#------------------------------------------------------------------------------
#$Date: 2019-11-03 15:16:51 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221733 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/86/4128652.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_4128652
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         '0.06(C96 H96 Co16 N64)'
_chemical_formula_sum            'C6 H6 Co N4'
_chemical_formula_weight         193.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-17
_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            16
_cell_length_a                   15.591(5)
_cell_length_b                   15.606(4)
_cell_length_c                   18.103(5)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    400(2)
_cell_measurement_theta_max      29.31
_cell_measurement_theta_min      2.60
_cell_volume                     4405(2)
_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(2)
_diffrn_measured_fraction_theta_full 0.997
_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  0.0425
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31691
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.843
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.512
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1359 before and 0.0574 after correction.
The Ratio of minimum to maximum transmission is 0.6954.
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    1.165
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.524
_exptl_crystal_size_mid          0.378
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         5307
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0479P)²+1.1887P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1238
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3129
_reflns_number_total             5307
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            VT_dry_ZIF-4_Co_400K.cif
_cod_data_source_block           mo_zif-4_co_400k
_cod_database_code               4128652
_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   0.627
_shelx_estimated_absorpt_t_min   0.505
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N21-C22A \\sim N22-C23A
 with sigma of 0.02
3. Others
 Fixed Sof: C22A(0.5) H22A(0.5) C23A(0.5) H23A(0.5) C22B(0.5) H22B(0.5)
 C23B(0.5) H23B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C21(H21), C22A(H22A), C23A(H23A), C31(H31), C32(H32), C33(H33),
 C41(H41), C42(H42), C43(H43), C13A(H13A), C12A(H12A), C22B(H22B), C23B(H23B)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.50324(2) 0.34105(2) 0.31205(2) 0.08510(16) Uani 1 1 d . . . .
Co2 Co 0.20016(3) 0.14369(3) 0.40525(2) 0.08753(16) Uani 1 1 d . . . .
N11 N 0.43918(16) 0.24054(15) 0.35034(15) 0.0986(7) Uani 1 1 d . . . .
N12 N 0.32381(18) 0.16706(17) 0.38797(16) 0.0986(7) Uani 1 1 d . . . .
N21 N 0.59411(16) 0.37024(18) 0.38485(14) 0.0995(7) Uani 1 1 d D . . .
N22 N 0.66961(18) 0.37577(19) 0.49011(14) 0.1035(8) Uani 1 1 d D . . .
N31 N 0.41916(16) 0.43640(15) 0.30508(13) 0.0911(6) Uani 1 1 d . . . .
N32 N 0.33685(16) 0.54421(15) 0.34431(14) 0.0940(7) Uani 1 1 d . . . .
N41 N 0.55769(17) 0.31750(16) 0.21479(14) 0.0949(7) Uani 1 1 d . . . .
N42 N 0.63444(17) 0.24386(15) 0.13260(14) 0.0937(7) Uani 1 1 d . . . .
C11 C 0.3544(2) 0.23868(19) 0.35908(18) 0.0955(8) Uani 1 1 d . . . .
H11 H 0.3186 0.2853 0.3456 0.115 Uiso 1 1 calc R . . .
C21 C 0.6019(2) 0.34983(19) 0.45450(17) 0.0944(9) Uani 1 1 d . . . .
H21 H 0.5591 0.3168 0.4786 0.113 Uiso 1 1 calc R . . .
C22A C 0.6782(8) 0.3839(12) 0.3666(8) 0.179(7) Uani 0.5 1 d D P A 1
H22A H 0.7005 0.3898 0.3180 0.215 Uiso 0.5 1 calc R P A 1
C23A C 0.7258(7) 0.3875(12) 0.4322(7) 0.181(7) Uani 0.5 1 d D P A 1
H23A H 0.7859 0.3965 0.4361 0.217 Uiso 0.5 1 calc R P A 1
C31 C 0.40134(19) 0.49169(18) 0.35832(17) 0.0923(8) Uani 1 1 d . . . .
H31 H 0.4326 0.4935 0.4033 0.111 Uiso 1 1 calc R . . .
C32 C 0.3611(3) 0.4558(2) 0.2519(2) 0.1274(12) Uani 1 1 d . . . .
H32 H 0.3562 0.4281 0.2054 0.153 Uiso 1 1 calc R . . .
C33 C 0.3114(3) 0.5207(2) 0.2760(2) 0.1300(14) Uani 1 1 d . . . .
H33 H 0.2656 0.5460 0.2491 0.156 Uiso 1 1 calc R . . .
C41 C 0.5896(2) 0.2432(2) 0.19435(17) 0.0982(9) Uani 1 1 d . . . .
H41 H 0.5809 0.1924 0.2222 0.118 Uiso 1 1 calc R . . .
C42 C 0.5835(3) 0.3698(2) 0.1612(2) 0.1497(18) Uani 1 1 d . . . .
H42 H 0.5714 0.4294 0.1587 0.180 Uiso 1 1 calc R . . .
C43 C 0.6295(4) 0.3254(3) 0.1109(2) 0.157(2) Uani 1 1 d . . . .
H43 H 0.6543 0.3484 0.0672 0.188 Uiso 1 1 calc R . . .
C13A C 0.3947(3) 0.1202(3) 0.3998(3) 0.1502(18) Uani 1 1 d . . . .
H13A H 0.3955 0.0647 0.4212 0.180 Uiso 1 1 calc R . . .
C12A C 0.4646(3) 0.1638(3) 0.3766(3) 0.1561(19) Uani 1 1 d . . . .
H12A H 0.5221 0.1437 0.3784 0.187 Uiso 1 1 calc R . . .
C22B C 0.6466(10) 0.4416(9) 0.3831(8) 0.158(6) Uani 0.5 1 d . P A 2
H22B H 0.6501 0.4815 0.3437 0.189 Uiso 0.5 1 calc R P A 2
C23B C 0.6915(8) 0.4455(9) 0.4454(8) 0.155(5) Uani 0.5 1 d . P A 2
H23B H 0.7320 0.4887 0.4576 0.186 Uiso 0.5 1 calc R P A 2
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 N11 107.95(11) . .
N21 Co1 N31 109.92(11) . .
N31 Co1 N11 106.39(11) . .
N41 Co1 N11 112.21(11) . .
N41 Co1 N21 108.97(11) . .
N41 Co1 N31 111.33(11) . .
N22 Co2 N12 114.38(12) 4_456 .
N22 Co2 N32 109.97(11) 4_456 8_655
N22 Co2 N42 109.05(11) 4_456 6_556
N32 Co2 N12 109.71(11) 8_655 .
N32 Co2 N42 105.81(11) 8_655 6_556
N42 Co2 N12 107.52(11) 6_556 .
C11 N11 Co1 123.9(2) . .
C11 N11 C12A 103.4(3) . .
C12A N11 Co1 132.6(3) . .
C11 N12 Co2 124.6(2) . .
C11 N12 C13A 103.1(3) . .
C13A N12 Co2 132.3(3) . .
C21 N21 Co1 130.6(2) . .
C21 N21 C22A 100.5(7) . .
C21 N21 C22B 99.4(6) . .
C22A N21 Co1 123.9(7) . .
C22B N21 Co1 126.3(6) . .
C21 N22 Co2 128.5(2) . 4_556
C21 N22 C23A 100.4(6) . .
C21 N22 C23B 98.8(6) . .
C23A N22 Co2 126.6(6) . 4_556
C23B N22 Co2 128.0(6) . 4_556
C31 N31 Co1 125.5(2) . .
C31 N31 C32 103.4(3) . .
C32 N31 Co1 130.8(2) . .
C31 N32 Co2 126.7(2) . 8_665
C31 N32 C33 103.4(3) . .
C33 N32 Co2 129.4(2) . 8_665
C41 N41 Co1 125.0(2) . .
C41 N41 C42 102.8(3) . .
C42 N41 Co1 131.4(2) . .
C41 N42 Co2 124.0(2) . 6_656
C41 N42 C43 103.1(3) . .
C43 N42 Co2 132.6(2) . 6_656
N12 C11 N11 115.0(3) . .
N21 C21 N22 118.5(3) . .
C23A C22A N21 107.9(9) . .
C22A C23A N22 107.7(9) . .
N31 C31 N32 115.1(3) . .
C33 C32 N31 108.8(3) . .
C32 C33 N32 109.3(3) . .
N42 C41 N41 115.6(3) . .
N41 C42 C43 109.7(3) . .
N42 C43 C42 108.7(3) . .
C12A C13A N12 109.9(3) . .
C13A C12A N11 108.6(4) . .
C23B C22B N21 109.3(10) . .
C22B C23B N22 109.1(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N11 1.985(2) .
Co1 N21 1.988(3) .
Co1 N31 1.987(2) .
Co1 N41 1.989(2) .
Co2 N12 1.987(3) .
Co2 N22 1.977(3) 4_456
Co2 N32 1.990(2) 8_655
Co2 N42 1.991(2) 6_556
N11 C11 1.331(4) .
N11 C12A 1.348(4) .
N12 C11 1.323(4) .
N12 C13A 1.342(5) .
N21 C21 1.306(4) .
N21 C22A 1.369(11) .
N21 C22B 1.383(12) .
N22 Co2 1.977(3) 4_556
N22 C21 1.301(4) .
N22 C23A 1.377(10) .
N22 C23B 1.398(11) .
N31 C31 1.323(3) .
N31 C32 1.355(4) .
N32 Co2 1.990(2) 8_665
N32 C31 1.322(3) .
N32 C33 1.350(4) .
N41 C41 1.315(4) .
N41 C42 1.330(4) .
N42 Co2 1.991(2) 6_656
N42 C41 1.318(4) .
N42 C43 1.334(4) .
C22A C23A 1.402(19) .
C32 C33 1.348(5) .
C42 C43 1.351(5) .
C13A C12A 1.353(5) .
C22B C23B 1.328(19) .
