#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:00:20 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179608 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/72/4507265.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_4507265
loop_
_publ_author_name
'Hou, Lei'
'Liu, Bin'
'Jia, Li-Na'
'Wei, Lei'
'Wang, Yao-Yu'
'Shi, Qi-Zhen'
_publ_section_title
;
 Two New (3,6)-Connected Frameworks Based on an Unsymmetrical Tritopic
 Pyridyldicarboxylate Ligand and Co2Dimer: Structures, Magnetic, and
 Sorption Properties
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              701
_journal_paper_doi               10.1021/cg301413u
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C26 H20 Co2 N2 O11'
_chemical_formula_weight         654.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.050(3)
_cell_length_b                   11.050(3)
_cell_length_c                   27.772(10)
_cell_measurement_reflns_used    5094
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.85
_cell_measurement_theta_min      2.18
_cell_volume                     2936.7(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0847
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11060
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_T_max  0.9161
_exptl_absorpt_correction_T_min  0.8418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0421
_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)+(0.0364P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                2567
_reflns_number_total             3800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301413u_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        2936.8(16)
_cod_original_sg_symbol_H-M      P3(1)21
_cod_database_code               4507265
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
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
N1 N 0.1503(4) 0.6878(4) 0.28022(13) 0.0457(10) Uani 1 1 d .
Co1 Co 0.92301(6) 0.75378(6) 0.02925(2) 0.03432(16) Uani 1 1 d .
C1 C 0.2400(5) 0.7207(5) 0.24356(16) 0.0457(12) Uani 1 1 d .
H1 H 0.2536 0.7932 0.2231 0.055 Uiso 1 1 calc R
C2 C 0.3142(5) 0.6512(5) 0.23461(16) 0.0421(11) Uani 1 1 d .
C3 C 0.2906(5) 0.5438(5) 0.26526(17) 0.0457(12) Uani 1 1 d .
H3 H 0.3365 0.4938 0.2602 0.055 Uiso 1 1 calc R
C4 C 0.1974(5) 0.5090(5) 0.30424(17) 0.0470(12) Uani 1 1 d .
C5 C 0.1245(5) 0.5834(5) 0.30878(16) 0.0452(12) Uani 1 1 d .
H5 H 0.0568 0.5576 0.3326 0.054 Uiso 1 1 calc R
C6 C 0.1680(5) 0.3923(5) 0.33822(17) 0.0445(12) Uani 1 1 d .
C7 C 0.4129(5) 0.6947(5) 0.19330(16) 0.0476(12) Uani 1 1 d .
C8 C 0.3844(6) 0.7423(5) 0.15122(17) 0.0559(13) Uani 1 1 d .
H8 H 0.3069 0.7540 0.1493 0.067 Uiso 1 1 calc R
C9 C 0.4729(5) 0.7726(6) 0.11163(17) 0.0504(13) Uani 1 1 d .
H9 H 0.4543 0.8067 0.0836 0.060 Uiso 1 1 calc R
C10 C 0.5898(5) 0.7531(5) 0.11285(17) 0.0412(11) Uani 1 1 d .
C11 C 0.6213(5) 0.7110(6) 0.15750(19) 0.0538(13) Uani 1 1 d .
H11 H 0.7019 0.7047 0.1603 0.065 Uiso 1 1 calc R
C12 C 0.5325(5) 0.6793(6) 0.19669(17) 0.0487(12) Uani 1 1 d .
H12 H 0.5515 0.6479 0.2252 0.058 Uiso 1 1 calc R
C13 C 0.6828(5) 0.7801(4) 0.07048(18) 0.0410(11) Uani 1 1 d .
O1 O 0.7793(4) 0.7539(3) 0.07519(11) 0.0505(9) Uani 1 1 d .
O1W O 0.9572(4) 0.9572(4) 0.0000 0.0410(10) Uani 1 2 d S
H1W1 H 1.0184 0.9846 -0.0222 0.061 Uiso 1 1 d R
O2W O 1.0601(4) 0.8615(4) 0.08851(12) 0.0635(10) Uani 1 1 d .
H2W1 H 1.0309 0.8050 0.1121 0.095 Uiso 1 1 d R
H2W2 H 1.1473 0.8923 0.0859 0.095 Uiso 1 1 d R
O2 O 0.6508(4) 0.8187(4) 0.03262(12) 0.0585(10) Uani 1 1 d .
O3 O 0.2261(4) 0.3225(3) 0.32827(12) 0.0481(8) Uani 1 1 d .
O4 O 0.0928(5) 0.3746(4) 0.37317(15) 0.0791(13) 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'
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
C5 N1 C1 120.3(4) . .
C5 N1 Co1 117.0(3) . 6_665
C1 N1 Co1 121.4(3) . 6_665
O1 Co1 O3 167.80(13) . 3_664
O1 Co1 O2 107.52(15) . 4
O3 Co1 O2 84.67(14) 3_664 4
O1 Co1 O2W 81.58(14) . .
O3 Co1 O2W 86.23(13) 3_664 .
O2 Co1 O2W 170.85(14) 4 .
O1 Co1 N1 87.04(14) . 6_655
O3 Co1 N1 94.26(14) 3_664 6_655
O2 Co1 N1 81.47(14) 4 6_655
O2W Co1 N1 98.36(15) . 6_655
O1 Co1 O1W 88.10(10) . .
O3 Co1 O1W 92.47(12) 3_664 .
O2 Co1 O1W 91.07(12) 4 .
O2W Co1 O1W 90.19(13) . .
N1 Co1 O1W 169.44(15) 6_655 .
N1 C1 C2 123.0(4) . .
N1 C1 H1 118.5 . .
C2 C1 H1 118.5 . .
C3 C2 C1 117.0(4) . .
C3 C2 C7 123.3(4) . .
C1 C2 C7 119.8(4) . .
C2 C3 C4 120.6(4) . .
C2 C3 H3 119.7 . .
C4 C3 H3 119.7 . .
C3 C4 C5 117.4(4) . .
C3 C4 C6 122.3(4) . .
C5 C4 C6 120.2(4) . .
N1 C5 C4 121.5(4) . .
N1 C5 H5 119.3 . .
C4 C5 H5 119.3 . .
O4 C6 O3 126.1(4) . .
O4 C6 C4 118.3(4) . .
O3 C6 C4 115.6(4) . .
C8 C7 C12 120.4(4) . .
C8 C7 C2 120.4(4) . .
C12 C7 C2 119.1(4) . .
C7 C8 C9 119.5(5) . .
C7 C8 H8 120.3 . .
C9 C8 H8 120.3 . .
C8 C9 C10 121.9(5) . .
C8 C9 H9 119.0 . .
C10 C9 H9 119.0 . .
C9 C10 C11 117.5(4) . .
C9 C10 C13 122.8(5) . .
C11 C10 C13 119.7(4) . .
C12 C11 C10 120.4(4) . .
C12 C11 H11 119.8 . .
C10 C11 H11 119.8 . .
C11 C12 C7 120.1(5) . .
C11 C12 H12 120.0 . .
C7 C12 H12 120.0 . .
O1 C13 O2 126.1(4) . .
O1 C13 C10 117.1(4) . .
O2 C13 C10 116.6(4) . .
C13 O1 Co1 133.9(3) . .
Co1 O1W Co1 108.17(19) 4 .
Co1 O1W H1W1 110.5 4 .
Co1 O1W H1W1 109.0 . .
Co1 O2W H2W1 106.3 . .
Co1 O2W H2W2 120.1 . .
H2W1 O2W H2W2 107.2 . .
C13 O2 Co1 136.0(3) . 4
C6 O3 Co1 134.8(3) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C5 1.309(5) .
N1 C1 1.339(5) .
N1 Co1 2.206(4) 6_665
Co1 O1 2.037(3) .
Co1 O3 2.050(3) 3_664
Co1 O2 2.065(3) 4
Co1 O2W 2.149(3) .
Co1 N1 2.206(4) 6_655
Co1 O1W 2.237(3) .
C1 C2 1.398(6) .
C1 H1 0.9300 .
C2 C3 1.375(6) .
C2 C7 1.487(6) .
C3 C4 1.408(6) .
C3 H3 0.9300 .
C4 C5 1.416(6) .
C4 C6 1.496(7) .
C5 H5 0.9300 .
C6 O4 1.228(6) .
C6 O3 1.257(5) .
C7 C8 1.381(7) .
C7 C12 1.418(7) .
C8 C9 1.396(6) .
C8 H8 0.9300 .
C9 C10 1.413(6) .
C9 H9 0.9300 .
C10 C11 1.427(7) .
C10 C13 1.491(7) .
C11 C12 1.388(7) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 O1 1.245(6) .
C13 O2 1.250(6) .
O1W Co1 2.237(3) 4
O1W H1W1 0.8505 .
O2W H2W1 0.8501 .
O2W H2W2 0.8501 .
O2 Co1 2.065(3) 4
O3 Co1 2.050(3) 2_655
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.105 1243 377 ' '
