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#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/17/4111700.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_4111700
loop_
_publ_author_name
'Gregory J. Halder'
'Cameron J. Kepert'
_publ_contact_author
;
 Cameron J. Kepert
 School of Chemistry, F11
 University of Sydney
 NSW 2006
 Australia
;
_publ_contact_author_email       c.kepert@chem.usyd.edu.au
_publ_contact_author_fax         +61-2-9351-3329
_publ_contact_author_phone       +61-2-9351-5741
_publ_section_title
;
 In Situ Single-Crystal X-ray Diffraction Studies of Desorption and
 Sorption in a Flexible Nanoporous Molecular Framework Material
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7891
_journal_page_last               7900
_journal_paper_doi               10.1021/ja042420k
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C15 H12 Co N5 O6, C3 H6 O'
_chemical_formula_sum            'C18 H18 Co N5 O7'
_chemical_formula_weight         475.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      68
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.699(13)
_cell_length_b                   19.21(2)
_cell_length_c                   17.76(2)
_cell_measurement_reflns_used    894
_cell_measurement_temperature    320(2)
_cell_measurement_theta_max      27.936
_cell_measurement_theta_min      3.233
_cell_volume                     4333(8)
_computing_cell_refinement       'SMART (BrukerAXS, 1997)'
_computing_data_collection       'SMART (BrukerAXS, 1997)'
_computing_data_reduction        'SAINT+ (BrukerAXS, 1997)'
_computing_molecular_graphics    'XPMA/ZORTEP, WebLab Viewer 3.7'
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      320(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       ω
_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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12987
_diffrn_reflns_theta_full        27.74
_diffrn_reflns_theta_max         27.74
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Bruker 1995'
_exptl_crystal_colour            purple-red
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0683
_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)+(0.0738P)²+13.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1709
_refine_ls_wR_factor_ref         0.1945
_reflns_number_gt                1651
_reflns_number_total             2350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja042420ksi20041217_015028.cif
_cod_data_source_block           1.(ACN)
_cod_original_cell_volume        4333(9)
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c a'
_cod_database_code               4111700
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1, -y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-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
Co1 Co 0.0000 0.2500 0.07478(4) 0.0489(3) Uani 1 2 d S
N1 N 0.0916(3) 0.15464(19) 0.07782(19) 0.0551(10) Uani 1 1 d .
C1 C 0.1462(4) 0.1364(2) 0.1400(2) 0.0559(12) Uani 1 1 d .
H1 H 0.1417 0.1648 0.1823 0.067 Uiso 1 1 calc R
C2 C 0.2091(3) 0.0771(2) 0.1439(2) 0.0540(11) Uani 1 1 d .
H2 H 0.2468 0.0676 0.1876 0.065 Uiso 1 1 calc R
C3 C 0.2158(3) 0.0318(2) 0.0824(2) 0.0515(11) Uani 1 1 d .
C4 C 0.1563(5) 0.0497(3) 0.0189(3) 0.0784(18) Uani 1 1 d .
H4 H 0.1574 0.0211 -0.0234 0.094 Uiso 1 1 calc R
C5 C 0.0957(5) 0.1098(3) 0.0187(3) 0.0779(18) Uani 1 1 d .
H5 H 0.0559 0.1199 -0.0239 0.094 Uiso 1 1 calc R
N2 N 0.0000 0.2500 -0.0475(3) 0.0507(12) Uani 1 2 d S
C6 C 0.0888(4) 0.2625(3) -0.0870(2) 0.0636(13) Uani 1 1 d .
H6 H 0.1509 0.2711 -0.0608 0.076 Uiso 1 1 calc R
C7 C 0.0914(4) 0.2631(3) -0.1662(2) 0.0641(13) Uani 1 1 d .
H7 H 0.1545 0.2723 -0.1909 0.077 Uiso 1 1 calc R
C8 C 0.0000 0.2500 -0.2088(3) 0.0434(12) Uani 1 2 d S
O1 O -0.1506(4) 0.1818(3) 0.0642(2) 0.1079(17) Uani 1 1 d .
O2 O -0.0910(4) 0.2028(2) 0.1726(2) 0.0880(12) Uani 1 1 d .
O3 O -0.2265(4) 0.1352(3) 0.1620(3) 0.127(2) Uani 1 1 d .
N4 N -0.1581(4) 0.1700(3) 0.1326(3) 0.0820(14) Uani 1 1 d .
O11 O 0.0358(11) 0.4184(9) -0.1788(8) 0.159(5) Uiso 0.50 1 d P
C12 C -0.0030(14) 0.4587(7) -0.2249(7) 0.088(4) Uiso 0.50 1 d P
C11 C -0.0744(12) 0.5126(8) -0.1920(8) 0.101(4) Uiso 0.50 1 d P
H11A H -0.0959 0.4983 -0.1425 0.152 Uiso 0.50 1 calc PR
H11B H -0.1354 0.5177 -0.2234 0.152 Uiso 0.50 1 calc PR
H11C H -0.0378 0.5562 -0.1889 0.152 Uiso 0.50 1 calc PR
C13 C 0.0370(17) 0.4656(12) -0.3040(12) 0.132(7) Uiso 0.50 1 d P
H13A H 0.0803 0.4262 -0.3161 0.197 Uiso 0.50 1 calc PR
H13B H 0.0778 0.5074 -0.3084 0.197 Uiso 0.50 1 calc PR
H13C H -0.0215 0.4675 -0.3382 0.197 Uiso 0.50 1 calc PR
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'
Co Co 0.3494 0.9721 '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 Co1 N1 91.42(9) . 6_455
N2 Co1 N1 91.42(9) . .
N1 Co1 N1 177.15(18) 6_455 .
N2 Co1 O2 139.78(13) . 6_455
N1 Co1 O2 85.24(16) 6_455 6_455
N1 Co1 O2 92.58(15) . 6_455
N2 Co1 O2 139.78(13) . .
N1 Co1 O2 92.58(15) 6_455 .
N1 Co1 O2 85.24(16) . .
O2 Co1 O2 80.4(3) 6_455 .
N2 Co1 O1 85.35(10) . .
N1 Co1 O1 92.11(19) 6_455 .
N1 Co1 O1 88.12(19) . .
O2 Co1 O1 134.76(17) 6_455 .
O2 Co1 O1 54.52(16) . .
N2 Co1 O1 85.35(10) . 6_455
N1 Co1 O1 88.12(19) 6_455 6_455
N1 Co1 O1 92.11(19) . 6_455
O2 Co1 O1 54.52(16) 6_455 6_455
O2 Co1 O1 134.76(17) . 6_455
O1 Co1 O1 170.7(2) . 6_455
C1 N1 C5 116.6(4) . .
C1 N1 Co1 121.0(3) . .
C5 N1 Co1 122.4(3) . .
N1 C1 C2 123.1(4) . .
N1 C1 H1 118.4 . .
C2 C1 H1 118.4 . .
C1 C2 C3 120.4(4) . .
C1 C2 H2 119.8 . .
C3 C2 H2 119.8 . .
C2 C3 C4 116.2(4) . .
C2 C3 C3 122.9(3) . 2
C4 C3 C3 120.9(3) . 2
C5 C4 C3 120.3(4) . .
C5 C4 H4 119.8 . .
C3 C4 H4 119.8 . .
N1 C5 C4 123.2(4) . .
N1 C5 H5 118.4 . .
C4 C5 H5 118.4 . .
C6 N2 C6 117.3(5) 6_455 .
C6 N2 Co1 121.4(3) 6_455 .
C6 N2 Co1 121.4(3) . .
N2 C6 C7 122.8(4) . .
N2 C6 H6 118.6 . .
C7 C6 H6 118.6 . .
C6 C7 C8 121.0(4) . .
C6 C7 H7 119.5 . .
C8 C7 H7 119.5 . .
C7 C8 C7 115.1(5) . 6_455
C7 C8 C8 122.4(3) . 3_554
C7 C8 C8 122.4(3) 6_455 3_554
N4 O1 Co1 95.0(4) . .
N4 O2 Co1 96.4(3) . .
O3 N4 O1 125.2(6) . .
O3 N4 O2 120.8(5) . .
O1 N4 O2 113.8(5) . .
O11 C12 C11 114.7(14) . .
O11 C12 C13 123.0(17) . .
C11 C12 C13 120.7(15) . .
C12 C11 H11A 109.5 . .
C12 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C12 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N2 2.171(6) .
Co1 N1 2.171(4) 6_455
Co1 N1 2.171(4) .
Co1 O2 2.275(5) 6_455
Co1 O2 2.275(5) .
Co1 O1 2.325(6) .
Co1 O1 2.325(6) 6_455
N1 C1 1.350(5) .
N1 C5 1.358(6) .
C1 C2 1.393(6) .
C1 H1 0.9300 .
C2 C3 1.399(6) .
C2 H2 0.9300 .
C3 C4 1.401(6) .
C3 C3 1.497(8) 2
C4 C5 1.389(6) .
C4 H4 0.9300 .
C5 H5 0.9300 .
N2 C6 1.350(6) 6_455
N2 C6 1.350(6) .
C6 C7 1.407(6) .
C6 H6 0.9300 .
C7 C8 1.407(6) .
C7 H7 0.9300 .
C8 C7 1.407(6) 6_455
C8 C8 1.465(11) 3_554
O1 N4 1.240(6) .
O2 N4 1.276(6) .
O3 N4 1.214(6) .
O11 C12 1.229(19) .
C12 C11 1.50(2) .
C12 C13 1.50(3) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C1 N1 N1 C1 -39.7(7) 6_455 6_455
C2 C3 C3 C2 43.5(11) 2 2
C7 C8 C8 C7 24.4(6) 3_554 8_454
