#------------------------------------------------------------------------------
#$Date: 2019-11-24 04:12:18 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236652 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/00/03/8000358.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_8000358
loop_
_publ_author_name
'Andrzejewski, Michał'
'Katrusiak, Andrzej'
_publ_section_title
;
 Piezochromic Porous Metal-Organic Framework.
;
_journal_issue                   1
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              279
_journal_page_last               284
_journal_paper_doi               10.1021/acs.jpclett.6b02458
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C14 H18 Co N2 O5'
_chemical_formula_sum            'C14 H18 Co N2 O5'
_chemical_formula_weight         353.23
_chemical_name_common            AMU1
_chemical_name_systematic
;
Co(1,4-benzenedicarboxylate)(1,4-diazabicyclo[2.2.2]octane)H2O
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           6
_space_group_name_Hall           'P -2y'
_space_group_name_H-M_alt        'P 1 m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.052(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   6.1006(2)
_cell_length_b                   7.0942(2)
_cell_length_c                   10.6767(2)
_cell_measurement_reflns_used    2382
_cell_measurement_temperature    273
_cell_measurement_theta_max      58.17
_cell_measurement_theta_min      5.74
_cell_volume                     460.28(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7131
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.085
_diffrn_reflns_theta_min         2.871
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Data were collected and reduced by program CrysAlisPro, 
and SCALE3 ABSPACK was used for absorption correction
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       plate
_exptl_crystal_F_000             183
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.148
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         2382
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0735P)²+0.2419P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1286
_reflns_Friedel_coverage         0.993
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                2227
_reflns_number_total             2382
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jz6b02458_si_004.cif
_cod_data_source_block           273K_Pm
_cod_database_code               8000358
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O1W-H1WA
 0.96 with sigma of 0.02
 H1WB-H1WA
 1.66 with sigma of 0.02
 O1W-H1WB
 0.97 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C6) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma
for terminal atoms of 0.002
4. Others
 Fixed X: H1WB(0.421281)
 Fixed Y: H1WB(0)
 Fixed Z: H1WB(0.06267)
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B), C11(H11A,H11B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C5(H5), C3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 0.00028(8) 0.0000 0.00446(7) 0.0195(3) Uani 1 2 d S T P
C6 C 0.0027(18) 0.0000 0.4467(11) 0.034(2) Uani 1 2 d S TU P
H6 H 0.1455 0.0000 0.4226 0.040 Uiso 1 2 calc RS T P
O2 O -0.2783(10) 0.0000 0.1356(5) 0.0324(14) Uani 1 2 d S T P
O1 O 0.0694(12) 0.0000 0.1988(7) 0.0260(16) Uani 1 2 d S T P
N1 N -0.0045(15) 0.3161(5) -0.0011(8) 0.0211(8) Uani 1 1 d . . .
O4 O -0.1298(13) 0.0000 0.8248(7) 0.0297(17) Uani 1 2 d S T P
C7 C -0.1271(14) 0.0000 0.2249(7) 0.0274(17) Uani 1 2 d S T P
C10 C -0.2268(10) 0.3909(8) -0.0018(7) 0.0352(14) Uani 1 1 d . . .
H10A H -0.2933 0.3456 0.0718 0.042 Uiso 1 1 calc R . .
H10B H -0.3147 0.3456 -0.0758 0.042 Uiso 1 1 calc R . .
C4 C -0.2483(14) 0.0000 0.6112(8) 0.0282(17) Uani 1 2 d S TU P
C2 C -0.3904(16) 0.0000 0.3928(10) 0.039(2) Uani 1 2 d S TU P
H2 H -0.5098 0.0000 0.3323 0.047 Uiso 1 2 calc RS T P
C5 C -0.038(2) 0.0000 0.5753(14) 0.053(4) Uani 1 2 d S TU P
H5 H 0.0804 0.0000 0.6366 0.064 Uiso 1 2 calc RS T P
C1 C -0.1751(13) 0.0000 0.3588(8) 0.0259(16) Uani 1 2 d S TU P
C8 C -0.2918(13) 0.0000 0.7501(7) 0.0327(19) Uani 1 2 d S T P
C3 C -0.4207(16) 0.0000 0.5210(10) 0.039(2) Uani 1 2 d S TU P
H3 H -0.5632 0.0000 0.5456 0.047 Uiso 1 2 calc RS T P
O3 O -0.4856(16) 0.0000 0.7733(9) 0.070(3) Uani 1 2 d S TU P
C9 C 0.0942(11) 0.3905(9) -0.1133(6) 0.0329(14) Uani 1 1 d . . .
H9A H 0.0111 0.3449 -0.1889 0.039 Uiso 1 1 calc R . .
H9B H 0.2441 0.3449 -0.1136 0.039 Uiso 1 1 calc R . .
C11 C 0.1296(12) 0.3916(8) 0.1116(6) 0.0340(14) Uani 1 1 d . . .
H11A H 0.2796 0.3461 0.1118 0.041 Uiso 1 1 calc R . .
H11B H 0.0701 0.3461 0.1872 0.041 Uiso 1 1 calc R . .
O1W O 0.3351(9) 0.0000 -0.0172(5) 0.0288(13) Uani 1 2 d DS T P
H1WA H 0.409(12) 0.0000 -0.093(3) 0.10(6) Uiso 1 2 d DS T P
H1WB H 0.4213 0.0000 0.0627 2(2) Uiso 1 2 d DS T P
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'
Co Co 0.3494 0.9721 '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'
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 O2 59.2(2) . .
O1 Co1 N1 91.6(2) . 2
O1 Co1 N1 91.6(2) . .
N1 Co1 O2 90.4(2) . .
N1 Co1 O2 90.4(2) 2 .
N1 Co1 N1 176.7(4) . 2
O4 Co1 O2 109.3(3) 1_554 .
O4 Co1 O1 168.5(3) 1_554 .
O4 Co1 N1 88.4(2) 1_554 .
O4 Co1 N1 88.4(2) 1_554 2
O4 Co1 O1W 101.7(3) 1_554 .
O1W Co1 O2 149.0(2) . .
O1W Co1 O1 89.8(3) . .
O1W Co1 N1 90.4(2) . 2
O1W Co1 N1 90.4(2) . .
C5 C6 H6 121.0 . .
C1 C6 H6 121.0 . .
C1 C6 C5 117.9(9) . .
C7 O2 Co1 86.0(5) . .
C7 O1 Co1 96.2(6) . .
C10 N1 Co1 112.0(4) . .
C10 N1 C9 108.1(6) . .
C10 N1 C11 108.5(6) . .
C9 N1 Co1 111.8(4) . .
C9 N1 C11 106.9(6) . .
C11 N1 Co1 109.4(4) . .
C8 O4 Co1 149.0(7) . 1_556
O2 C7 C1 122.2(7) . .
O1 C7 O2 118.7(8) . .
O1 C7 C1 119.1(8) . .
N1 C10 C10 111.4(3) . 2_565
N1 C10 H10A 109.4 . .
N1 C10 H10B 109.4 . .
C10 C10 H10A 109.4 2_565 .
C10 C10 H10B 109.4 2_565 .
H10A C10 H10B 108.0 . .
C5 C4 C8 121.1(9) . .
C3 C4 C5 119.1(10) . .
C3 C4 C8 119.8(8) . .
C1 C2 H2 121.2 . .
C1 C2 C3 117.6(9) . .
C3 C2 H2 121.2 . .
C6 C5 H5 119.4 . .
C4 C5 C6 121.2(11) . .
C4 C5 H5 119.4 . .
C6 C1 C7 116.6(8) . .
C6 C1 C2 122.0(8) . .
C2 C1 C7 121.4(8) . .
O4 C8 C4 115.9(8) . .
O4 C8 O3 127.6(9) . .
O3 C8 C4 116.6(8) . .
C4 C3 C2 122.1(9) . .
C4 C3 H3 118.9 . .
C2 C3 H3 118.9 . .
N1 C9 C9 110.8(3) . 2_565
N1 C9 H9A 109.5 . .
N1 C9 H9B 109.5 . .
C9 C9 H9A 109.5 2_565 .
C9 C9 H9B 109.5 2_565 .
H9A C9 H9B 108.1 . .
N1 C11 C11 111.0(3) . 2_565
N1 C11 H11A 109.4 . .
N1 C11 H11B 109.4 . .
C11 C11 H11A 109.4 2_565 .
C11 C11 H11B 109.4 2_565 .
H11A C11 H11B 108.0 . .
Co1 O1W H1WA 129(4) . .
Co1 O1W H1WB 111.5(4) . .
H1WA O1W H1WB 119(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 2.295(6) .
Co1 O1 2.081(8) .
Co1 N1 2.244(4) 2
Co1 N1 2.244(4) .
Co1 O4 2.011(8) 1_554
Co1 O1W 2.076(5) .
C6 H6 0.9300 .
C6 C5 1.417(14) .
C6 C1 1.370(14) .
O2 C7 1.267(10) .
O1 C7 1.255(10) .
N1 C10 1.456(10) .
N1 C9 1.484(10) .
N1 C11 1.494(10) .
O4 Co1 2.011(8) 1_556
O4 C8 1.214(12) .
C7 C1 1.485(11) .
C10 C10 1.547(12) 2_565
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C4 C5 1.371(16) .
C4 C8 1.530(11) .
C4 C3 1.362(13) .
C2 H2 0.9300 .
C2 C1 1.393(13) .
C2 C3 1.397(13) .
C5 H5 0.9300 .
C8 O3 1.229(12) .
C3 H3 0.9300 .
C9 C9 1.553(13) 2_565
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C11 C11 1.538(11) 2_565
C11 H11A 0.9700 .
C11 H11B 0.9700 .
O1W H1WA 0.96(3) .
O1W H1WB 0.962(6) .
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_4
Co1 O2 C7 O1 0.000(1) . .
Co1 O2 C7 C1 180.000(1) . .
Co1 O1 C7 O2 0.000(1) . .
Co1 O1 C7 C1 180.000(1) . .
Co1 N1 C10 C10 178.4(2) . 2_565
Co1 N1 C9 C9 -178.6(2) . 2_565
Co1 N1 C11 C11 -179.7(2) . 2_565
Co1 O4 C8 C4 180.000(4) 1_556 .
Co1 O4 C8 O3 0.000(7) 1_556 .
O2 C7 C1 C6 180.000(2) . .
O2 C7 C1 C2 0.000(2) . .
O1 C7 C1 C6 0.000(2) . .
O1 C7 C1 C2 180.000(2) . .
C10 N1 C9 C9 57.7(5) . 2_565
C10 N1 C11 C11 -57.3(6) . 2_565
C5 C6 C1 C7 180.000(2) . .
C5 C6 C1 C2 0.000(3) . .
C5 C4 C8 O4 0.000(3) . .
C5 C4 C8 O3 180.000(4) . .
C5 C4 C3 C2 0.000(3) . .
C1 C6 C5 C4 0.000(3) . .
C1 C2 C3 C4 0.000(3) . .
C8 C4 C5 C6 180.000(3) . .
C8 C4 C3 C2 180.000(3) . .
C3 C4 C5 C6 0.000(4) . .
C3 C4 C8 O4 180.000(3) . .
C3 C4 C8 O3 0.000(4) . .
C3 C2 C1 C6 0.000(3) . .
C3 C2 C1 C7 180.000(2) . .
C9 N1 C10 C10 -58.0(5) . 2_565
C9 N1 C11 C11 59.0(5) . 2_565
C11 N1 C10 C10 57.5(6) . 2_565
C11 N1 C9 C9 -58.9(5) . 2_565
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 -0.144 0.500 0.501 144.9 54.3
