#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:49:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179349 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/46/4324619.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_4324619
loop_
_publ_author_name
'Qing Chen'
'Jian-Bin Lin'
'Wei Xue'
'Ming-Hua Zeng'
'Xiao-Ming Chen'
_publ_section_title
;
 A Porous Coordination Polymer Assembled from 8-Connected {CoII3(OH)}
 Clusters and Isonicotinate: Multiple Active Metal Sites, Apical Ligand
 Substitution, H2 Adsorption, and Magnetism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2321
_journal_page_last               2328
_journal_paper_doi               10.1021/ic102015g
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C32 H39 Co3 N4 O12'
_chemical_formula_weight         848.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   18.9705(17)
_cell_length_b                   19.4783(18)
_cell_length_c                   12.0751(11)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     4461.9(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20157
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.156
_exptl_absorpt_correction_T_max  0.7851
_exptl_absorpt_correction_T_min  0.6679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.770
_refine_diff_density_min         -1.837
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4055
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0886
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1324P)²+36.4892P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2401
_refine_ls_wR_factor_ref         0.2417
_reflns_number_gt                3845
_reflns_number_total             4055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102015g_si_001_1.cif
_cod_data_source_block           1-BuOH
_cod_database_code               4324619
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
Co1 Co -0.31279(4) 0.33787(4) 0.14724(6) 0.0198(3) Uani 1 1 d . . .
Co2 Co -0.34452(6) 0.2500 0.40731(9) 0.0200(3) Uani 1 2 d S . .
C3 C -0.2734(3) 0.4567(3) 0.4447(5) 0.0313(14) Uani 1 1 d . . .
C2 C -0.3092(4) 0.4817(4) 0.5348(6) 0.0361(16) Uani 1 1 d . . .
H2A H -0.3512 0.4600 0.5597 0.043 Uiso 1 1 calc R . .
C1 C -0.2831(4) 0.5396(4) 0.5893(6) 0.0353(15) Uani 1 1 d . . .
H1A H -0.3094 0.5579 0.6493 0.042 Uiso 1 1 calc R . .
C5 C -0.1872(4) 0.5444(4) 0.4752(6) 0.0419(18) Uani 1 1 d . . .
H5A H -0.1437 0.5651 0.4553 0.050 Uiso 1 1 calc R . .
C4 C -0.2106(4) 0.4889(4) 0.4139(6) 0.0429(18) Uani 1 1 d . . .
H4A H -0.1845 0.4730 0.3519 0.051 Uiso 1 1 calc R . .
C6 C -0.2997(4) 0.3956(3) 0.3798(5) 0.0325(15) Uani 1 1 d . . .
C9A C -0.1026(4) 0.2500 0.1072(7) 0.0236(17) Uani 1 2 d S . .
C8 C -0.0641(6) 0.3079(7) 0.1294(15) 0.035(3) Uani 0.50 1 d P A 1
H8A H -0.0864 0.3489 0.1534 0.042 Uiso 0.50 1 calc PR A 1
C8' C -0.0682(9) 0.3057(9) 0.0641(16) 0.046(4) Uiso 0.50 1 d P A 2
H8'A H -0.0930 0.3460 0.0431 0.055 Uiso 0.50 1 calc PR A 2
C7 C 0.0088(6) 0.3048(7) 0.1156(16) 0.036(3) Uani 0.50 1 d P A 1
H7A H 0.0351 0.3456 0.1280 0.043 Uiso 0.50 1 calc PR A 1
C7' C 0.0055(9) 0.3010(9) 0.0523(16) 0.045(4) Uiso 0.50 1 d P A 2
H7'A H 0.0292 0.3378 0.0164 0.054 Uiso 0.50 1 calc PR A 2
C10 C -0.1817(5) 0.2500 0.1240(17) 0.074(3) Uani 1 2 d SU . .
C13 C -0.3443(5) 0.2500 -0.1784(7) 0.0263(18) Uani 1 2 d S . .
C12 C -0.3082(8) 0.3009(8) -0.2368(11) 0.042(4) Uani 0.50 1 d P . 1
H12A H -0.2833 0.3358 -0.1983 0.050 Uiso 0.50 1 calc PR . 1
C12' C -0.3801(7) 0.2998(7) -0.2395(10) 0.031(3) Uani 0.50 1 d P . 2
H12B H -0.4058 0.3349 -0.2028 0.037 Uiso 0.50 1 calc PR . 2
C11 C -0.3090(8) 0.2997(8) -0.3524(11) 0.036(3) Uani 0.50 1 d P . 1
H11A H -0.2850 0.3349 -0.3916 0.043 Uiso 0.50 1 calc PR . 1
C11' C -0.3779(8) 0.2975(7) -0.3535(10) 0.032(3) Uani 0.50 1 d P . 2
H11B H -0.4028 0.3317 -0.3936 0.038 Uiso 0.50 1 calc PR . 2
C14 C -0.3436(4) 0.2500 -0.0511(8) 0.0266(18) Uani 1 2 d S . .
C15 C -0.4805(7) 0.3573(11) 0.1332(18) 0.090(3) Uani 0.573(9) 1 d PDU A 1
H15C H -0.5136 0.3926 0.1610 0.109 Uiso 0.573(9) 1 calc PR A 1
H15A H -0.4844 0.3190 0.1868 0.109 Uiso 0.573(9) 1 calc PR A 1
C15' C -0.4292(14) 0.4548(7) 0.199(2) 0.083(3) Uani 0.427(9) 1 d PDU A 2
H15D H -0.4510 0.4802 0.1369 0.100 Uiso 0.427(9) 1 calc PR A 2
H15B H -0.3835 0.4771 0.2149 0.100 Uiso 0.427(9) 1 calc PR A 2
C16 C -0.5198(9) 0.3290(13) 0.0327(18) 0.114(4) Uani 0.573(9) 1 d PDU A 1
H16A H -0.5026 0.3518 -0.0353 0.137 Uiso 0.573(9) 1 calc PR A 1
H16B H -0.5106 0.2791 0.0257 0.137 Uiso 0.573(9) 1 calc PR A 1
C16' C -0.4761(15) 0.4653(11) 0.300(2) 0.099(4) Uani 0.427(9) 1 d PDU A 2
H16C H -0.5216 0.4417 0.2878 0.119 Uiso 0.427(9) 1 calc PR A 2
H16D H -0.4534 0.4434 0.3653 0.119 Uiso 0.427(9) 1 calc PR A 2
C17 C -0.5988(9) 0.3411(15) 0.045(2) 0.126(5) Uani 0.573(9) 1 d PDU A 1
H17A H -0.6199 0.3038 0.0894 0.151 Uiso 0.573(9) 1 calc PR A 1
H17B H -0.6071 0.3851 0.0840 0.151 Uiso 0.573(9) 1 calc PR A 1
C17' C -0.4904(15) 0.5401(13) 0.327(2) 0.107(5) Uani 0.427(9) 1 d PDU A 2
H17C H -0.4459 0.5664 0.3235 0.128 Uiso 0.427(9) 1 calc PR A 2
H17D H -0.5092 0.5439 0.4036 0.128 Uiso 0.427(9) 1 calc PR A 2
C18 C -0.6332(14) 0.3434(16) -0.069(2) 0.141(7) Uani 0.573(9) 1 d PDU A 1
H18A H -0.6838 0.3521 -0.0604 0.212 Uiso 0.573(9) 1 calc PR A 1
H18B H -0.6261 0.2994 -0.1064 0.212 Uiso 0.573(9) 1 calc PR A 1
H18C H -0.6119 0.3803 -0.1127 0.212 Uiso 0.573(9) 1 calc PR A 1
C18' C -0.5435(17) 0.5699(16) 0.246(3) 0.124(7) Uani 0.427(9) 1 d PDU A 2
H18D H -0.5523 0.6182 0.2636 0.186 Uiso 0.427(9) 1 calc PR A 2
H18E H -0.5878 0.5441 0.2503 0.186 Uiso 0.427(9) 1 calc PR A 2
H18F H -0.5246 0.5664 0.1702 0.186 Uiso 0.427(9) 1 calc PR A 2
N1 N -0.2228(3) 0.5703(3) 0.5610(4) 0.0301(12) Uani 1 1 d . . .
N2 N 0.0430(4) 0.2500 0.0871(6) 0.0240(15) Uani 1 2 d S . .
O1 O -0.3477(3) 0.2500 0.2320(4) 0.0186(11) Uani 1 2 d S . .
H1B H -0.3900 0.2424 0.2125 0.022 Uiso 0.50 1 d PR . .
O1W O -0.2320(4) 0.2500 0.3950(6) 0.064(3) Uani 1 2 d S . .
H1WA H -0.2198 0.2500 0.3272 0.096 Uiso 1 2 d SR . .
H1WC H -0.2156 0.2144 0.4265 0.096 Uiso 0.50 1 d PR . .
O2 O -0.3428(2) 0.3562(2) 0.4273(4) 0.0299(10) Uani 1 1 d . . .
O3 O -0.2764(3) 0.3896(3) 0.2836(4) 0.0439(13) Uani 1 1 d . . .
O4 O -0.2108(3) 0.3038(3) 0.1313(9) 0.090(3) Uani 1 1 d U . .
O5 O -0.3441(5) 0.3062(3) -0.0066(4) 0.071(2) Uani 1 1 d . . .
O6 O -0.4143(3) 0.3858(3) 0.1603(6) 0.0632(17) Uani 1 1 d DU . .
H6A H -0.4204 0.3702 0.2254 0.076 Uiso 1 1 d R A .
N3 N -0.3428(4) 0.2500 -0.4108(6) 0.0272(16) Uiso 1 2 d S . .
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
O3 Co1 O5 167.3(2) . .
O3 Co1 O4 85.2(3) . .
O5 Co1 O4 95.2(4) . .
O3 Co1 O1 96.62(19) . .
O5 Co1 O1 96.0(2) . .
O4 Co1 O1 94.6(2) . .
O3 Co1 O6 91.7(3) . .
O5 Co1 O6 86.4(3) . .
O4 Co1 O6 173.0(2) . .
O1 Co1 O6 92.0(2) . .
O3 Co1 N1 82.87(19) . 2_464
O5 Co1 N1 84.5(2) . 2_464
O4 Co1 N1 85.9(2) . 2_464
O1 Co1 N1 179.28(19) . 2_464
O6 Co1 N1 87.5(2) . 2_464
O2 Co2 O2 166.5(2) . 7_565
O2 Co2 O1 96.69(12) . .
O2 Co2 O1 96.69(12) 7_565 .
O2 Co2 N2 90.70(13) . 6_556
O2 Co2 N2 90.70(13) 7_565 6_556
O1 Co2 N2 90.2(2) . 6_556
O2 Co2 O1W 89.56(13) . .
O2 Co2 O1W 89.56(13) 7_565 .
O1 Co2 O1W 87.6(2) . .
N2 Co2 O1W 177.8(3) 6_556 .
O2 Co2 N3 83.32(12) . 1_556
O2 Co2 N3 83.32(12) 7_565 1_556
O1 Co2 N3 179.2(2) . 1_556
N2 Co2 N3 89.0(3) 6_556 1_556
O1W Co2 N3 93.1(3) . 1_556
C2 C3 C4 118.3(6) . .
C2 C3 C6 121.8(6) . .
C4 C3 C6 119.9(6) . .
C3 C2 C1 119.0(6) . .
N1 C1 C2 123.0(6) . .
N1 C5 C4 123.2(6) . .
C5 C4 C3 118.8(7) . .
O2 C6 O3 126.7(6) . .
O2 C6 C3 117.3(6) . .
O3 C6 C3 116.1(6) . .
C8 C9A C8 110.7(13) . 7_565
C8 C9A C8' 118.1(10) . 7_565
C8 C9A C8' 33.6(8) 7_565 7_565
C8 C9A C8' 33.6(8) . .
C8 C9A C8' 118.1(10) 7_565 .
C8' C9A C8' 104.8(17) 7_565 .
C8 C9A C10 120.2(7) . .
C8 C9A C10 120.2(7) 7_565 .
C8' C9A C10 121.6(9) 7_565 .
C8' C9A C10 121.6(9) . .
C9A C8 C7 118.1(11) . .
C9A C8' C7' 117.5(15) . .
N2 C7 C8 124.4(11) . .
N2 C7' C8' 124.2(16) . .
O4 C10 O4 123.8(10) 7_565 .
O4 C10 C9A 118.1(5) 7_565 .
O4 C10 C9A 118.1(5) . .
C12' C13 C12' 88.1(12) 7_565 .
C12' C13 C12 117.7(10) 7_565 .
C12' C13 C12 58.6(9) . .
C12' C13 C12 58.6(9) 7_565 7_565
C12' C13 C12 117.7(10) . 7_565
C12 C13 C12 90.4(14) . 7_565
C12' C13 C14 122.2(7) 7_565 .
C12' C13 C14 122.2(7) . .
C12 C13 C14 120.0(7) . .
C12 C13 C14 120.0(7) 7_565 .
C11 C12 C13 119.2(12) . .
C11 C12 C12 89.1(9) . 7_565
C13 C12 C12 44.8(7) . 7_565
C11' C12' C13 119.4(11) . .
C11' C12' C12' 88.2(8) . 7_565
C13 C12' C12' 46.0(6) . 7_565
N3 C11 C12 122.4(12) . .
N3 C11 C11 44.6(7) . 7_565
C12 C11 C11 90.9(9) . 7_565
N3 C11' C12' 123.8(11) . .
N3 C11' C11' 46.1(6) . 7_565
C12' C11' C11' 91.8(8) . 7_565
O5 C14 O5 127.7(9) . 7_565
O5 C14 C13 116.1(5) . .
O5 C14 C13 116.1(5) 7_565 .
O6 C15 C16 139.5(18) . .
O6 C15' C16' 119.8(17) . .
C17 C16 C15 110.3(13) . .
C17' C16' C15' 113.9(13) . .
C18 C17 C16 109.9(13) . .
C16' C17' C18' 110.2(14) . .
C5 N1 C1 117.5(6) . .
C5 N1 Co1 121.6(4) . 2_465
C1 N1 Co1 120.8(4) . 2_465
C7' N2 C7' 100.5(18) 7_565 .
C7' N2 C7 116.4(10) 7_565 .
C7' N2 C7 34.6(9) . .
C7' N2 C7 34.6(9) 7_565 7_565
C7' N2 C7 116.4(10) . 7_565
C7 N2 C7 110.9(14) . 7_565
C7' N2 Co2 124.1(9) 7_565 6_656
C7' N2 Co2 124.1(9) . 6_656
C7 N2 Co2 119.5(6) . 6_656
C7 N2 Co2 119.5(6) 7_565 6_656
Co1 O1 Co1 109.1(2) 7_565 .
Co1 O1 Co2 118.54(15) 7_565 .
Co1 O1 Co2 118.54(15) . .
C6 O2 Co2 124.2(4) . .
C6 O3 Co1 132.4(4) . .
C10 O4 Co1 136.9(6) . .
C14 O5 Co1 131.9(6) . .
C15 O6 C15' 105.4(15) . .
C15 O6 Co1 127.6(10) . .
C15' O6 Co1 127.0(12) . .
C11 N3 C11 90.8(14) . 7_565
C11 N3 C11' 58.1(9) . .
C11 N3 C11' 117.4(9) 7_565 .
C11 N3 C11' 117.4(9) . 7_565
C11 N3 C11' 58.1(9) 7_565 7_565
C11' N3 C11' 87.8(13) . 7_565
C11 N3 Co2 121.8(7) . 1_554
C11 N3 Co2 121.8(7) 7_565 1_554
C11' N3 Co2 120.8(6) . 1_554
C11' N3 Co2 120.8(6) 7_565 1_554
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O3 2.050(4) .
Co1 O5 2.046(5) .
Co1 O4 2.054(6) .
Co1 O1 2.101(3) .
Co1 O6 2.147(5) .
Co1 N1 2.177(5) 2_464
Co2 O2 2.082(4) .
Co2 O2 2.082(4) 7_565
Co2 O1 2.118(5) .
Co2 N2 2.135(7) 6_556
Co2 O1W 2.141(7) .
Co2 N3 2.196(8) 1_556
C3 C2 1.372(10) .
C3 C4 1.396(10) .
C3 C6 1.510(9) .
C2 C1 1.396(10) .
C1 N1 1.335(9) .
C5 N1 1.335(9) .
C5 C4 1.383(10) .
C6 O2 1.260(8) .
C6 O3 1.249(8) .
C9A C8 1.371(14) .
C9A C8 1.371(14) 7_565
C9A C8' 1.369(18) 7_565
C9A C8' 1.369(18) .
C9A C10 1.513(12) .
C8 C7 1.393(17) .
C8' C7' 1.41(2) .
C7 N2 1.296(13) .
C7' N2 1.293(18) .
C10 O4 1.189(7) 7_565
C10 O4 1.189(7) .
C13 C12' 1.395(14) 7_565
C13 C12' 1.395(14) .
C13 C12 1.396(16) .
C13 C12 1.396(16) 7_565
C13 C14 1.538(12) .
C12 C11 1.396(19) .
C12 C12 1.98(3) 7_565
C12' C11' 1.378(18) .
C12' C12' 1.94(3) 7_565
C11 N3 1.359(14) .
C11 C11 1.94(3) 7_565
C11' N3 1.333(14) .
C11' C11' 1.85(3) 7_565
C14 O5 1.219(7) .
C14 O5 1.219(7) 7_565
C15 O6 1.412(9) .
C15 C16 1.527(10) .
C15' O6 1.450(10) .
C15' C16' 1.526(10) .
C16 C17 1.523(10) .
C16' C17' 1.517(10) .
C17 C18 1.520(10) .
C17' C18' 1.526(10) .
N1 Co1 2.177(5) 2_465
N2 C7' 1.293(18) 7_565
N2 C7 1.296(13) 7_565
N2 Co2 2.135(7) 6_656
O1 Co1 2.101(3) 7_565
N3 C11 1.359(14) 7_565
N3 C11' 1.333(14) 7_565
N3 Co2 2.196(8) 1_554
