#------------------------------------------------------------------------------
#$Date: 2019-11-03 15:05:23 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221716 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/86/4128635.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_4128635
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(C115.2 H95.2 Co16 N64)'
_chemical_formula_sum            'C7.2 H6.6 Co N4'
_chemical_formula_weight         208.09
_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             2018-10-29
_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                   15.5146(11)
_cell_length_b                   15.7585(10)
_cell_length_c                   18.0597(11)
_cell_measurement_reflns_used    9435
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      29.28
_cell_measurement_theta_min      2.16
_cell_volume                     4415.4(5)
_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      300(2)
_diffrn_measured_fraction_theta_full 0.998
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45024
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.820
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.513
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1195 before and 0.0633 after correction.
The Ratio of minimum to maximum transmission is 0.6304.
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    1.252
_exptl_crystal_description       prism
_exptl_crystal_F_000             1677
_exptl_crystal_size_max          0.765
_exptl_crystal_size_mid          0.726
_exptl_crystal_size_min          0.599
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5319
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0466
_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)+(0.0817P)²+2.6686P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1740
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3600
_reflns_number_total             5319
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            VT_dry_ZIF-62_Co_0-30_300K.cif
_cod_data_source_block           int1_zif-62_co_1_no_guest_300k
_cod_original_formula_sum        'C7.20 H6.60 Co N4'
_cod_database_code               4128635
_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   0.464
_shelx_estimated_absorpt_t_min   0.391
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C23B-C22B \\sim C24B-C23B \\sim C25B-C24B \\sim C26B-C25B \\sim C27B-C26B
\\sim C27B-C22B
 with sigma of 0.02
 N22B-C21 \\sim N22A-C21 \\sim N21A-C21 \\sim N21B-C21
 with sigma of 0.02
 C16-C15 \\sim C17-C16 \\sim C13-C12 \\sim C14-C13 \\sim C15-C14 \\sim C17-C12
 with sigma of 0.02
 N22B-C23B \\sim N22A-C23A \\sim N21B-C22B \\sim N21A-C22A
 with sigma of 0.02
3. Restrained planarity
 C22B, C23B, C24B, C25B, C26B, C27B
 with sigma of 0.1
 C12, C13, C14, C15, C16, C17
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N22B \\sim N22A \\sim N21A \\sim N21B: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C25B \\sim C24B \\sim C26B \\sim C27B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C22A \\sim C23A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
5. Others
 Fixed Sof: N21B(0.5) N21A(0.5) N22B(0.5) N22A(0.5) H12(0.5) H13(0.5) C14(0.4)
 H14(0.4) C15(0.4) H15(0.4) C16(0.4) H16(0.4) C17(0.4) H17(0.4) H21(0.5)
 C22A(0.5) H22A(0.5) C22B(0.5) C23A(0.5) H23A(0.5) C23B(0.5) C24B(0.2)
 H24B(0.2) C25B(0.2) H25B(0.2) C26B(0.2) H26B(0.2) C27B(0.2) H27B(0.2)
6.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C21(H21), C22A(H22A), C23A(H23A), C24B(H24B), C25B(H25B), C26B(H26B),
 C27B(H27B), C31(H31), C32(H32), C33(H33), C41(H41), C42(H42), C43(H43)
;
_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_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.50262(3) 0.33495(3) 0.31435(3) 0.06666(19) Uani 1 1 d . . . . .
Co2 Co 0.19921(3) 0.13592(3) 0.40348(3) 0.06818(19) Uani 1 1 d . . . . .
N11 N 0.4390(2) 0.23536(19) 0.35345(19) 0.0735(8) Uani 1 1 d . . . . .
N12 N 0.3231(2) 0.1611(2) 0.3889(2) 0.0769(8) Uani 1 1 d . . . . .
N21B N 0.5895(12) 0.3831(10) 0.3903(7) 0.077(5) Uani 0.5 1 d D U P A 2
N21A N 0.5928(11) 0.3574(11) 0.3841(6) 0.072(4) Uani 0.5 1 d D U P A 1
N22B N 0.6599(7) 0.3950(6) 0.4936(7) 0.066(3) Uani 0.5 1 d D U P A 2
N22A N 0.6734(7) 0.3664(7) 0.4909(7) 0.073(3) Uani 0.5 1 d D U P A 1
N31 N 0.4171(2) 0.42804(19) 0.30543(17) 0.0710(7) Uani 1 1 d . . . . .
N32 N 0.3358(2) 0.53634(19) 0.34331(19) 0.0751(8) Uani 1 1 d . . . . .
N41 N 0.5584(2) 0.3087(2) 0.21847(17) 0.0756(8) Uani 1 1 d . . . . .
N42 N 0.6336(2) 0.23446(19) 0.13617(17) 0.0728(8) Uani 1 1 d . . . . .
C11 C 0.3535(2) 0.2326(2) 0.3602(2) 0.0718(9) Uani 1 1 d . . . . .
H11 H 0.3180 0.2772 0.3459 0.086 Uiso 1 1 calc R . . . .
C12 C 0.4672(3) 0.1592(3) 0.3820(3) 0.1013(15) Uani 1 1 d D . . . .
H12 H 0.5241 0.1411 0.3853 0.122 Uiso 0.5 1 calc R . P B 2
C13 C 0.3957(3) 0.1148(3) 0.4046(3) 0.1012(16) Uani 1 1 d D . . . .
H13 H 0.3964 0.0617 0.4270 0.121 Uiso 0.5 1 calc R . P C 2
C14 C 0.4068(7) 0.0398(5) 0.4476(6) 0.089(3) Uani 0.4 1 d D . P D 1
H14 H 0.3592 0.0117 0.4672 0.107 Uiso 0.4 1 calc R . P D 1
C15 C 0.4893(8) 0.0093(8) 0.4599(8) 0.107(4) Uani 0.4 1 d D . P D 1
H15 H 0.4973 -0.0416 0.4851 0.128 Uiso 0.4 1 calc R . P D 1
C16 C 0.5602(8) 0.0548(7) 0.4347(7) 0.104(4) Uani 0.4 1 d D . P D 1
H16 H 0.6151 0.0326 0.4420 0.125 Uiso 0.4 1 calc R . P D 1
C17 C 0.5513(6) 0.1332(7) 0.3984(7) 0.097(4) Uani 0.4 1 d D . P D 1
H17 H 0.5989 0.1662 0.3860 0.116 Uiso 0.4 1 calc R . P D 1
C21 C 0.6006(3) 0.3513(3) 0.4570(2) 0.0746(10) Uani 1 1 d D . . . .
H21 H 0.5709 0.3047 0.4758 0.090 Uiso 0.5 1 calc R . P A 2
C22A C 0.6755(7) 0.3823(11) 0.3677(5) 0.121(4) Uani 0.5 1 d D U P A 1
H22A H 0.6967 0.3918 0.3203 0.145 Uiso 0.5 1 calc R . P A 1
C22B C 0.6261(9) 0.4619(9) 0.3892(6) 0.136(5) Uani 0.5 1 d D . P A 2
C23A C 0.7217(7) 0.3907(11) 0.4316(6) 0.132(5) Uani 0.5 1 d D U P A 1
H23A H 0.7781 0.4104 0.4342 0.159 Uiso 0.5 1 calc R . P A 1
C23B C 0.6718(8) 0.4706(8) 0.4571(6) 0.135(5) Uani 0.5 1 d D . P A 2
C24B C 0.7028(12) 0.5547(9) 0.4769(13) 0.094(5) Uani 0.2 1 d D U P A 2
H24B H 0.7287 0.5615 0.5229 0.113 Uiso 0.2 1 calc R . P A 2
C25B C 0.6959(14) 0.6281(11) 0.4295(11) 0.092(4) Uani 0.2 1 d D U P A 2
H25B H 0.7224 0.6795 0.4408 0.111 Uiso 0.2 1 calc R . P A 2
C26B C 0.6460(14) 0.6165(12) 0.3645(12) 0.091(4) Uani 0.2 1 d D U P A 2
H26B H 0.6378 0.6626 0.3331 0.109 Uiso 0.2 1 calc R . P A 2
C27B C 0.6076(14) 0.5372(9) 0.3452(11) 0.084(4) Uani 0.2 1 d D U P A 2
H27B H 0.5709 0.5336 0.3046 0.101 Uiso 0.2 1 calc R . P A 2
C31 C 0.4001(3) 0.4839(2) 0.3576(2) 0.0760(10) Uani 1 1 d . . . . .
H31 H 0.4313 0.4862 0.4016 0.091 Uiso 1 1 calc R . . . .
C32 C 0.3588(4) 0.4467(3) 0.2516(3) 0.1070(16) Uani 1 1 d . . . . .
H32 H 0.3540 0.4195 0.2061 0.128 Uiso 1 1 calc R . . . .
C33 C 0.3094(3) 0.5110(3) 0.2752(3) 0.1064(17) Uani 1 1 d . . . . .
H33 H 0.2639 0.5347 0.2489 0.128 Uiso 1 1 calc R . . . .
C41 C 0.5905(3) 0.2341(2) 0.1985(2) 0.0741(9) Uani 1 1 d . . . . .
H41 H 0.5829 0.1853 0.2267 0.089 Uiso 1 1 calc R . . . .
C42 C 0.5826(5) 0.3607(3) 0.1639(3) 0.118(2) Uani 1 1 d . . . . .
H42 H 0.5706 0.4184 0.1614 0.141 Uiso 1 1 calc R . . . .
C43 C 0.6275(5) 0.3160(3) 0.1132(3) 0.124(2) Uani 1 1 d . . . . .
H43 H 0.6504 0.3377 0.0695 0.149 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
N11 Co1 N21B 112.2(3) . .
N21A Co1 N11 106.0(4) . .
N21A Co1 N31 113.9(6) . .
N21A Co1 N41 107.1(5) . .
N31 Co1 N11 106.34(13) . .
N31 Co1 N21B 102.6(6) . .
N41 Co1 N11 111.32(14) . .
N41 Co1 N21B 111.8(5) . .
N41 Co1 N31 112.07(13) . .
N12 Co2 N22B 117.7(4) . 4_456
N12 Co2 N32 110.57(14) . 8_655
N12 Co2 N42 107.03(14) . 6_556
N22A Co2 N12 109.5(3) 4_456 .
N22A Co2 N32 117.7(3) 4_456 8_655
N22A Co2 N42 105.1(3) 4_456 6_556
N32 Co2 N22B 103.3(3) 8_655 4_456
N32 Co2 N42 106.25(13) 8_655 6_556
N42 Co2 N22B 111.4(3) 6_556 4_456
C11 N11 Co1 123.6(3) . .
C11 N11 C12 104.6(3) . .
C12 N11 Co1 131.7(3) . .
C11 N12 Co2 124.5(3) . .
C11 N12 C13 103.9(3) . .
C13 N12 Co2 131.5(3) . .
C21 N21B Co1 123.5(8) . .
C21 N21B C22B 107.8(10) . .
C22B N21B Co1 126.5(9) . .
C21 N21A Co1 134.9(9) . .
C21 N21A C22A 98.6(10) . .
C22A N21A Co1 126.4(8) . .
C21 N22B Co2 122.9(7) . 4_556
C21 N22B C23B 107.7(9) . .
C23B N22B Co2 127.7(8) . 4_556
C21 N22A Co2 129.3(9) . 4_556
C21 N22A C23A 99.1(9) . .
C23A N22A Co2 131.5(8) . 4_556
C31 N31 Co1 124.7(3) . .
C31 N31 C32 103.5(3) . .
C32 N31 Co1 131.5(3) . .
C31 N32 Co2 126.5(3) . 8_665
C31 N32 C33 102.8(3) . .
C33 N32 Co2 130.3(3) . 8_665
C41 N41 Co1 125.9(3) . .
C41 N41 C42 103.8(3) . .
C42 N41 Co1 129.8(3) . .
C41 N42 Co2 124.6(3) . 6_656
C41 N42 C43 103.4(3) . .
C43 N42 Co2 131.8(3) . 6_656
N12 C11 N11 114.7(3) . .
N11 C12 C17 129.0(6) . .
C13 C12 N11 107.4(4) . .
C13 C12 C17 122.8(6) . .
N12 C13 C12 109.3(4) . .
N12 C13 C14 130.8(6) . .
C12 C13 C14 119.2(6) . .
C15 C14 C13 119.1(9) . .
C14 C15 C16 120.0(11) . .
C15 C16 C17 122.0(11) . .
C12 C17 C16 116.5(10) . .
N21B C21 N22B 110.4(8) . .
N22A C21 N21A 122.0(9) . .
C23A C22A N21A 109.6(9) . .
N21B C22B C23B 106.4(9) . .
N21B C22B C27B 131.8(12) . .
C23B C22B C27B 119.3(12) . .
N22A C23A C22A 110.4(9) . .
N22B C23B C22B 105.2(9) . .
N22B C23B C24B 135.7(12) . .
C22B C23B C24B 117.7(12) . .
C25B C24B C23B 124.1(17) . .
C26B C25B C24B 115.3(16) . .
C25B C26B C27B 122.9(17) . .
C26B C27B C22B 119.9(16) . .
N31 C31 N32 115.4(4) . .
C33 C32 N31 108.4(4) . .
C32 C33 N32 109.8(4) . .
N42 C41 N41 114.9(3) . .
N41 C42 C43 109.0(4) . .
C42 C43 N42 108.9(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N11 1.984(3) .
Co1 N21B 2.067(13) .
Co1 N21A 1.915(13) .
Co1 N31 1.984(3) .
Co1 N41 1.980(3) .
Co2 N12 1.981(3) .
Co2 N22B 2.016(12) 4_456
Co2 N22A 1.949(13) 4_456
Co2 N32 1.985(3) 8_655
Co2 N42 1.990(3) 6_556
N11 C11 1.332(5) .
N11 C12 1.378(5) .
N12 C11 1.327(5) .
N12 C13 1.371(6) .
N21B C21 1.316(11) .
N21B C22B 1.366(13) .
N21A C21 1.326(11) .
N21A C22A 1.373(14) .
N22B Co2 2.016(12) 4_556
N22B C21 1.327(10) .
N22B C23B 1.374(12) .
N22A Co2 1.949(13) 4_556
N22A C21 1.308(11) .
N22A C23A 1.363(13) .
N31 C31 1.316(5) .
N31 C32 1.361(5) .
N32 Co2 1.985(3) 8_665
N32 C31 1.321(5) .
N32 C33 1.356(6) .
N41 C41 1.326(5) .
N41 C42 1.335(6) .
N42 Co2 1.990(3) 6_656
N42 C41 1.310(5) .
N42 C43 1.354(6) .
C12 C13 1.373(6) .
C12 C17 1.400(9) .
C13 C14 1.424(9) .
C14 C15 1.386(11) .
C15 C16 1.389(12) .
C16 C17 1.406(11) .
C22A C23A 1.365(15) .
C22B C23B 1.422(11) .
C22B C27B 1.457(14) .
C23B C24B 1.454(13) .
C24B C25B 1.444(15) .
C25B C26B 1.418(15) .
C26B C27B 1.428(14) .
C32 C33 1.339(7) .
C42 C43 1.349(7) .
