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#$Date: 2019-11-25 16:51:11 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241372 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/10/4131069.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_4131069
loop_
_publ_author_name
'Taylor, Mercedes K.'
'Runčevski, Tomče'
'Oktawiec, Julia'
'Gonzalez, Miguel I.'
'Siegelman, Rebecca L.'
'Mason, Jarad A.'
'Ye, Jinxing'
'Brown, Craig M.'
'Long, Jeffrey R.'
_publ_section_title
;
 Tuning the Adsorption-Induced Phase Change in the Flexible Metal-Organic
 Framework Co(bdp).
;
_journal_issue                   45
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15019
_journal_page_last               15026
_journal_paper_doi               10.1021/jacs.6b09155
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C12 H8 Co N4'
_chemical_formula_sum            'C12 H8 Co N4'
_chemical_formula_weight         267.15
_chemical_name_common            Co(bdp)
_space_group_crystal_system      tetragonal
_space_group_IT_number           91
_space_group_name_Hall           'P 4w 2c'
_space_group_name_H-M_alt        'P 41 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2708(4)
_cell_length_b                   13.2708(4)
_cell_length_c                   14.3502(5)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.6665
_cell_measurement_theta_min      2.279
_cell_volume                     2527.27(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32160
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         27.798
_diffrn_reflns_theta_min         2.279
_diffrn_source                   'Advanced Light Source, station 11.3.1'
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.9249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014) was used for absorption correction. wR2(int) was 0.1467 before and 0.0732 after correction. The Ratio of minimum to maximum transmission is 0.9346. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    0.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.014
_refine_diff_density_max         0.190
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         2322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0279
_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)+(0.0481P)²+0.2518P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0836
_reflns_Friedel_coverage         0.672
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2154
_reflns_number_total             2322
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b09155_si_005.cif
_cod_data_source_block           mkt015s_sq
_cod_original_cell_volume        2527.27(18)
_cod_database_code               4131069
_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.
;
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.936
_exptl_absorpt_special_details
;
 X-ray diffraction analyses were performed on single crystals coated with
 Paratone-N oil and mounted on MiTeGen loops. Crystals kept at a temperature of 298 K 
by an Oxford Cryosystems Cyrostream using N2 during
 the experiments. Data was collected at Beamline 11.3.1 at the Advanced
 Light Source, Lawrence Berkeley National Laboratory using synchrotron
 radiation (lamda = 0.7749 angstroms) and a Bruker PHOTON100 CMOS diffractometer.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52(4) 0.48(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C5(H5), C4(H4)
;
_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+1/2'
'-y, x, z+1/4'
'y, -x, z+3/4'
'-x, y, -z'
'x, -y, -z+1/2'
'y, x, -z+3/4'
'-y, -x, -z+1/4'
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 0.98884(2) 0.98884(2) 0.3750 0.02542(17) Uani 1 2 d S T P
N1 N 0.86742(15) 0.9840(2) 0.29491(14) 0.0336(6) Uani 1 1 d . . .
N2 N 0.11114(15) 1.0065(2) 0.20340(14) 0.0384(6) Uani 1 1 d . . .
C1 C 0.77203(19) 0.9752(3) 0.3214(2) 0.0442(8) Uani 1 1 d . . .
H1 H 0.7512 0.9546 0.3818 0.053 Uiso 1 1 calc R . .
C7 C 0.2716(3) 1.0000 0.2500 0.0474(13) Uani 1 2 d S T P
C2 C 0.7071(3) 1.0000 0.2500 0.0417(11) Uani 1 2 d S T P
C8 C 0.2071(2) 1.0101(3) 0.1757(2) 0.0529(10) Uani 1 1 d . . .
H8 H 0.2280 1.0186 0.1129 0.063 Uiso 1 1 calc R . .
C3 C 0.5955(3) 1.0000 0.2500 0.0509(14) Uani 1 2 d S T P
C6 C 0.3839(3) 1.0000 0.2500 0.0545(14) Uani 1 2 d S T P
C5 C 0.4377(2) 1.0226(4) 0.1711(2) 0.0683(13) Uani 1 1 d . . .
H5 H 0.4027 1.0396 0.1156 0.082 Uiso 1 1 calc R . .
C4 C 0.5411(2) 1.0211(4) 0.1708(2) 0.0756(14) Uani 1 1 d . . .
H4 H 0.5759 1.0350 0.1145 0.091 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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 0.3550 1.1300 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0080 0.0040 '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
N1 Co1 N1 106.53(16) . 7
N2 Co1 N1 109.81(8) 6_675 .
N2 Co1 N1 109.81(8) 3_765 7
N2 Co1 N1 112.48(13) 3_765 .
N2 Co1 N1 112.48(13) 6_675 7
N2 Co1 N2 105.83(17) 3_765 6_675
N1 N1 Co1 122.78(10) 6_575 .
C1 N1 Co1 127.78(19) . .
C1 N1 N1 107.45(16) . 6_575
N2 N2 Co1 124.66(6) 6_575 4_474
C8 N2 Co1 127.83(19) . 4_474
C8 N2 N2 107.43(16) . 6_575
N1 C1 H1 124.4 . .
N1 C1 C2 111.2(3) . .
C2 C1 H1 124.4 . .
C8 C7 C8 102.9(3) . 6_575
C8 C7 C6 128.54(17) . .
C8 C7 C6 128.54(17) 6_575 .
C1 C2 C1 102.6(3) 6_575 .
C1 C2 C3 128.68(16) . .
C1 C2 C3 128.68(16) 6_575 .
N2 C8 C7 111.1(3) . .
N2 C8 H8 124.4 . .
C7 C8 H8 124.4 . .
C4 C3 C2 121.71(19) 6_575 .
C4 C3 C2 121.71(19) . .
C4 C3 C4 116.6(4) 6_575 .
C5 C6 C7 121.37(19) . .
C5 C6 C7 121.37(19) 6_575 .
C5 C6 C5 117.3(4) . 6_575
C6 C5 H5 119.3 . .
C6 C5 C4 121.3(3) . .
C4 C5 H5 119.3 . .
C3 C4 H4 119.1 . .
C5 C4 C3 121.7(3) . .
C5 C4 H4 119.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 1.980(2) .
Co1 N1 1.980(2) 7
Co1 N2 1.976(2) 3_765
Co1 N2 1.976(2) 6_675
N1 N1 1.357(4) 6_575
N1 C1 1.327(3) .
N2 Co1 1.976(2) 4_474
N2 N2 1.349(4) 6_575
N2 C8 1.334(3) .
C1 H1 0.9500 .
C1 C2 1.379(4) .
C7 C8 1.373(4) 6_575
C7 C8 1.373(4) .
C7 C6 1.491(5) .
C2 C1 1.379(4) 6_575
C2 C3 1.481(5) .
C8 H8 0.9500 .
C3 C4 1.376(4) 6_575
C3 C4 1.376(4) .
C6 C5 1.371(4) .
C6 C5 1.372(4) 6_575
C5 H5 0.9500 .
C5 C4 1.372(4) .
C4 H4 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_4
Co1 N1 C1 C2 164.7(2) . .
Co1 N2 C8 C7 -177.0(2) 4_474 .
N1 N1 C1 C2 0.6(4) 6_575 .
N1 C1 C2 C1 -0.23(17) . 6_575
N1 C1 C2 C3 179.77(17) . .
N2 N2 C8 C7 -0.2(5) 6_575 .
C1 C2 C3 C4 -176.1(3) . .
C1 C2 C3 C4 -176.1(3) 6_575 6_575
C1 C2 C3 C4 3.9(3) 6_575 .
C1 C2 C3 C4 3.9(3) . 6_575
C7 C6 C5 C4 -179.0(4) . .
C2 C3 C4 C5 -179.0(4) . .
C8 C7 C8 N2 0.08(18) 6_575 .
C8 C7 C6 C5 7.6(3) . .
C8 C7 C6 C5 -172.4(3) 6_575 .
C8 C7 C6 C5 7.6(3) 6_575 6_575
C8 C7 C6 C5 -172.4(3) . 6_575
C6 C7 C8 N2 -179.92(18) . .
C6 C5 C4 C3 -2.0(8) . .
C5 C6 C5 C4 1.0(4) 6_575 .
C4 C3 C4 C5 1.0(4) 6_575 .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.52(4)
2 0.48(4)
