#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:08:22 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178770 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/24/4102400.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_4102400
loop_
_publ_author_name
'Jian-Bin Lin'
'Jie-Peng Zhang'
'Xiao-Ming Chen'
_publ_section_title
;
 Nonclassical Active Site for Enhanced Gas Sorption in Porous Coordination
 Polymer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6654
_journal_page_last               6656
_journal_paper_doi               10.1021/ja1009635
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C24 H16 Co N10'
_chemical_formula_weight         503.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            9
_cell_length_a                   28.222(5)
_cell_length_b                   28.222(5)
_cell_length_c                   9.413(3)
_cell_measurement_reflns_used    3768
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.66
_cell_measurement_theta_min      2.3185
_cell_volume                     6493(3)
_computing_cell_refinement       'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.'
_computing_data_collection       'SMART Bruker AXS Inc., 1998.'
_computing_data_reduction        'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.'
_computing_molecular_graphics    'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex CCd'
_diffrn_measurement_method       'ω scan'
_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  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16372
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.9015
_exptl_absorpt_correction_T_min  0.7888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2313
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0416
_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)+(0.0580P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                1920
_reflns_number_total             2842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1009635_si_002_1.cif
_cod_data_source_block           compound_1
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4102400
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.5000 1.0000 0.04877(18) Uani 1 2 d S
N1 N -0.06879(8) 0.48484(8) 0.8656(2) 0.0576(5) Uani 1 1 d .
N2 N 0.01567(8) 0.47118(8) 0.81846(19) 0.0494(5) Uani 1 1 d .
N3 N 0.05461(8) 0.45986(8) 0.7724(2) 0.0507(5) Uani 1 1 d .
N4 N -0.01175(9) 0.43189(8) 0.6051(2) 0.0596(5) Uani 1 1 d .
N5 N 0.12548(8) 0.37581(8) 0.4193(2) 0.0562(5) Uani 1 1 d .
C1 C -0.10855(13) 0.49622(13) 0.8912(3) 0.0769(8) Uani 1 1 d .
H1A H -0.1090 0.5115 0.9784 0.092 Uiso 1 1 calc R
C2 C -0.14863(14) 0.48634(16) 0.7951(4) 0.0990(11) Uani 1 1 d .
H2A H -0.1756 0.4949 0.8168 0.119 Uiso 1 1 calc R
C3 C -0.14877(15) 0.46374(16) 0.6662(4) 0.1001(11) Uani 1 1 d .
H3A H -0.1760 0.4565 0.5998 0.120 Uiso 1 1 calc R
C4 C -0.10843(13) 0.45199(13) 0.6368(3) 0.0818(9) Uani 1 1 d .
H4A H -0.1076 0.4368 0.5498 0.098 Uiso 1 1 calc R
C5 C -0.06888(10) 0.46299(10) 0.7380(3) 0.0570(6) Uani 1 1 d .
C6 C -0.02246(10) 0.45404(9) 0.7172(3) 0.0515(6) Uani 1 1 d .
C7 C 0.03624(10) 0.43642(9) 0.6461(2) 0.0483(6) Uani 1 1 d .
C8 C 0.06715(9) 0.41681(9) 0.5637(2) 0.0493(6) Uani 1 1 d .
C12 C 0.04748(11) 0.38659(13) 0.4427(3) 0.0748(8) Uani 1 1 d .
H12A H 0.0139 0.3794 0.4061 0.090 Uiso 1 1 calc R
C11 C 0.07680(12) 0.36681(14) 0.3751(3) 0.0795(9) Uani 1 1 d .
H11A H 0.0620 0.3459 0.2936 0.095 Uiso 1 1 calc R
C10 C 0.14465(11) 0.40610(12) 0.5346(3) 0.0700(8) Uani 1 1 d .
H10A H 0.1790 0.4141 0.5670 0.084 Uiso 1 1 calc R
C9 C 0.11713(11) 0.42652(12) 0.6097(3) 0.0694(8) Uani 1 1 d .
H9A H 0.1324 0.4469 0.6917 0.083 Uiso 1 1 calc R
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'
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 N2 180.00(6) . 10_567
N2 Co1 N1 77.50(8) . .
N2 Co1 N1 102.50(8) 10_567 .
N2 Co1 N1 102.50(8) . 10_567
N2 Co1 N1 77.50(8) 10_567 10_567
N1 Co1 N1 180.000(1) . 10_567
N2 Co1 N5 89.45(7) . 8
N2 Co1 N5 90.55(7) 10_567 8
N1 Co1 N5 92.81(8) . 8
N1 Co1 N5 87.19(8) 10_567 8
N2 Co1 N5 90.55(7) . 14_456
N2 Co1 N5 89.45(7) 10_567 14_456
N1 Co1 N5 87.19(8) . 14_456
N1 Co1 N5 92.81(8) 10_567 14_456
N5 Co1 N5 180.0 8 14_456
C1 N1 C5 117.5(2) . .
C1 N1 Co1 128.56(19) . .
C5 N1 Co1 113.92(16) . .
C6 N2 N3 106.69(18) . .
C6 N2 Co1 116.63(15) . .
N3 N2 Co1 136.43(16) . .
C7 N3 N2 103.97(19) . .
C6 N4 C7 100.5(2) . .
C10 N5 C11 115.5(2) . .
C10 N5 Co1 119.92(16) . 6_454
C11 N5 Co1 123.85(16) . 6_454
N1 C1 C2 122.8(3) . .
N1 C1 H1A 118.6 . .
C2 C1 H1A 118.6 . .
C1 C2 C3 119.5(3) . .
C1 C2 H2A 120.3 . .
C3 C2 H2A 120.3 . .
C4 C3 C2 119.0(3) . .
C4 C3 H3A 120.5 . .
C2 C3 H3A 120.5 . .
C3 C4 C5 119.0(3) . .
C3 C4 H4A 120.5 . .
C5 C4 H4A 120.5 . .
N1 C5 C4 122.3(2) . .
N1 C5 C6 113.6(2) . .
C4 C5 C6 124.1(2) . .
N2 C6 N4 113.8(2) . .
N2 C6 C5 118.0(2) . .
N4 C6 C5 128.1(2) . .
N3 C7 N4 115.1(2) . .
N3 C7 C8 120.1(2) . .
N4 C7 C8 124.8(2) . .
C12 C8 C9 116.6(2) . .
C12 C8 C7 123.0(2) . .
C9 C8 C7 120.4(2) . .
C8 C12 C11 120.3(2) . .
C8 C12 H12A 119.8 . .
C11 C12 H12A 119.8 . .
N5 C11 C12 123.7(2) . .
N5 C11 H11A 118.2 . .
C12 C11 H11A 118.2 . .
N5 C10 C9 124.2(2) . .
N5 C10 H10A 117.9 . .
C9 C10 H10A 117.9 . .
C8 C9 C10 119.8(2) . .
C8 C9 H9A 120.1 . .
C10 C9 H9A 120.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N2 2.0339(18) .
Co1 N2 2.0339(18) 10_567
Co1 N1 2.173(2) .
Co1 N1 2.173(2) 10_567
Co1 N5 2.1990(19) 8
Co1 N5 2.1990(19) 14_456
N1 C1 1.335(3) .
N1 C5 1.349(3) .
N2 C6 1.334(3) .
N2 N3 1.360(2) .
N3 C7 1.333(3) .
N4 C6 1.335(3) .
N4 C7 1.351(3) .
N5 C10 1.319(3) .
N5 C11 1.333(3) .
N5 Co1 2.1988(19) 6_454
C1 C2 1.364(4) .
C1 H1A 0.9300 .
C2 C3 1.369(4) .
C2 H2A 0.9300 .
C3 C4 1.364(4) .
C3 H3A 0.9300 .
C4 C5 1.380(4) .
C4 H4A 0.9300 .
C5 C6 1.466(3) .
C7 C8 1.467(3) .
C8 C12 1.363(3) .
C8 C9 1.366(3) .
C12 C11 1.365(3) .
C12 H12A 0.9300 .
C11 H11A 0.9300 .
C10 C9 1.372(3) .
C10 H10A 0.9300 .
C9 H9A 0.9300 .
