#------------------------------------------------------------------------------
#$Date: 2019-11-24 04:12:18 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236652 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/00/03/8000359.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_8000359
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     direct
_audit_creation_date             2016-07-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.090(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   6.0947(2)
_cell_length_b                   7.0901(2)
_cell_length_c                   10.6768(2)
_cell_measurement_reflns_used    2375
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      58.21
_cell_measurement_theta_min      5.75
_cell_volume                     459.55(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.932
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_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            7095
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.103
_diffrn_reflns_theta_min         2.873
_exptl_absorpt_coefficient_mu    0.954
_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    1.276
_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         1.117
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.115
_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   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2375
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      5.220
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0511
_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)+(0.0759P)²+0.2230P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.993
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.932
_reflns_number_gt                2228
_reflns_number_total             2375
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jz6b02458_si_004.cif
_cod_data_source_block           250K_Pm
_cod_database_code               8000359
_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
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H1WB-O1W
 0.96 with sigma of 0.001
 H1WA-H1WB
 1.44 with sigma of 0.02
 H1WA-O1W
 0.96 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5)
5.a Rotating group:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C6(H6), C5(H5)
;
_shelx_shelxl_version_number     2014/7
_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 0.00000(8) 0.0000 0.00000(7) 0.0185(3) Uani 1 2 d S T P
O1 O 0.0704(12) 0.0000 0.1948(7) 0.0226(15) Uani 1 2 d S TU P
O2 O -0.2769(10) 0.0000 0.1309(5) 0.0307(14) Uani 1 2 d S T P
N1 N -0.0046(15) 0.3155(5) -0.0059(8) 0.0199(8) Uani 1 1 d . . .
C7 C -0.1268(13) 0.0000 0.2212(7) 0.0239(16) Uani 1 2 d S T P
C1 C -0.1757(13) 0.0000 0.3542(8) 0.0248(16) Uani 1 2 d S TU P
C9 C 0.0961(12) 0.3904(9) -0.1179(6) 0.0325(14) Uani 1 1 d . . .
H9A H 0.0139 0.3448 -0.1938 0.039 Uiso 1 1 calc R . .
H9B H 0.2463 0.3448 -0.1175 0.039 Uiso 1 1 calc R . .
C10 C -0.2282(10) 0.3914(8) -0.0062(7) 0.0326(13) Uani 1 1 d . . .
H10A H -0.2945 0.3461 0.0675 0.039 Uiso 1 1 calc R . .
H10B H -0.3167 0.3461 -0.0801 0.039 Uiso 1 1 calc R . .
C3 C -0.4223(16) 0.0000 0.5162(10) 0.037(2) Uani 1 2 d S TU P
H3 H -0.5652 0.0000 0.5404 0.044 Uiso 1 2 calc RS T P
C2 C -0.3906(17) 0.0000 0.3876(10) 0.040(2) Uani 1 2 d S TU P
H2 H -0.5097 0.0000 0.3268 0.048 Uiso 1 2 calc RS T P
C6 C 0.0028(18) 0.0000 0.4422(10) 0.031(2) Uani 1 2 d S TU P
H6 H 0.1461 0.0000 0.4187 0.037 Uiso 1 2 calc RS T P
O4 O -0.1315(13) 0.0000 0.8202(7) 0.0290(16) Uani 1 2 d S T P
C4 C -0.2507(14) 0.0000 0.6063(8) 0.0276(17) Uani 1 2 d S TU P
C8 C -0.2911(14) 0.0000 0.7456(8) 0.0322(19) Uani 1 2 d S T P
O3 O -0.4853(17) 0.0000 0.7688(10) 0.071(3) Uani 1 2 d S TU P
C5 C -0.041(3) 0.0000 0.5718(15) 0.055(4) Uani 1 2 d S TU P
H5 H 0.0764 0.0000 0.6337 0.066 Uiso 1 2 calc RS T P
C11 C 0.1299(12) 0.3911(8) 0.1071(6) 0.0319(14) Uani 1 1 d . . .
H11A H 0.2800 0.3455 0.1074 0.038 Uiso 1 1 calc R . .
H11B H 0.0702 0.3455 0.1827 0.038 Uiso 1 1 calc R . .
O1W O 0.3335(9) 0.0000 -0.0225(5) 0.0281(13) Uani 1 2 d DS T P
H1WA H 0.4051 0.0176 0.0370 0.042 Uiso 0.5 1 d DGR . .
H1WB H 0.3560 0.0171 -0.1009 0.042 Uiso 0.5 1 d DGR . .
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 91.7(2) . .
O1 Co1 N1 91.7(2) . 2
N1 Co1 O2 90.5(2) 2 .
N1 Co1 O2 90.5(2) . .
N1 Co1 N1 176.6(4) 2 .
O4 Co1 O1 168.5(3) 1_554 .
O4 Co1 O2 109.3(3) 1_554 .
O4 Co1 N1 88.3(2) 1_554 2
O4 Co1 N1 88.3(2) 1_554 .
O4 Co1 O1W 101.6(3) 1_554 .
O1W Co1 O1 89.9(3) . .
O1W Co1 O2 149.1(2) . .
O1W Co1 N1 90.4(2) . .
O1W Co1 N1 90.4(2) . 2
C7 O1 Co1 96.1(6) . .
C7 O2 Co1 86.7(5) . .
C9 N1 Co1 111.9(5) . .
C9 N1 C11 106.5(6) . .
C10 N1 Co1 112.1(4) . .
C10 N1 C9 108.5(6) . .
C10 N1 C11 108.3(6) . .
C11 N1 Co1 109.3(4) . .
O1 C7 O2 118.0(7) . .
O1 C7 C1 119.6(8) . .
O2 C7 C1 122.5(7) . .
C2 C1 C7 121.5(8) . .
C6 C1 C7 116.3(8) . .
C6 C1 C2 122.2(8) . .
N1 C9 C9 110.9(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 C10 C10 111.5(3) . 2_565
N1 C10 H10A 109.3 . .
N1 C10 H10B 109.3 . .
C10 C10 H10A 109.3 2_565 .
C10 C10 H10B 109.3 2_565 .
H10A C10 H10B 108.0 . .
C2 C3 H3 119.0 . .
C4 C3 H3 119.0 . .
C4 C3 C2 122.0(9) . .
C1 C2 C3 117.8(9) . .
C1 C2 H2 121.1 . .
C3 C2 H2 121.1 . .
C1 C6 H6 121.4 . .
C1 C6 C5 117.2(10) . .
C5 C6 H6 121.4 . .
C8 O4 Co1 149.6(7) . 1_556
C3 C4 C8 120.6(8) . .
C3 C4 C5 119.4(11) . .
C5 C4 C8 120.0(10) . .
O4 C8 C4 117.0(8) . .
O4 C8 O3 127.1(9) . .
O3 C8 C4 115.9(8) . .
C6 C5 H5 119.3 . .
C4 C5 C6 121.5(11) . .
C4 C5 H5 119.3 . .
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 113.9 . .
Co1 O1W H1WB 110.7 . .
H1WA O1W H1WB 131.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.086(7) .
Co1 O2 2.285(6) .
Co1 N1 2.238(4) 2
Co1 N1 2.238(4) .
Co1 O4 2.013(7) 1_554
Co1 O1W 2.068(6) .
O1 C7 1.259(10) .
O2 C7 1.268(10) .
N1 C9 1.490(11) .
N1 C10 1.465(10) .
N1 C11 1.496(9) .
C7 C1 1.477(11) .
C1 C2 1.388(13) .
C1 C6 1.373(13) .
C9 C9 1.554(13) 2_565
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 C10 1.540(12) 2_565
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C3 H3 0.9300 .
C3 C2 1.403(14) .
C3 C4 1.357(13) .
C2 H2 0.9300 .
C6 H6 0.9300 .
C6 C5 1.432(15) .
O4 Co1 2.013(7) 1_556
O4 C8 1.202(11) .
C4 C8 1.529(11) .
C4 C5 1.361(17) .
C8 O3 1.230(13) .
C5 H5 0.9300 .
C11 C11 1.545(11) 2_565
C11 H11A 0.9700 .
C11 H11B 0.9700 .
O1W H1WA 0.7491 .
O1W H1WB 0.8682 .
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 O1 C7 O2 0.000(1) . .
Co1 O1 C7 C1 180.000(1) . .
Co1 O2 C7 O1 0.000(1) . .
Co1 O2 C7 C1 180.000(1) . .
Co1 N1 C9 C9 -178.6(2) . 2_565
Co1 N1 C10 C10 178.3(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(8) 1_556 .
O1 C7 C1 C2 180.000(2) . .
O1 C7 C1 C6 0.000(2) . .
O2 C7 C1 C2 0.000(2) . .
O2 C7 C1 C6 180.000(2) . .
C7 C1 C2 C3 180.000(2) . .
C7 C1 C6 C5 180.000(3) . .
C1 C6 C5 C4 0.000(3) . .
C9 N1 C10 C10 -57.6(5) . 2_565
C9 N1 C11 C11 59.2(5) . 2_565
C10 N1 C9 C9 57.2(5) . 2_565
C10 N1 C11 C11 -57.2(6) . 2_565
C3 C4 C8 O4 180.000(3) . .
C3 C4 C8 O3 0.000(4) . .
C3 C4 C5 C6 0.000(4) . .
C2 C1 C6 C5 0.000(3) . .
C2 C3 C4 C8 180.000(3) . .
C2 C3 C4 C5 0.000(4) . .
C6 C1 C2 C3 0.000(3) . .
C4 C3 C2 C1 0.000(3) . .
C8 C4 C5 C6 180.000(3) . .
C5 C4 C8 O4 0.000(4) . .
C5 C4 C8 O3 180.000(4) . .
C11 N1 C9 C9 -59.1(5) . 2_565
C11 N1 C10 C10 57.6(6) . 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 -0.736 0.500 0.496 144.7 56.6
