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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/39/4333971.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_4333971
loop_
_publ_author_name
'Ming-Hua Zeng'
'Yan-Xi Tan'
'Yan-Ping He'
'Zheng Yin'
'Qing Chen'
'Mohamedally Kurmoo'
_publ_contact_author_address
'No.15, Yucai Road, GuangXi Normal University, Guilin, China'
_publ_contact_author_email       ZMH@MAILBOX.GXNU.EDU.CN
_publ_contact_author_name        'Ming-Hua Zeng'
_publ_section_title
;
 A Porous 4-Fold-Interpenetrated Chiral Framework Exhibiting Vapochromism,
 Single-Crystal-to-Single-Crystal Solvent Exchange, Gas Sorption, and a
 Poisoning Effect
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2353
_journal_page_last               2360
_journal_paper_doi               10.1021/ic301857h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C29 H16 Co N2 O6.5'
_chemical_formula_weight         555.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           90
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4ab 2ab'
_symmetry_space_group_name_H-M   'P 4 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            8
_cell_length_a                   22.6904(17)
_cell_length_b                   22.6904(17)
_cell_length_c                   12.695(2)
_cell_measurement_temperature    173(2)
_cell_volume                     6536.1(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0853
_diffrn_reflns_av_sigmaI/netI    0.0796
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            30993
_diffrn_reflns_theta_full        26.15
_diffrn_reflns_theta_max         26.15
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.8956
_exptl_absorpt_correction_T_min  0.8582
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(4)
_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     305
_refine_ls_number_reflns         6522
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0779
_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)+(0.1328P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2060
_refine_ls_wR_factor_ref         0.2260
_reflns_number_gt                4193
_reflns_number_total             6522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301857h_si_001_4.cif
_cod_data_source_block           1.2.5EtOH
_cod_original_cell_volume        6536.2(12)
_cod_original_formula_sum        'C29 H16 Co N2 O6.50'
_cod_database_code               4333971
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y+1/2, x+1/2, z'
'y+1/2, -x+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'y, x, -z'
'-y, -x, -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
Co1 Co 0.23208(3) 0.24086(3) 0.25335(6) 0.0279(2) Uani 1 1 d .
C1 C -0.1835(3) 0.2671(2) 0.5668(5) 0.0356(14) Uani 1 1 d .
H1A H -0.2136 0.2916 0.5387 0.043 Uiso 1 1 calc R
C2 C -0.1325(3) 0.2579(3) 0.5050(5) 0.0369(14) Uani 1 1 d .
H2A H -0.1275 0.2775 0.4394 0.044 Uiso 1 1 calc R
C3 C -0.0902(3) 0.2195(3) 0.5430(5) 0.0379(15) Uani 1 1 d .
C4 C -0.0988(3) 0.1926(3) 0.6385(5) 0.0416(16) Uani 1 1 d .
H4A H -0.0706 0.1655 0.6656 0.050 Uiso 1 1 calc R
C5 C -0.1497(3) 0.2059(3) 0.6949(5) 0.0372(15) Uani 1 1 d .
H5A H -0.1554 0.1873 0.7613 0.045 Uiso 1 1 calc R
C6 C -0.0339(3) 0.2126(3) 0.4838(5) 0.0415(16) Uani 1 1 d .
C7 C -0.0315(3) 0.2193(4) 0.3750(5) 0.0521(19) Uani 1 1 d .
H7A H -0.0670 0.2246 0.3364 0.063 Uiso 1 1 calc R
C8 C 0.0212(2) 0.2184(4) 0.3227(6) 0.0486(19) Uani 1 1 d .
H8A H 0.0220 0.2247 0.2488 0.058 Uiso 1 1 calc R
C9 C 0.0728(3) 0.2084(3) 0.3761(5) 0.0362(14) Uani 1 1 d .
C10 C 0.0721(3) 0.1992(3) 0.4816(5) 0.0415(16) Uani 1 1 d .
H10A H 0.1079 0.1924 0.5183 0.050 Uiso 1 1 calc R
C11 C 0.0183(3) 0.1997(3) 0.5370(5) 0.0410(16) Uani 1 1 d .
H11A H 0.0175 0.1912 0.6103 0.049 Uiso 1 1 calc R
C12 C 0.1327(3) 0.2145(3) 0.3198(5) 0.0318(14) Uani 1 1 d .
C13 C 0.2460(3) 0.6100(2) -0.2330(5) 0.0502(18) Uani 1 1 d .
H13A H 0.2506 0.6104 -0.3073 0.060 Uiso 1 1 calc R
C14 C 0.2399(3) 0.5567(2) -0.1831(6) 0.0466(18) Uani 1 1 d .
H14A H 0.2405 0.5213 -0.2230 0.056 Uiso 1 1 calc R
C15 C 0.2330(3) 0.5543(2) -0.0752(5) 0.0313(14) Uani 1 1 d .
C16 C 0.2303(3) 0.6069(3) -0.0228(5) 0.0428(17) Uani 1 1 d .
H16A H 0.2241 0.6075 0.0512 0.051 Uiso 1 1 calc R
C17 C 0.2368(3) 0.6602(3) -0.0782(5) 0.0391(15) Uani 1 1 d .
H17A H 0.2347 0.6964 -0.0407 0.047 Uiso 1 1 calc R
C18 C 0.2276(3) 0.4983(3) -0.0156(5) 0.0386(15) Uani 1 1 d .
C19 C 0.2585(4) 0.4480(2) -0.0499(6) 0.0465(18) Uani 1 1 d .
H19A H 0.2811 0.4502 -0.1127 0.056 Uiso 1 1 calc R
C20 C 0.2566(3) 0.3956(3) 0.0054(6) 0.0518(19) Uani 1 1 d .
H20A H 0.2772 0.3620 -0.0200 0.062 Uiso 1 1 calc R
C21 C 0.2247(3) 0.3924(2) 0.0981(5) 0.0329(14) Uani 1 1 d .
C22 C 0.1935(3) 0.4416(3) 0.1330(6) 0.0481(18) Uani 1 1 d .
H22A H 0.1706 0.4393 0.1955 0.058 Uiso 1 1 calc R
C23 C 0.1958(3) 0.4946(3) 0.0755(5) 0.0423(16) Uani 1 1 d .
H23A H 0.1750 0.5282 0.1004 0.051 Uiso 1 1 calc R
C24 C 0.2253(3) 0.3372(2) 0.1622(5) 0.0306(14) Uani 1 1 d .
N1A N -0.1920(2) 0.2441(2) 0.6601(4) 0.0329(11) Uani 1 1 d .
N2 N 0.2457(2) 0.6613(2) -0.1813(4) 0.0357(12) Uiso 1 1 d .
O1 O 0.17862(16) 0.21404(18) 0.3749(3) 0.0362(10) Uani 1 1 d .
O2 O 0.13335(19) 0.2212(2) 0.2227(4) 0.0506(13) Uani 1 1 d .
O3 O 0.20619(19) 0.33654(16) 0.2532(4) 0.0437(10) Uani 1 1 d .
O4 O 0.25058(19) 0.29206(16) 0.1230(3) 0.0372(10) Uani 1 1 d .
O5 O 0.1278(8) 0.4609(8) -0.3229(15) 0.296(7) Uiso 1 1 d D
C25 C 0.1334(13) 0.4108(10) -0.263(2) 0.296(7) Uiso 1 1 d D
C26 C 0.1075(14) 0.4286(12) -0.164(2) 0.296(7) Uiso 1 1 d D
O6 O 0.1246(10) 0.5670(9) 0.3353(14) 0.310(8) Uiso 1 1 d D
C27 C 0.1212(14) 0.5898(12) 0.437(2) 0.310(8) Uiso 1 1 d D
C28 C 0.1414(12) 0.5300(13) 0.452(2) 0.310(8) Uiso 1 1 d D
O7 O -0.0038(8) 0.1108(8) 0.7898(13) 0.131(5) Uiso 0.50 1 d PD
C29 C -0.0337(10) 0.0795(11) 0.8693(19) 0.131(5) Uiso 0.50 1 d PD
C30 C -0.0985(11) 0.0699(12) 0.864(2) 0.131(5) Uiso 0.50 1 d PD
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
O1 Co1 O4 152.67(17) . .
O1 Co1 N1A 98.14(18) . 6_556
O4 Co1 N1A 99.39(18) . 6_556
O1 Co1 N2 102.45(19) . 5_545
O4 Co1 N2 94.94(18) . 5_545
N1A Co1 N2 100.0(2) 6_556 5_545
O1 Co1 O3 97.62(17) . .
O4 Co1 O3 60.61(17) . .
N1A Co1 O3 93.36(18) 6_556 .
N2 Co1 O3 153.91(19) 5_545 .
O1 Co1 O2 59.90(16) . .
O4 Co1 O2 99.80(17) . .
N1A Co1 O2 157.66(18) 6_556 .
N2 Co1 O2 89.59(19) 5_545 .
O3 Co1 O2 86.18(17) . .
O1 Co1 C24 125.11(18) . .
O4 Co1 C24 30.94(18) . .
N1A Co1 C24 98.85(19) 6_556 .
N2 Co1 C24 125.0(2) 5_545 .
O3 Co1 C24 29.74(17) . .
O2 Co1 C24 91.80(18) . .
O1 Co1 C12 30.31(18) . .
O4 Co1 C12 126.36(19) . .
N1A Co1 C12 128.0(2) 6_556 .
N2 Co1 C12 99.21(19) 5_545 .
O3 Co1 C12 89.75(18) . .
O2 Co1 C12 29.77(18) . .
C24 Co1 C12 108.4(2) . .
N1A C1 C2 124.4(6) . .
C3 C2 C1 117.8(6) . .
C4 C3 C2 119.3(6) . .
C4 C3 C6 121.4(6) . .
C2 C3 C6 119.0(6) . .
C3 C4 C5 118.4(6) . .
N1A C5 C4 123.6(6) . .
C7 C6 C11 118.1(6) . .
C7 C6 C3 121.6(6) . .
C11 C6 C3 120.3(6) . .
C8 C7 C6 121.0(6) . .
C7 C8 C9 120.6(7) . .
C10 C9 C8 120.2(6) . .
C10 C9 C12 118.9(5) . .
C8 C9 C12 120.6(6) . .
C9 C10 C11 120.2(6) . .
C6 C11 C10 119.7(6) . .
O2 C12 O1 123.0(6) . .
O2 C12 C9 118.8(6) . .
O1 C12 C9 118.2(5) . .
O2 C12 Co1 67.8(3) . .
O1 C12 Co1 55.7(3) . .
C9 C12 Co1 168.7(4) . .
N2 C13 C14 122.7(6) . .
C13 C14 C15 120.3(6) . .
C16 C15 C14 116.9(6) . .
C16 C15 C18 119.7(6) . .
C14 C15 C18 123.4(5) . .
C15 C16 C17 120.1(6) . .
N2 C17 C16 121.8(6) . .
C23 C18 C19 118.4(6) . .
C23 C18 C15 121.8(5) . .
C19 C18 C15 119.7(6) . .
C20 C19 C18 121.7(7) . .
C19 C20 C21 119.6(6) . .
C20 C21 C22 119.6(6) . .
C20 C21 C24 120.2(5) . .
C22 C21 C24 120.2(6) . .
C21 C22 C23 120.1(6) . .
C18 C23 C22 120.7(6) . .
O3 C24 O4 120.9(5) . .
O3 C24 C21 121.2(5) . .
O4 C24 C21 117.7(6) . .
O3 C24 Co1 64.8(3) . .
O4 C24 Co1 56.3(3) . .
C21 C24 Co1 174.0(5) . .
C1 N1A C5 116.3(5) . .
C1 N1A Co1 122.5(4) . 6_456
C5 N1A Co1 121.1(4) . 6_456
C17 N2 C13 118.0(5) . .
C17 N2 Co1 119.1(4) . 5
C13 N2 Co1 122.5(4) . 5
C12 O1 Co1 94.0(4) . .
C12 O2 Co1 82.4(4) . .
C24 O3 Co1 85.5(3) . .
C24 O4 Co1 92.7(4) . .
O5 C25 C26 102(2) . .
C27 O6 C28 53.3(11) . .
O6 C27 C28 76.0(18) . .
C27 C28 O6 50.7(11) . .
O7 C29 C30 121(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.055(4) .
Co1 O4 2.065(4) .
Co1 N1A 2.072(5) 6_556
Co1 N2 2.085(5) 5_545
Co1 O3 2.249(4) .
Co1 O2 2.317(4) .
Co1 C24 2.479(6) .
Co1 C12 2.481(6) .
C1 N1A 1.309(8) .
C1 C2 1.412(9) .
C2 C3 1.384(9) .
C3 C4 1.372(9) .
C3 C6 1.490(9) .
C4 C5 1.393(8) .
C5 N1A 1.366(7) .
C6 C7 1.390(9) .
C6 C11 1.395(9) .
C7 C8 1.367(9) .
C8 C9 1.373(9) .
C9 C10 1.356(9) .
C9 C12 1.542(8) .
C10 C11 1.409(9) .
C12 O2 1.242(8) .
C12 O1 1.255(7) .
C13 N2 1.337(8) .
C13 C14 1.371(8) .
C14 C15 1.379(9) .
C15 C16 1.370(8) .
C15 C18 1.484(8) .
C16 C17 1.406(9) .
C17 N2 1.324(8) .
C18 C23 1.367(9) .
C18 C19 1.407(9) .
C19 C20 1.382(8) .
C20 C21 1.384(9) .
C21 C22 1.393(8) .
C21 C24 1.493(8) .
C22 C23 1.408(9) .
C24 O3 1.234(7) .
C24 O4 1.276(7) .
N1A Co1 2.072(5) 6_456
N2 Co1 2.085(5) 5
O5 C25 1.371(17) .
C25 C26 1.445(18) .
O6 C27 1.394(17) .
O6 C28 1.75(3) .
C27 C28 1.445(18) .
O7 C29 1.410(17) .
C29 C30 1.485(17) .
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 0.500 0.269 186 54 ' '
2 0.000 0.000 -0.042 366 94 ' '
3 0.500 0.500 0.041 366 94 ' '
4 0.500 0.000 -0.269 186 54 ' '
