#------------------------------------------------------------------------------
#$Date: 2019-11-03 15:09:36 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221720 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/86/4128639.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_4128639
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                   23.549(5)
_cell_length_b                   23.549(5)
_cell_length_c                   12.446(2)
_cell_measurement_reflns_used    9651
_cell_measurement_temperature    400(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.45
_cell_volume                     6902(2)
_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      400.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.1245
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            154274
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.307
_diffrn_reflns_theta_min         2.533
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.929
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0880 before and 0.0496 after correction.
The Ratio of minimum to maximum transmission is 0.7435.
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    1.486
_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         0.213
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 1595 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         8340
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0411
_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)+(0.0744P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                4409
_reflns_number_total             8340
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            VT_ZIF-zni_Co_400K.cif
_cod_data_source_block           pk59zni_co_400k_red
_cod_original_cell_volume        6902(3)
_cod_database_code               4128639
_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   0.497
_shelx_estimated_absorpt_t_min   0.385
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C41(H41), C13(H13), C12(H12), C22(H22), C21(H21), C43(H43),
 C23(H23), C31(H31), C32(H32), C33(H33), C42(H42)
;
_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 0.40038(2) 0.64880(2) 0.45746(3) 0.05210(16) Uani 1 1 d .
Co2 Co 0.35093(2) 0.40329(2) 0.41152(3) 0.05052(15) Uani 1 1 d .
N21 N 0.48284(16) 0.64050(17) 0.4889(3) 0.0655(10) Uani 1 1 d .
N41 N 0.37758(15) 0.71693(12) 0.3732(3) 0.0533(7) Uani 1 1 d .
N12 N 0.34924(14) 0.48636(14) 0.3784(3) 0.0589(8) Uani 1 1 d .
N31 N 0.3652(2) 0.65849(18) 0.6022(3) 0.0679(10) Uani 1 1 d .
N11 N 0.37212(16) 0.57781(15) 0.3900(3) 0.0626(9) Uani 1 1 d .
C11 C 0.3797(2) 0.52504(16) 0.4280(4) 0.0639(11) Uani 1 1 d .
H11 H 0.4048 0.5164 0.4855 0.077 Uiso 1 1 calc R
C41 C 0.40752(14) 0.74787(19) 0.3035(4) 0.0534(7) Uani 1 1 d .
H41 H 0.4456 0.7395 0.2841 0.064 Uiso 1 1 calc R
C13 C 0.3205(2) 0.5148(2) 0.3023(4) 0.0774(13) Uani 1 1 d .
H13 H 0.2945 0.4984 0.2530 0.093 Uiso 1 1 calc R
C12 C 0.3348(2) 0.5712(2) 0.3070(4) 0.0718(12) Uani 1 1 d .
H12 H 0.3212 0.6004 0.2610 0.086 Uiso 1 1 calc R
C22 C 0.5082(3) 0.6494(4) 0.5845(5) 0.127(3) Uani 1 1 d .
H22 H 0.4898 0.6636 0.6469 0.153 Uiso 1 1 calc R
C21 C 0.52572(19) 0.6230(3) 0.4286(4) 0.0775(14) Uani 1 1 d .
H21 H 0.5215 0.6154 0.3541 0.093 Uiso 1 1 calc R
C43 C 0.32612(18) 0.7887(2) 0.3138(4) 0.0698(11) Uani 1 1 d .
H43 H 0.2953 0.8141 0.3031 0.084 Uiso 1 1 calc R
N22 N 0.57449(16) 0.61688(17) 0.4783(3) 0.0660(9) Uani 1 1 d .
C23 C 0.5629(3) 0.6354(5) 0.5784(5) 0.128(3) Uani 1 1 d .
H23 H 0.5894 0.6380 0.6356 0.154 Uiso 1 1 calc R
C31 C 0.3586(2) 0.61854(19) 0.6763(4) 0.0717(12) Uani 1 1 d .
H31 H 0.3623 0.5792 0.6607 0.086 Uiso 1 1 calc R
C32 C 0.3582(3) 0.7075(2) 0.6572(5) 0.108(2) Uani 1 1 d .
H32 H 0.3612 0.7446 0.6275 0.129 Uiso 1 1 calc R
N32 N 0.34653(18) 0.63758(18) 0.7727(3) 0.0649(10) Uani 1 1 d .
C33 C 0.3463(3) 0.6955(2) 0.7613(5) 0.110(2) Uani 1 1 d .
H33 H 0.3391 0.7224 0.8166 0.131 Uiso 1 1 calc R
C42 C 0.32615(17) 0.74324(18) 0.3807(4) 0.0661(10) Uani 1 1 d .
H42 H 0.2955 0.7317 0.4252 0.079 Uiso 1 1 calc R
N42 N 0.37845(14) 0.79197(14) 0.2638(3) 0.0552(7) Uani 1 1 d .
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
N21 Co1 N31 103.79(18) . .
N41 Co1 N21 116.47(15) . .
N41 Co1 N31 105.76(15) . .
N11 Co1 N21 109.10(17) . .
N11 Co1 N41 111.43(16) . .
N11 Co1 N31 109.83(18) . .
N12 Co2 N22 109.60(16) . 10_554
N32 Co2 N12 107.14(18) 5_564 .
N32 Co2 N22 107.04(17) 5_564 10_554
N42 Co2 N12 114.14(15) 8_455 .
N42 Co2 N22 106.23(15) 8_455 10_554
N42 Co2 N32 112.46(16) 8_455 5_564
C22 N21 Co1 126.2(4) . .
C21 N21 Co1 131.6(3) . .
C21 N21 C22 102.2(4) . .
C41 N41 Co1 129.8(3) . .
C41 N41 C42 105.4(3) . .
C42 N41 Co1 124.7(3) . .
C11 N12 Co2 124.8(3) . .
C11 N12 C13 105.1(3) . .
C13 N12 Co2 130.0(3) . .
C31 N31 Co1 126.5(3) . .
C31 N31 C32 103.9(4) . .
C32 N31 Co1 127.2(3) . .
C11 N11 Co1 125.9(3) . .
C11 N11 C12 104.3(4) . .
C12 N11 Co1 129.2(3) . .
N12 C11 N11 113.8(4) . .
N12 C11 H11 123.1 . .
N11 C11 H11 123.1 . .
N41 C41 H41 123.4 . .
N41 C41 N42 113.2(3) . .
N42 C41 H41 123.4 . .
N12 C13 H13 125.4 . .
N12 C13 C12 109.3(4) . .
C12 C13 H13 125.4 . .
N11 C12 C13 107.4(4) . .
N11 C12 H12 126.3 . .
C13 C12 H12 126.3 . .
N21 C22 H22 125.1 . .
C23 C22 N21 109.9(5) . .
C23 C22 H22 125.1 . .
N21 C21 H21 122.1 . .
N22 C21 N21 115.8(4) . .
N22 C21 H21 122.1 . .
C42 C43 H43 125.7 . .
C42 C43 N42 108.6(4) . .
N42 C43 H43 125.7 . .
C21 N22 Co2 126.8(3) . 10_554
C21 N22 C23 102.8(4) . .
C23 N22 Co2 129.7(4) . 10_554
C22 C23 N22 109.2(5) . .
C22 C23 H23 125.4 . .
N22 C23 H23 125.4 . .
N31 C31 H31 122.6 . .
N32 C31 N31 114.7(4) . .
N32 C31 H31 122.6 . .
N31 C32 H32 125.4 . .
N31 C32 C33 109.3(4) . .
C33 C32 H32 125.4 . .
C31 N32 Co2 128.3(3) . 5_565
C31 N32 C33 104.3(4) . .
C33 N32 Co2 125.0(4) . 5_565
C32 C33 N32 107.8(5) . .
C32 C33 H33 126.1 . .
N32 C33 H33 126.1 . .
N41 C42 H42 125.7 . .
C43 C42 N41 108.5(4) . .
C43 C42 H42 125.7 . .
C41 N42 Co2 129.3(3) . 16_454
C41 N42 C43 104.3(3) . .
C43 N42 Co2 126.4(3) . 16_454
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N21 1.991(4) .
Co1 N41 1.991(3) .
Co1 N31 1.996(4) .
Co1 N11 1.986(4) .
Co2 N12 2.000(3) .
Co2 N22 2.000(4) 10_554
Co2 N32 1.981(4) 5_564
Co2 N42 1.972(3) 8_455
N21 C22 1.347(7) .
N21 C21 1.323(6) .
N41 C41 1.334(5) .
N41 C42 1.364(5) .
N12 C11 1.313(5) .
N12 C13 1.342(6) .
N31 C31 1.326(6) .
N31 C32 1.352(7) .
N11 C11 1.342(5) .
N11 C12 1.365(7) .
C11 H11 0.9500 .
C41 H41 0.9500 .
C41 N42 1.339(5) .
C13 H13 0.9500 .
C13 C12 1.372(7) .
C12 H12 0.9500 .
C22 H22 0.9500 .
C22 C23 1.331(9) .
C21 H21 0.9500 .
C21 N22 1.313(6) .
C43 H43 0.9500 .
C43 C42 1.357(6) .
C43 N42 1.383(6) .
N22 Co2 2.000(4) 10_554
N22 C23 1.348(8) .
C23 H23 0.9500 .
C31 H31 0.9500 .
C31 N32 1.312(7) .
C32 H32 0.9500 .
C32 C33 1.356(8) .
N32 Co2 1.981(4) 5_565
N32 C33 1.371(7) .
C33 H33 0.9500 .
C42 H42 0.9500 .
N42 Co2 1.972(3) 16_454
