#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:33:06 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179066 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/28/4302803.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_4302803
loop_
_publ_author_name
'Ming-Hua Zeng'
'Sheng Hu'
'Qing Chen'
'Gang Xie'
'Qi Shuai'
'Sheng-Li Gao'
_publ_contact_author             'prof.MING HUA ZENG '
_publ_contact_author_email       ZMH@MAIBOX.GXNU.EDU.CN
_publ_section_title
;
Apical Ligand Substitution, Shape Recognition, Vapor-Adsorption Phenomenon,
and Microcalorimetry for a Pillared Bilayer Porous Framework That Shrinks
or Expands in Crystal-to-Crystal Manners upon Change in the Cobalt(II)
Coordination Environment
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7070
_journal_page_last               7079
_journal_paper_doi               10.1021/ic801794e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C14 H13 Co N2 O5, H2 O'
_chemical_formula_sum            'C14 H15 Co N2 O6'
_chemical_formula_weight         366.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 105.609(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3072(19)
_cell_length_b                   7.7045(12)
_cell_length_c                   15.867(2)
_cell_measurement_reflns_used    2306
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      1.7
_cell_volume                     1449.0(4)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8323
_diffrn_reflns_theta_full        27.06
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    1.219
_exptl_absorpt_correction_T_max  0.8479
_exptl_absorpt_correction_T_min  0.7266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0407P)²+1.5841P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                2306
_reflns_number_total             3166
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801794e_si_002_08.cif
_cod_data_source_block           3h
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4302803
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.29952(3) 0.48788(5) 0.18183(2) 0.02003(12) Uani 1 1 d . . .
O1 O 0.36406(18) 0.2411(2) 0.18454(13) 0.0274(5) Uani 1 1 d . . .
O2 O 0.2900(2) 0.3333(3) 0.05126(14) 0.0354(5) Uani 1 1 d . . .
O3 O 0.32610(19) -0.0528(3) -0.19381(12) 0.0305(5) Uani 1 1 d . . .
O4 O 0.37573(19) -0.3299(3) -0.16856(13) 0.0329(5) Uani 1 1 d . . .
N1 N 0.45073(19) -0.3910(3) 0.16205(14) 0.0208(5) Uani 1 1 d . . .
H1A H 0.4579 -0.4950 0.1447 0.025 Uiso 1 1 calc R . .
H1B H 0.4596 -0.3704 0.2168 0.025 Uiso 1 1 calc R . .
N2 N 0.1789(2) 0.6667(3) 0.11453(15) 0.0260(6) Uani 1 1 d . . .
C1 C 0.3658(2) 0.0445(3) 0.06930(17) 0.0184(6) Uani 1 1 d . . .
C2 C 0.3508(2) 0.0145(3) -0.01938(17) 0.0201(6) Uani 1 1 d . . .
H2 H 0.3256 0.1035 -0.0595 0.024 Uiso 1 1 calc R . .
C3 C 0.3735(2) -0.1478(3) -0.04801(17) 0.0185(6) Uani 1 1 d . . .
C4 C 0.4092(2) -0.2817(4) 0.01185(17) 0.0204(6) Uani 1 1 d . . .
H4 H 0.4231 -0.3911 -0.0077 0.025 Uiso 1 1 calc R . .
C5 C 0.4240(2) -0.2528(3) 0.10021(16) 0.0180(6) Uani 1 1 d . . .
C6 C 0.4034(2) -0.0891(4) 0.12875(17) 0.0191(6) Uani 1 1 d . . .
H6 H 0.4149 -0.0686 0.1883 0.023 Uiso 1 1 calc R . .
C7 C 0.3382(2) 0.2166(4) 0.10237(19) 0.0224(6) Uani 1 1 d . . .
C8 C 0.3584(2) -0.1817(4) -0.14398(17) 0.0208(6) Uani 1 1 d . . .
C9 C 0.1656(3) 0.8166(4) 0.1526(2) 0.0312(7) Uani 1 1 d . . .
H9 H 0.2047 0.8328 0.2110 0.037 Uiso 1 1 calc R . .
C10 C 0.0968(3) 0.9491(4) 0.1100(2) 0.0294(7) Uani 1 1 d . . .
H10 H 0.0911 1.0514 0.1396 0.035 Uiso 1 1 calc R . .
C11 C 0.0370(3) 0.9305(4) 0.0242(2) 0.0282(7) Uani 1 1 d . . .
C12 C 0.0497(4) 0.7732(5) -0.0143(2) 0.0709(16) Uani 1 1 d . . .
H12 H 0.0090 0.7516 -0.0718 0.085 Uiso 1 1 calc R . .
C13 C 0.1219(4) 0.6485(5) 0.0314(2) 0.0575(12) Uani 1 1 d . . .
H13 H 0.1310 0.5466 0.0026 0.069 Uiso 1 1 calc R . .
O5 O 0.15701(19) 0.3353(3) 0.21409(15) 0.0368(5) Uani 1 1 d . . .
H5 H 0.1936 0.2680 0.2510 0.044 Uiso 1 1 calc R . .
C14 C 0.0743(3) 0.4186(6) 0.2471(3) 0.0605(12) Uani 1 1 d . . .
H14A H 0.0310 0.3327 0.2676 0.091 Uiso 1 1 calc R . .
H14B H 0.0253 0.4857 0.2014 0.091 Uiso 1 1 calc R . .
H14C H 0.1107 0.4937 0.2946 0.091 Uiso 1 1 calc R . .
O1W O 0.2312(3) 0.3974(4) -0.14452(18) 0.0637(8) Uani 1 1 d . . .
H1WA H 0.2727 0.4783 -0.1554 0.096 Uiso 1 1 d R . .
H1WB H 0.2332 0.4084 -0.0908 0.096 Uiso 1 1 d 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'
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
O3 Co1 O1 104.71(8) 4_566 . ?
O3 Co1 N2 104.29(9) 4_566 . ?
O1 Co1 N2 146.64(9) . . ?
O3 Co1 N1 96.73(9) 4_566 1_565 ?
O1 Co1 N1 93.37(8) . 1_565 ?
N2 Co1 N1 99.25(9) . 1_565 ?
O3 Co1 O5 80.62(8) 4_566 . ?
O1 Co1 O5 80.50(8) . . ?
N2 Co1 O5 88.32(9) . . ?
N1 Co1 O5 172.39(8) 1_565 . ?
O3 Co1 O2 163.39(8) 4_566 . ?
O1 Co1 O2 58.72(7) . . ?
N2 Co1 O2 91.32(8) . . ?
N1 Co1 O2 86.13(8) 1_565 . ?
O5 Co1 O2 94.42(8) . . ?
C7 O1 Co1 97.33(17) . . ?
C7 O2 Co1 83.74(17) . . ?
C8 O3 Co1 139.69(19) . 4_565 ?
C5 N1 Co1 111.80(17) . 1_545 ?
C5 N1 H1A 120.0 . . ?
Co1 N1 H1A 79.2 1_545 . ?
C5 N1 H1B 120.0 . . ?
Co1 N1 H1B 79.4 1_545 . ?
H1A N1 H1B 120.0 . . ?
C13 N2 C9 116.5(3) . . ?
C13 N2 Co1 123.4(2) . . ?
C9 N2 Co1 119.63(19) . . ?
C2 C1 C6 119.6(2) . . ?
C2 C1 C7 121.4(2) . . ?
C6 C1 C7 118.9(2) . . ?
C3 C2 C1 119.9(2) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 120.0(2) . . ?
C2 C3 C8 120.5(2) . . ?
C4 C3 C8 119.5(2) . . ?
C5 C4 C3 120.3(2) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 119.5(2) . . ?
C4 C5 N1 121.4(2) . . ?
C6 C5 N1 118.9(2) . . ?
C5 C6 C1 120.6(2) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
O2 C7 O1 120.2(3) . . ?
O2 C7 C1 121.5(3) . . ?
O1 C7 C1 118.2(2) . . ?
O4 C8 O3 125.2(3) . . ?
O4 C8 C3 119.4(2) . . ?
O3 C8 C3 115.3(2) . . ?
N2 C9 C10 123.4(3) . . ?
N2 C9 H9 118.3 . . ?
C10 C9 H9 118.3 . . ?
C11 C10 C9 120.3(3) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 115.9(3) . . ?
C10 C11 C11 122.1(3) . 3_575 ?
C12 C11 C11 122.1(4) . 3_575 ?
C13 C12 C11 120.8(3) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
N2 C13 C12 123.1(3) . . ?
N2 C13 H13 118.5 . . ?
C12 C13 H13 118.5 . . ?
C14 O5 Co1 121.4(2) . . ?
C14 O5 H5 109.5 . . ?
Co1 O5 H5 100.3 . . ?
O5 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
H1WA O1W H1WB 105.9 . . ?
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 O3 1.9756(19) 4_566 ?
Co1 O1 2.0563(19) . ?
Co1 N2 2.095(2) . ?
Co1 N1 2.179(2) 1_565 ?
Co1 O5 2.281(2) . ?
Co1 O2 2.365(2) . ?
O1 C7 1.270(3) . ?
O2 C7 1.249(3) . ?
O3 C8 1.265(3) . ?
O3 Co1 1.9756(19) 4_565 ?
O4 C8 1.243(3) . ?
N1 C5 1.425(3) . ?
N1 Co1 2.179(2) 1_545 ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N2 C13 1.324(4) . ?
N2 C9 1.334(4) . ?
C1 C2 1.388(4) . ?
C1 C6 1.389(4) . ?
C1 C7 1.499(4) . ?
C2 C3 1.384(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.391(4) . ?
C3 C8 1.507(4) . ?
C4 C5 1.382(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.386(4) . ?
C6 H6 0.9300 . ?
C9 C10 1.382(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.369(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.385(5) . ?
C11 C11 1.480(6) 3_575 ?
C12 C13 1.375(5) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
O5 C14 1.417(4) . ?
O5 H5 0.8200 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
O1W H1WA 0.8522 . ?
O1W H1WB 0.8498 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O4 0.86 2.40 3.013(3) 129.2 3_645
N1 H1A O1 0.86 2.50 3.083(3) 125.6 1_545
N1 H1A O2 0.86 2.56 3.106(3) 122.0 1_545
N1 H1B O1 0.86 2.46 3.028(3) 123.9 2_645
O5 H5 O1W 0.82 2.04 2.825(4) 159.2 4_566
O1W H1WA O4 0.85 1.99 2.844(4) 174.5 1_565
O1W H1WB O2 0.85 2.25 3.034(4) 153.7 .
