#------------------------------------------------------------------------------
#$Date: 2019-11-25 16:50:54 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241371 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/10/4131068.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_4131068
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 H4 Co D4 N4'
_chemical_formula_sum            'C12 H4 Co D4 N4'
_chemical_formula_weight         271.18
_space_group_crystal_system      tetragonal
_space_group_IT_number           95
_space_group_name_Hall           'P 4cw 2c'
_space_group_name_H-M_alt        'P 43 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                   13.2909(5)
_cell_length_b                   13.2909(5)
_cell_length_c                   14.3560(6)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.350
_cell_measurement_theta_min      2.277
_cell_volume                     2535.96(17)
_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 PHOTON100 CMOS 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  0.0570
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38643
_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         30.699
_diffrn_reflns_theta_min         2.277
_diffrn_source                   'Advanced Light Source, station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.880
_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    0.710
_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          0.071
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.31(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         3051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0270
_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)+(0.0480P)²+0.2563P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.696
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2881
_reflns_number_total             3051
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b09155_si_004.cif
_cod_data_source_block           mkt018s_sq
_cod_original_cell_volume        2536.0(2)
_cod_database_code               4131068
_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   0.942
_shelx_estimated_absorpt_t_min   0.936
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.69(3) 0.31(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(D4), C5(D5), C8(H8)
;
_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+3/4'
'y, -x, z+1/4'
'-x, y, -z'
'x, -y, -z+1/2'
'y, x, -z+1/4'
'-y, -x, -z+3/4'
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 -0.01088(2) -0.01088(2) 0.1250 0.02273(13) Uani 1 2 d S T P
N1 N 0.11116(13) -0.00718(19) 0.20313(11) 0.0363(5) Uani 1 1 d . . .
N2 N 0.86751(13) 0.01515(18) 0.29506(12) 0.0326(4) Uani 1 1 d . . .
C1 C 0.20793(17) -0.0108(3) 0.17550(17) 0.0508(8) Uani 1 1 d . . .
H1 H 0.2286 -0.0194 0.1141 0.061 Uiso 1 1 calc R . .
C2 C 0.2724(2) 0.0000 0.2500 0.0435(10) Uani 1 2 d S T P
C3 C 0.3835(2) 0.0000 0.2500 0.0486(11) Uani 1 2 d S T P
C4 C 0.43648(19) 0.0233(3) 0.32953(19) 0.0638(10) Uani 1 1 d . . .
D4 D 0.4020 0.0402 0.3837 0.077 Uiso 1 1 calc R . .
C5 C 0.5417(2) 0.0219(3) 0.32961(19) 0.0755(13) Uani 1 1 d . . .
D5 D 0.5759 0.0361 0.3846 0.091 Uiso 1 1 calc R . .
C6 C 0.5961(2) 0.0000 0.2500 0.0505(12) Uani 1 2 d S T P
C7 C 0.7071(2) 0.0000 0.2500 0.0387(9) Uani 1 2 d S T P
C8 C 0.77138(16) 0.0245(3) 0.32160(16) 0.0435(7) Uani 1 1 d . . .
H8 H 0.7508 0.0449 0.3806 0.052 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'
D D 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'
H H 0.0000 0.0000 '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 106.39(14) . 7
N1 Co1 N2 111.90(10) 7 6_455
N1 Co1 N2 109.99(7) 7 3_544
N1 Co1 N2 109.99(7) . 6_455
N1 Co1 N2 111.89(10) . 3_544
N2 Co1 N2 106.75(13) 3_544 6_455
N1 N1 Co1 124.50(5) 6 .
C1 N1 Co1 128.09(15) . .
C1 N1 N1 107.25(13) . 6
N2 N2 Co1 122.96(8) 6 4_655
C8 N2 Co1 128.00(15) . 4_655
C8 N2 N2 107.42(13) . 6
N1 C1 H1 124.4 . .
N1 C1 C2 111.2(2) . .
C2 C1 H1 124.4 . .
C1 C2 C1 103.1(3) . 6
C1 C2 C3 128.43(14) . .
C1 C2 C3 128.43(14) 6 .
C4 C3 C2 120.76(16) 6 .
C4 C3 C2 120.76(16) . .
C4 C3 C4 118.5(3) 6 .
C3 C4 D4 119.7 . .
C3 C4 C5 120.6(2) . .
C5 C4 D4 119.7 . .
C4 C5 D5 119.2 . .
C6 C5 C4 121.7(2) . .
C6 C5 D5 119.2 . .
C5 C6 C5 116.9(3) 6 .
C5 C6 C7 121.53(16) . .
C5 C6 C7 121.53(16) 6 .
C8 C7 C6 128.36(13) 6 .
C8 C7 C6 128.36(13) . .
C8 C7 C8 103.3(3) 6 .
N2 C8 C7 110.9(2) . .
N2 C8 H8 124.5 . .
C7 C8 H8 124.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 1.9727(17) .
Co1 N1 1.9727(17) 7
Co1 N2 1.9831(17) 6_455
Co1 N2 1.9831(17) 3_544
N1 N1 1.359(3) 6
N1 C1 1.347(3) .
N2 Co1 1.9830(17) 4_655
N2 N2 1.355(3) 6
N2 C8 1.339(3) .
C1 H1 0.9300 .
C1 C2 1.378(3) .
C2 C1 1.378(3) 6
C2 C3 1.477(4) .
C3 C4 1.377(3) 6
C3 C4 1.377(3) .
C4 D4 0.9300 .
C4 C5 1.398(3) .
C5 D5 0.9300 .
C5 C6 1.384(3) .
C6 C5 1.384(3) 6
C6 C7 1.476(4) .
C7 C8 1.375(3) .
C7 C8 1.375(3) 6
C8 H8 0.9300 .
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 176.21(17) . .
Co1 N2 C8 C7 -165.19(16) 4_655 .
N1 N1 C1 C2 0.6(4) 6 .
N1 C1 C2 C1 -0.24(15) . 6
N1 C1 C2 C3 179.76(15) . .
N2 N2 C8 C7 0.4(4) 6 .
C1 C2 C3 C4 172.4(3) 6 6
C1 C2 C3 C4 -7.6(3) . 6
C1 C2 C3 C4 -7.6(3) 6 .
C1 C2 C3 C4 172.4(3) . .
C2 C3 C4 C5 179.1(3) . .
C3 C4 C5 C6 1.8(7) . .
C4 C3 C4 C5 -0.9(3) 6 .
C4 C5 C6 C5 -0.9(3) . 6
C4 C5 C6 C7 179.1(3) . .
C5 C6 C7 C8 -3.3(3) 6 6
C5 C6 C7 C8 -3.3(3) . .
C5 C6 C7 C8 176.7(3) . 6
C5 C6 C7 C8 176.7(3) 6 .
C6 C7 C8 N2 179.83(14) . .
C8 C7 C8 N2 -0.17(14) 6 .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.69(3)
2 0.31(3)
