#------------------------------------------------------------------------------
#$Date: 2019-11-03 15:10:31 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221721 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/86/4128640.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_4128640
loop_
_publ_author_name
'Frentzel-Beyme, Louis'
'Kloß, Marvin'
'Kolodzeiski, Pascal'
'Pallach, Roman'
'Henke, Sebastian'
_publ_section_title
;
 Meltable Mixed-Linker Zeolitic Imidazolate Frameworks and Their
 Microporous Glasses: From Melting Point Engineering to Selective
 Hydrocarbon Sorption.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12362
_journal_page_last               12371
_journal_paper_doi               10.1021/jacs.9b05558
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C6 H6 Co N4'
_chemical_formula_sum            'C6 H6 Co N4'
_chemical_formula_weight         193.08
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-21
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   23.4363(6)
_cell_length_b                   23.4363(6)
_cell_length_c                   12.4615(3)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      36.10
_cell_measurement_theta_min      2.54
_cell_volume                     6844.6(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1059
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            76970
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.312
_diffrn_reflns_theta_min         2.539
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.945
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0798 before and 0.0486 after correction.
The Ratio of minimum to maximum transmission is 0.7850.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       prism
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.612
_exptl_crystal_size_mid          0.492
_exptl_crystal_size_min          0.422
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 2559 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         8287
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0724P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6544
_reflns_number_total             8287
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            VT_ZIF-zni_Co_200K.cif
_cod_data_source_block           pk59zni_co_200k_red
_cod_original_cell_volume        6844.6(4)
_cod_database_code               4128640
_shelx_shelxl_version_number     2014/7
_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   0.494
_shelx_estimated_absorpt_t_min   0.382
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C11(H11), C41(H41), C31(H31), C43(H43), C13(H13), C23(H23),
 C22(H22), C42(H42), C33(H33), C12(H12), C32(H32)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x, -y, z+1/2'
'-x+1/2, y+1/2, z'
'-y, -x+1/2, z+3/4'
'y+1/2, x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
'x+1/2, -y+1/2, z+1'
'-x+1, y+1, z+1/2'
'-y+1/2, -x+1, z+5/4'
'y+1, x+1/2, 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
Co1 Co 0.40233(2) 0.64734(2) 0.45621(2) 0.02573(9) Uani 1 1 d .
Co2 Co 0.35028(2) 0.39721(2) 0.41261(2) 0.02632(10) Uani 1 1 d .
N12 N 0.35847(12) 0.47987(12) 0.3813(2) 0.0338(5) Uani 1 1 d .
N22 N 0.57791(11) 0.62935(12) 0.4813(2) 0.0322(5) Uani 1 1 d .
N41 N 0.37552(11) 0.70564(11) 0.35283(19) 0.0285(4) Uani 1 1 d .
N42 N 0.37369(11) 0.78143(10) 0.24386(19) 0.0277(4) Uani 1 1 d .
N31 N 0.36112(12) 0.65270(13) 0.5947(2) 0.0329(5) Uani 1 1 d .
N11 N 0.38247(12) 0.57233(12) 0.3911(2) 0.0336(5) Uani 1 1 d .
N21 N 0.48518(11) 0.65130(11) 0.4900(2) 0.0302(5) Uani 1 1 d .
N32 N 0.34048(13) 0.63712(14) 0.7672(2) 0.0343(5) Uani 1 1 d .
C21 C 0.52545(12) 0.62093(15) 0.4410(3) 0.0336(6) Uani 1 1 d .
H21 H 0.5178 0.5957 0.3831 0.040 Uiso 1 1 calc R
C11 C 0.37774(16) 0.52252(14) 0.4418(3) 0.0371(7) Uani 1 1 d .
H11 H 0.3874 0.5178 0.5153 0.045 Uiso 1 1 calc R
C41 C 0.40382(11) 0.75144(14) 0.3160(2) 0.0272(5) Uani 1 1 d .
H41 H 0.4412 0.7615 0.3386 0.033 Uiso 1 1 calc R
C31 C 0.38112(14) 0.64220(15) 0.6925(3) 0.0352(6) Uani 1 1 d .
H31 H 0.4207 0.6386 0.7080 0.042 Uiso 1 1 calc R
C43 C 0.32298(13) 0.75261(14) 0.2336(2) 0.0322(5) Uani 1 1 d .
H43 H 0.2924 0.7630 0.1876 0.039 Uiso 1 1 calc R
C13 C 0.3488(2) 0.50474(19) 0.2826(3) 0.0529(10) Uani 1 1 d .
H13 H 0.3341 0.4860 0.2210 0.063 Uiso 1 1 calc R
C23 C 0.57007(15) 0.66733(15) 0.5640(3) 0.0353(6) Uani 1 1 d .
H23 H 0.5990 0.6817 0.6100 0.042 Uiso 1 1 calc R
C22 C 0.51367(15) 0.68088(15) 0.5687(3) 0.0378(7) Uani 1 1 d .
H22 H 0.4967 0.7066 0.6182 0.045 Uiso 1 1 calc R
C42 C 0.32374(13) 0.70689(14) 0.2999(3) 0.0335(6) Uani 1 1 d .
H42 H 0.2937 0.6801 0.3087 0.040 Uiso 1 1 calc R
C33 C 0.29113(17) 0.6446(2) 0.7125(3) 0.0538(11) Uani 1 1 d .
H33 H 0.2540 0.6435 0.7432 0.065 Uiso 1 1 calc R
C12 C 0.3641(2) 0.56053(18) 0.2884(3) 0.0548(11) Uani 1 1 d .
H12 H 0.3624 0.5871 0.2310 0.066 Uiso 1 1 calc R
C32 C 0.30271(16) 0.6541(2) 0.6068(3) 0.0532(11) Uani 1 1 d .
H32 H 0.2755 0.6605 0.5516 0.064 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 0.0033 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'
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
N41 Co1 N31 111.61(11) . .
N41 Co1 N11 105.64(11) . .
N41 Co1 N21 114.55(10) . .
N31 Co1 N11 107.28(12) . .
N31 Co1 N21 106.75(11) . .
N21 Co1 N11 110.84(11) . .
N12 Co2 N22 107.95(12) . 10_554
N12 Co2 N32 103.08(12) . 5_564
N22 Co2 N32 111.23(12) 10_554 5_564
N42 Co2 N12 116.75(11) 8_455 .
N42 Co2 N22 112.45(11) 8_455 10_554
N42 Co2 N32 104.95(11) 8_455 5_564
C11 N12 Co2 130.9(2) . .
C11 N12 C13 104.1(3) . .
C13 N12 Co2 124.8(3) . .
C21 N22 Co2 124.6(2) . 10_554
C21 N22 C23 104.7(3) . .
C23 N22 Co2 129.7(2) . 10_554
C41 N41 Co1 128.12(19) . .
C41 N41 C42 104.7(2) . .
C42 N41 Co1 127.2(2) . .
C41 N42 Co2 128.5(2) . 16_454
C41 N42 C43 105.1(2) . .
C43 N42 Co2 126.40(19) . 16_454
C31 N31 Co1 128.0(2) . .
C31 N31 C32 104.8(3) . .
C32 N31 Co1 125.5(2) . .
C11 N11 Co1 126.8(2) . .
C11 N11 C12 103.8(3) . .
C12 N11 Co1 129.0(2) . .
C21 N21 Co1 124.8(2) . .
C21 N21 C22 104.6(3) . .
C22 N21 Co1 130.5(2) . .
C31 N32 Co2 125.9(2) . 5_565
C31 N32 C33 104.3(3) . .
C33 N32 Co2 127.4(2) . 5_565
N22 C21 H21 123.2 . .
N21 C21 N22 113.5(3) . .
N21 C21 H21 123.2 . .
N12 C11 N11 114.7(3) . .
N12 C11 H11 122.7 . .
N11 C11 H11 122.7 . .
N41 C41 H41 123.6 . .
N42 C41 N41 112.8(2) . .
N42 C41 H41 123.6 . .
N31 C31 N32 113.8(3) . .
N31 C31 H31 123.1 . .
N32 C31 H31 123.1 . .
N42 C43 H43 125.6 . .
C42 C43 N42 108.7(2) . .
C42 C43 H43 125.6 . .
N12 C13 H13 125.8 . .
C12 C13 N12 108.4(3) . .
C12 C13 H13 125.8 . .
N22 C23 H23 125.9 . .
C22 C23 N22 108.2(3) . .
C22 C23 H23 125.9 . .
N21 C22 H22 125.5 . .
C23 C22 N21 108.9(3) . .
C23 C22 H22 125.5 . .
N41 C42 H42 125.7 . .
C43 C42 N41 108.7(3) . .
C43 C42 H42 125.7 . .
N32 C33 H33 125.1 . .
N32 C33 C32 109.7(3) . .
C32 C33 H33 125.1 . .
N11 C12 H12 125.5 . .
C13 C12 N11 109.0(3) . .
C13 C12 H12 125.5 . .
N31 C32 H32 126.3 . .
C33 C32 N31 107.4(3) . .
C33 C32 H32 126.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N41 1.980(2) .
Co1 N31 1.982(3) .
Co1 N11 1.992(3) .
Co1 N21 1.989(3) .
Co2 N12 1.985(3) .
Co2 N22 1.988(3) 10_554
Co2 N42 1.983(2) 8_455
Co2 N32 1.996(3) 5_564
N12 C11 1.331(4) .
N12 C13 1.380(4) .
N22 Co2 1.988(3) 10_554
N22 C21 1.343(4) .
N22 C23 1.374(4) .
N41 C41 1.343(4) .
N41 C42 1.381(4) .
N42 Co2 1.983(2) 16_454
N42 C41 1.342(4) .
N42 C43 1.373(4) .
N31 C31 1.329(4) .
N31 C32 1.378(5) .
N11 C11 1.332(4) .
N11 C12 1.377(5) .
N21 C21 1.331(4) .
N21 C22 1.373(4) .
N32 Co2 1.996(3) 5_565
N32 C31 1.337(4) .
N32 C33 1.354(5) .
C21 H21 0.9500 .
C11 H11 0.9500 .
C41 H41 0.9500 .
C31 H31 0.9500 .
C43 H43 0.9500 .
C43 C42 1.353(4) .
C13 H13 0.9500 .
C13 C12 1.358(6) .
C23 H23 0.9500 .
C23 C22 1.361(5) .
C22 H22 0.9500 .
C42 H42 0.9500 .
C33 H33 0.9500 .
C33 C32 1.363(5) .
C12 H12 0.9500 .
C32 H32 0.9500 .
