#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/19/7201962.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_7201962
loop_
_publ_author_name
'Zhu, Ping'
'Gu, Wen'
'Cheng, Fang-Yi'
'Liu, Xin'
'Chen, Jun'
'Yan, Shi-Ping'
'Liao, Dai-Zheng'
_publ_section_title
;
 Design of two 3D homochiral Co(II) metal--organic open frameworks by
 layered-pillar strategy: structure and properties
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              963
_journal_paper_doi               10.1039/b801177j
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C9 H12 Co N2 O5.50'
_chemical_formula_sum            'C9 H12 Co N2 O5.5'
_chemical_formula_weight         295.14
_chemical_name_systematic
;
?
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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            4
_cell_length_a                   22.113(3)
_cell_length_b                   6.9149(12)
_cell_length_c                   7.7209(14)
_cell_measurement_reflns_used    2949
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.6
_cell_volume                     1180.6(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8796
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_T_max  0.8433
_exptl_absorpt_correction_T_min  0.7988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.14(7)
_refine_ls_extinction_coef       0.010(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2084
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0700
_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)+(0.0666P)²+7.4016P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1716
_reflns_number_gt                1956
_reflns_number_total             2084
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801177j.txt
_cod_data_source_block           shelxl
_cod_original_formula_sum        'C9 H12 Co N2 O5.50'
_cod_database_code               7201962
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
'-x, -y, z'
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 0.71252(4) 0.45830(13) 0.24225(15) 0.0236(3) Uani 1 1 d . . .
N1 N 0.6983(3) 1.0653(8) -0.2199(10) 0.0298(15) Uani 1 1 d D . .
H1A H 0.6964 1.1629 -0.1392 0.036 Uiso 1 1 calc RD . .
H1B H 0.6847 1.1115 -0.3246 0.036 Uiso 1 1 calc RD . .
O1 O 0.6708(3) 0.6563(9) 0.0615(9) 0.0365(16) Uani 1 1 d . A .
O2 O 0.7551(3) 0.7960(9) -0.0367(7) 0.0320(15) Uani 1 1 d . . .
O3 O 0.7470(2) 0.7536(9) -0.4186(7) 0.0258(13) Uani 1 1 d . . .
O4 O 0.6729(3) 0.6144(12) -0.5668(10) 0.0470(19) Uani 1 1 d . . .
C1 C 0.6987(4) 0.7687(13) -0.0408(11) 0.030(2) Uani 1 1 d . . .
C2 C 0.6624(3) 0.8958(11) -0.1636(11) 0.0284(18) Uani 1 1 d . A .
H2 H 0.6254 0.9426 -0.1019 0.034 Uiso 1 1 calc R . .
C3 C 0.6433(4) 0.7778(12) -0.3170(11) 0.0312(19) Uani 1 1 d . . .
H3A H 0.6123 0.8521 -0.3814 0.037 Uiso 1 1 calc R A .
H3B H 0.6235 0.6588 -0.2736 0.037 Uiso 1 1 calc R . .
C4 C 0.6945(5) 0.7160(15) -0.4496(13) 0.040(3) Uani 1 1 d . A .
N2 N 0.6318(4) 0.288(2) 0.2670(16) 0.026(2) Uani 0.521(11) 1 d PGU A 1
C5 C 0.5774(5) 0.3730(15) 0.3151(16) 0.027(4) Uani 0.521(11) 1 d PGU A 1
H5A H 0.5758 0.5080 0.3377 0.032 Uiso 0.521(11) 1 calc PR A 1
C6 C 0.5255(4) 0.2610(16) 0.3303(16) 0.035(4) Uani 0.521(11) 1 d PGU A 1
H6A H 0.4884 0.3194 0.3631 0.042 Uiso 0.521(11) 1 calc PR A 1
C7 C 0.5280(5) 0.0635(16) 0.2973(17) 0.027(4) Uani 0.521(11) 1 d PGU . 1
C8 C 0.5823(7) -0.0219(15) 0.2492(19) 0.039(16) Uani 0.521(11) 1 d PGU A 1
H8A H 0.5840 -0.1568 0.2266 0.047 Uiso 0.521(11) 1 calc PR A 1
C9 C 0.6342(5) 0.090(2) 0.2340(19) 0.022(3) Uani 0.521(11) 1 d PGU A 1
H9A H 0.6714 0.0318 0.2012 0.026 Uiso 0.521(11) 1 calc PR A 1
N3 N 0.6325(4) 0.288(2) 0.2083(18) 0.026(2) Uani 0.479(11) 1 d PGU A 2
C10 C 0.6353(5) 0.097(2) 0.2651(19) 0.018(3) Uani 0.479(11) 1 d PGU A 2
H10A H 0.6722 0.0462 0.3079 0.022 Uiso 0.479(11) 1 calc PR A 2
C11 C 0.5839(7) -0.0186(16) 0.2593(18) 0.017(11) Uani 0.479(11) 1 d PGU A 2
H11A H 0.5858 -0.1488 0.2981 0.021 Uiso 0.479(11) 1 calc PR A 2
C12 C 0.5298(5) 0.0562(15) 0.1967(17) 0.023(4) Uani 0.479(11) 1 d PGU . 2
C13 C 0.5270(4) 0.2467(17) 0.1399(17) 0.028(4) Uani 0.479(11) 1 d PGU A 2
H13A H 0.4900 0.2978 0.0972 0.033 Uiso 0.479(11) 1 calc PR A 2
C14 C 0.5784(5) 0.3625(15) 0.1457(18) 0.035(5) Uani 0.479(11) 1 d PGU A 2
H14A H 0.5765 0.4927 0.1069 0.042 Uiso 0.479(11) 1 calc PR A 2
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
_geom_angle_publ_flag
O4 Co1 O2 174.6(3) 1_556 3_645 ?
O4 Co1 N1 106.0(3) 1_556 3_645 ?
O2 Co1 N1 78.7(3) 3_645 3_645 ?
O4 Co1 N3 91.5(5) 1_556 . ?
O2 Co1 N3 83.9(4) 3_645 . ?
N1 Co1 N3 162.4(4) 3_645 . ?
O4 Co1 N2 82.5(4) 1_556 . ?
O2 Co1 N2 93.3(4) 3_645 . ?
N1 Co1 N2 167.1(4) 3_645 . ?
N3 Co1 N2 12.1(5) . . ?
O4 Co1 O3 94.0(3) 1_556 3_645 ?
O2 Co1 O3 89.1(2) 3_645 3_645 ?
N1 Co1 O3 83.9(2) 3_645 3_645 ?
N3 Co1 O3 93.4(4) . 3_645 ?
N2 Co1 O3 85.9(4) . 3_645 ?
O4 Co1 O1 87.0(2) 1_556 . ?
O2 Co1 O1 89.8(3) 3_645 . ?
N1 Co1 O1 97.1(2) 3_645 . ?
N3 Co1 O1 85.3(4) . . ?
N2 Co1 O1 92.9(4) . . ?
O3 Co1 O1 178.3(3) 3_645 . ?
C2 N1 Co1 104.3(4) . 3_655 ?
C2 N1 H1A 110.9 . . ?
Co1 N1 H1A 110.9 3_655 . ?
C2 N1 H1B 110.9 . . ?
Co1 N1 H1B 110.9 3_655 . ?
H1A N1 H1B 108.9 . . ?
C1 O1 Co1 125.6(5) . . ?
C1 O2 Co1 113.8(5) . 3_655 ?
C4 O3 Co1 131.5(6) . 3_655 ?
C4 O4 Co1 131.8(7) . 1_554 ?
O2 C1 O1 123.8(8) . . ?
O2 C1 C2 116.8(7) . . ?
O1 C1 C2 119.0(7) . . ?
N1 C2 C3 110.5(7) . . ?
N1 C2 C1 110.9(6) . . ?
C3 C2 C1 109.1(7) . . ?
N1 C2 H2 108.8 . . ?
C3 C2 H2 108.8 . . ?
C1 C2 H2 108.8 . . ?
C2 C3 C4 117.1(7) . . ?
C2 C3 H3A 108.0 . . ?
C4 C3 H3A 108.0 . . ?
C2 C3 H3B 108.0 . . ?
C4 C3 H3B 108.0 . . ?
H3A C3 H3B 107.3 . . ?
O3 C4 O4 129.3(9) . . ?
O3 C4 C3 119.9(8) . . ?
O4 C4 C3 110.4(9) . . ?
C5 N2 C9 120.0 . . ?
C5 N2 Co1 120.6(7) . . ?
C9 N2 Co1 119.4(7) . . ?
C6 C5 N2 120.0 . . ?
C6 C5 H5A 120.0 . . ?
N2 C5 H5A 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 H6A 120.0 . . ?
C7 C6 H6A 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 C7 117.3(16) . 4_655 ?
C6 C7 C7 122.5(16) . 4_655 ?
C7 C8 C9 120.0 . . ?
C7 C8 H8A 120.0 . . ?
C9 C8 H8A 120.0 . . ?
C8 C9 N2 120.0 . . ?
C8 C9 H9A 120.0 . . ?
N2 C9 H9A 120.0 . . ?
C10 N3 C14 120.0 . . ?
C10 N3 Co1 116.5(8) . . ?
C14 N3 Co1 123.3(8) . . ?
N3 C10 C11 120.0 . . ?
N3 C10 H10A 120.0 . . ?
C11 C10 H10A 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 H11A 120.0 . . ?
C12 C11 H11A 120.0 . . ?
C13 C12 C11 120.0 . . ?
C13 C12 C12 116.3(15) . 4_655 ?
C11 C12 C12 123.6(14) . 4_655 ?
C12 C13 C14 120.0 . . ?
C12 C13 H13A 120.0 . . ?
C14 C13 H13A 120.0 . . ?
C13 C14 N3 120.0 . . ?
C13 C14 H14A 120.0 . . ?
N3 C14 H14A 120.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O4 2.025(7) 1_556 ?
Co1 O2 2.072(6) 3_645 ?
Co1 N1 2.113(6) 3_645 ?
Co1 N3 2.143(10) . ?
Co1 N2 2.148(10) . ?
Co1 O3 2.158(6) 3_645 ?
Co1 O1 2.162(6) . ?
N1 C2 1.481(10) . ?
N1 Co1 2.113(6) 3_655 ?
N1 H1A 0.9200 . ?
N1 H1B 0.9200 . ?
O1 C1 1.268(11) . ?
O2 C1 1.261(11) . ?
O2 Co1 2.072(6) 3_655 ?
O3 C4 1.213(12) . ?
O3 Co1 2.158(6) 3_655 ?
O4 C4 1.241(12) . ?
O4 Co1 2.026(7) 1_554 ?
C1 C2 1.522(11) . ?
C2 C3 1.499(11) . ?
C2 H2 1.0000 . ?
C3 C4 1.586(12) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N2 C5 1.3900 . ?
N2 C9 1.3900 . ?
C5 C6 1.3900 . ?
C5 H5A 0.9500 . ?
C6 C7 1.3900 . ?
C6 H6A 0.9500 . ?
C7 C8 1.3900 . ?
C7 C7 1.517(19) 4_655 ?
C8 C9 1.3900 . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9500 . ?
N3 C10 1.3900 . ?
N3 C14 1.3900 . ?
C10 C11 1.3900 . ?
C10 H10A 0.9500 . ?
C11 C12 1.3900 . ?
C11 H11A 0.9500 . ?
C12 C13 1.3900 . ?
C12 C12 1.53(2) 4_655 ?
C13 C14 1.3900 . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Co1 O1 C1 116.9(8) 1_556 . . . ?
O2 Co1 O1 C1 -67.5(8) 3_645 . . . ?
N1 Co1 O1 C1 11.1(8) 3_645 . . . ?
N3 Co1 O1 C1 -151.4(9) . . . . ?
N2 Co1 O1 C1 -160.8(8) . . . . ?
O3 Co1 O1 C1 -115(8) 3_645 . . . ?
Co1 O2 C1 O1 172.0(7) 3_655 . . . ?
Co1 O2 C1 C2 -14.8(10) 3_655 . . . ?
Co1 O1 C1 O2 -8.5(13) . . . . ?
Co1 O1 C1 C2 178.4(6) . . . . ?
Co1 N1 C2 C3 -85.1(6) 3_655 . . . ?
Co1 N1 C2 C1 36.0(7) 3_655 . . . ?
O2 C1 C2 N1 -15.9(11) . . . . ?
O1 C1 C2 N1 157.6(8) . . . . ?
O2 C1 C2 C3 106.1(9) . . . . ?
O1 C1 C2 C3 -80.4(10) . . . . ?
N1 C2 C3 C4 51.5(9) . . . . ?
C1 C2 C3 C4 -70.6(9) . . . . ?
Co1 O3 C4 O4 170.1(8) 3_655 . . . ?
Co1 O3 C4 C3 -18.2(14) 3_655 . . . ?
Co1 O4 C4 O3 1.6(18) 1_554 . . . ?
Co1 O4 C4 C3 -170.7(6) 1_554 . . . ?
C2 C3 C4 O3 4.8(13) . . . . ?
C2 C3 C4 O4 177.9(8) . . . . ?
O4 Co1 N2 C5 31.5(7) 1_556 . . . ?
O2 Co1 N2 C5 -145.1(7) 3_645 . . . ?
N1 Co1 N2 C5 163.7(15) 3_645 . . . ?
N3 Co1 N2 C5 -106(4) . . . . ?
O3 Co1 N2 C5 126.1(7) 3_645 . . . ?
O1 Co1 N2 C5 -55.1(7) . . . . ?
O4 Co1 N2 C9 -148.7(6) 1_556 . . . ?
O2 Co1 N2 C9 34.8(6) 3_645 . . . ?
N1 Co1 N2 C9 -16(2) 3_645 . . . ?
N3 Co1 N2 C9 74(4) . . . . ?
O3 Co1 N2 C9 -54.1(6) 3_645 . . . ?
O1 Co1 N2 C9 124.7(6) . . . . ?
C9 N2 C5 C6 0.0 . . . . ?
Co1 N2 C5 C6 179.8(8) . . . . ?
N2 C5 C6 C7 0.0 . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C5 C6 C7 C7 -174.9(4) . . . 4_655 ?
C6 C7 C8 C9 0.0 . . . . ?
C7 C7 C8 C9 175.2(5) 4_655 . . . ?
C7 C8 C9 N2 0.0 . . . . ?
C5 N2 C9 C8 0.0 . . . . ?
Co1 N2 C9 C8 -179.8(8) . . . . ?
O4 Co1 N3 C10 -108.5(6) 1_556 . . . ?
O2 Co1 N3 C10 74.4(6) 3_645 . . . ?
N1 Co1 N3 C10 66.1(16) 3_645 . . . ?
N2 Co1 N3 C10 -66(3) . . . . ?
O3 Co1 N3 C10 -14.4(6) 3_645 . . . ?
O1 Co1 N3 C10 164.6(6) . . . . ?
O4 Co1 N3 C14 66.7(8) 1_556 . . . ?
O2 Co1 N3 C14 -110.5(8) 3_645 . . . ?
N1 Co1 N3 C14 -118.8(14) 3_645 . . . ?
N2 Co1 N3 C14 109(4) . . . . ?
O3 Co1 N3 C14 160.8(7) 3_645 . . . ?
O1 Co1 N3 C14 -20.2(7) . . . . ?
C14 N3 C10 C11 0.0 . . . . ?
Co1 N3 C10 C11 175.3(9) . . . . ?
N3 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C10 C11 C12 C12 -175.8(8) . . . 4_655 ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C12 C13 C14 176.1(6) 4_655 . . . ?
C12 C13 C14 N3 0.0 . . . . ?
C10 N3 C14 C13 0.0 . . . . ?
Co1 N3 C14 C13 -175.0(9) . . . . ?
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
1 0.000 -0.021 0.255 84.7 26.6
2 0.500 -0.033 0.745 84.7 27.3
