.9(2) . .
C21 C20 H20 120.1 . .
C19 C20 H20 120.1 . .
C20 C21 C19 119.5(2) . 3_667
C20 C21 H21 120.3 . .
C19 C21 H21 120.3 3_667 .
C23 Cr1 C24 83.34(10) . .
C23 Cr1 C26 178.15(11) . .
C24 Cr1 C26 94.92(11) . .
C23 Cr1 C27 91.88(10) . .
C24 Cr1 C27 173.80(10) . .
C26 Cr1 C27 89.90(11) . .
C23 Cr1 C22 91.31(10) . .
C24 Cr1 C22 89.37(11) . .
C26 Cr1 C22 88.05(10) . .
C27 Cr1 C22 94.69(11) . .
C23 Cr1 C25 88.47(10) . .
C24 Cr1 C25 90.50(11) . .
C26 Cr1 C25 92.16(10) . .
C27 Cr1 C25 85.41(10) . .
C22 Cr1 C25 179.76(12) . .
N7 C22 Cr1 177.5(3) . .
N8 C23 Cr1 171.9(2) . .
N9 C24 Cr1 171.3(2) . .
N10 C25 Cr1 177.4(3) . .
N11 C26 Cr1 177.3(3) . .
N12 C27 Cr1 171.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.305(3) .
C1 N2 1.324(3) .
C1 C5 1.489(3) .
N1 C2 1.464(3) .
N1 H1 0.8800 .
C2 C3 1.519(4) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.519(4) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 N2 1.461(3) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
N2 H2 0.8800 .
C5 C10 1.388(4) .
C5 C6 1.400(3) .
C6 C7 1.395(4) .
C6 H6 0.9500 .
C7 C8 1.383(4) .
C7 H7 0.9500 .
C8 C9 1.405(4) .
C8 C11 1.485(4) .
C9 C10 1.389(4) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C11 N4 1.305(3) .
C11 N3 1.319(3) .
N3 C12 1.465(3) .
N3 H3 0.8800 .
C12 C13 1.510(4) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C14 1.516(4) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 N4 1.471(3) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
N4 H4 0.8800 .
C15 N6 1.310(3) .
C15 N5 1.320(3) .
C15 C19 1.489(3) .
N5 C16 1.457(3) .
N5 H5 0.8800 .
C16 C17 1.489(4) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.511(4) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 N6 1.469(3) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
N6 H6A 0.8800 .
C19 C21 1.388(3) 3_667
C19 C20 1.392(3) .
C20 C21 1.388(4) .
C20 H20 0.9500 .
C21 C19 1.388(3) 3_667
C21 H21 0.9500 .
Cr1 C23 2.073(3) .
Cr1 C24 2.079(3) .
Cr1 C26 2.079(3) .
Cr1 C27 2.079(3) .
Cr1 C22 2.082(3) .
Cr1 C25 2.085(3) .
C22 N7 1.144(3) .
C23 N8 1.152(3) .
C24 N9 1.146(3) .
C25 N10 1.145(3) .
C26 N11 1.143(3) .
C27 N12 1.148(3) .
