#------------------------------------------------------------------------------
#$Date: 2019-11-03 15:05:06 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221715 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/86/4128634.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_4128634
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                   15.342(4)
_cell_length_b                   15.808(3)
_cell_length_c                   18.030(3)
_cell_measurement_reflns_used    2230
_cell_measurement_temperature    400(2)
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.26
_cell_volume                     4372.7(16)
_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 0.996
_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  0.0431
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_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            25592
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.994
_diffrn_reflns_theta_min         2.577
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.528
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1029 before and 0.0668 after correction.
The Ratio of minimum to maximum transmission is 0.5528.
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    1.264
_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         0.365
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5250
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0432
_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)+(0.0514P)²+1.7827P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3154
_reflns_number_total             5250
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            VT_dry_ZIF-62_Co_0-30_400K.cif
_cod_data_source_block           int1_zif-62_co_1_no_guest_400k
_cod_original_cell_volume        4372.5(17)
_cod_original_formula_sum        'C7.20 H6.60 Co N4'
_cod_database_code               4128634
_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   0.461
_shelx_estimated_absorpt_t_min   0.388
_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 0.50133(3) 0.33477(3) 0.31511(3) 0.08342(17) Uani 1 1 d . . . . .
Co2 Co 0.19758(3) 0.13665(3) 0.40295(3) 0.08511(18) Uani 1 1 d . . . . .
N11 N 0.43756(18) 0.23602(18) 0.35396(17) 0.0942(8) Uani 1 1 d . . . . .
N12 N 0.3214(2) 0.16172(19) 0.38859(18) 0.0961(8) Uani 1 1 d . . . . .
N21B N 0.5872(11) 0.3826(9) 0.3911(6) 0.093(5) Uani 0.5 1 d D U P A 2
N21A N 0.5924(10) 0.3554(10) 0.3847(6) 0.090(4) Uani 0.5 1 d D U P A 1
N22B N 0.6583(7) 0.3947(5) 0.4941(7) 0.083(3) Uani 0.5 1 d D U P A 2
N22A N 0.6720(6) 0.3642(6) 0.4918(7) 0.088(3) Uani 0.5 1 d D U P A 1
N31 N 0.41674(19) 0.42799(18) 0.30601(16) 0.0910(7) Uani 1 1 d . . . . .
N32 N 0.3367(2) 0.53704(18) 0.34341(17) 0.0936(8) Uani 1 1 d . . . . .
N41 N 0.5565(2) 0.30840(19) 0.21961(16) 0.0942(8) Uani 1 1 d . . . . .
N42 N 0.63200(19) 0.23447(18) 0.13708(16) 0.0923(8) Uani 1 1 d . . . . .
C11 C 0.3525(2) 0.2325(2) 0.3606(2) 0.0916(9) Uani 1 1 d . . . . .
H11 H 0.3166 0.2771 0.3466 0.110 Uiso 1 1 calc R . . . .
C12 C 0.4651(3) 0.1599(3) 0.3817(3) 0.1259(16) Uani 1 1 d D . . . .
H12 H 0.5226 0.1417 0.3844 0.151 Uiso 0.5 1 calc R . P B 2
C13 C 0.3939(3) 0.1157(3) 0.4045(3) 0.1280(16) Uani 1 1 d D . . . .
H13 H 0.3947 0.0628 0.4272 0.154 Uiso 0.5 1 calc R . P C 2
C14 C 0.4048(7) 0.0415(5) 0.4476(6) 0.115(3) Uani 0.4 1 d D . P D 1
H14 H 0.3565 0.0140 0.4675 0.138 Uiso 0.4 1 calc R . P D 1
C15 C 0.4868(8) 0.0105(7) 0.4598(7) 0.134(4) Uani 0.4 1 d D . P D 1
H15 H 0.4947 -0.0407 0.4844 0.161 Uiso 0.4 1 calc R . P D 1
C16 C 0.5582(8) 0.0567(7) 0.4349(7) 0.133(4) Uani 0.4 1 d D . P D 1
H16 H 0.6139 0.0351 0.4425 0.159 Uiso 0.4 1 calc R . P D 1
C17 C 0.5489(6) 0.1344(6) 0.3989(6) 0.116(3) Uani 0.4 1 d D . P D 1
H17 H 0.5970 0.1676 0.3870 0.140 Uiso 0.4 1 calc R . P D 1
C21 C 0.5987(2) 0.3513(2) 0.4577(2) 0.0930(10) Uani 1 1 d D . . . .
H21 H 0.5690 0.3048 0.4766 0.112 Uiso 0.5 1 calc R . P A 2
C22A C 0.6752(6) 0.3783(10) 0.3683(5) 0.150(4) Uani 0.5 1 d D U P A 1
H22A H 0.6972 0.3873 0.3209 0.180 Uiso 0.5 1 calc R . P A 1
C22B C 0.6258(7) 0.4584(8) 0.3889(6) 0.150(4) Uani 0.5 1 d D . P A 2
C23A C 0.7204(6) 0.3860(10) 0.4320(5) 0.157(5) Uani 0.5 1 d D U P A 1
H23A H 0.7780 0.4041 0.4346 0.189 Uiso 0.5 1 calc R . P A 1
C23B C 0.6713(7) 0.4680(7) 0.4572(6) 0.156(4) Uani 0.5 1 d D . P A 2
C24B C 0.7026(12) 0.5525(9) 0.4784(12) 0.125(5) Uani 0.2 1 d D U P A 2
H24B H 0.7287 0.5591 0.5247 0.149 Uiso 0.2 1 calc R . P A 2
C25B C 0.6948(14) 0.6267(11) 0.4305(11) 0.119(4) Uani 0.2 1 d D U P A 2
H25B H 0.7206 0.6782 0.4421 0.142 Uiso 0.2 1 calc R . P A 2
C26B C 0.6447(14) 0.6147(12) 0.3642(11) 0.118(4) Uani 0.2 1 d D U P A 2
H26B H 0.6368 0.6605 0.3326 0.142 Uiso 0.2 1 calc R . P A 2
C27B C 0.6058(13) 0.5343(9) 0.3444(11) 0.112(5) Uani 0.2 1 d D U P A 2
H27B H 0.5684 0.5306 0.3039 0.135 Uiso 0.2 1 calc R . P A 2
C31 C 0.4002(2) 0.4844(2) 0.3577(2) 0.0936(10) Uani 1 1 d . . . . .
H31 H 0.4318 0.4866 0.4018 0.112 Uiso 1 1 calc R . . . .
C32 C 0.3584(3) 0.4462(3) 0.2531(3) 0.1307(16) Uani 1 1 d . . . . .
H32 H 0.3526 0.4183 0.2080 0.157 Uiso 1 1 calc R . . . .
C33 C 0.3099(3) 0.5113(3) 0.2761(3) 0.1335(17) Uani 1 1 d . . . . .
H33 H 0.2642 0.5352 0.2495 0.160 Uiso 1 1 calc R . . . .
C41 C 0.5891(2) 0.2345(2) 0.1994(2) 0.0956(10) Uani 1 1 d . . . . .
H41 H 0.5818 0.1858 0.2277 0.115 Uiso 1 1 calc R . . . .
C42 C 0.5802(4) 0.3591(3) 0.1646(3) 0.1405(19) Uani 1 1 d . . . . .
H42 H 0.5672 0.4164 0.1615 0.169 Uiso 1 1 calc R . . . .
C43 C 0.6255(4) 0.3154(3) 0.1143(3) 0.151(2) Uani 1 1 d . . . . .
H43 H 0.6488 0.3373 0.0707 0.181 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 112.0(3) . .
N21A Co1 N11 105.4(4) . .
N21A Co1 N31 114.2(6) . .
N21A Co1 N41 107.3(4) . .
N31 Co1 N11 107.16(12) . .
N31 Co1 N21B 101.7(5) . .
N41 Co1 N11 110.94(13) . .
N41 Co1 N21B 112.8(5) . .
N41 Co1 N31 111.68(12) . .
N12 Co2 N22B 117.5(3) . 4_456
N12 Co2 N32 110.34(13) . 8_655
N12 Co2 N42 106.65(12) . 6_556
N22A Co2 N12 109.1(3) 4_456 .
N22A Co2 N32 118.2(3) 4_456 8_655
N22A Co2 N42 105.0(3) 4_456 6_556
N32 Co2 N22B 103.0(3) 8_655 4_456
N32 Co2 N42 106.79(12) 8_655 6_556
N42 Co2 N22B 112.1(3) 6_556 4_456
C11 N11 Co1 124.0(2) . .
C11 N11 C12 103.7(3) . .
C12 N11 Co1 132.3(3) . .
C11 N12 Co2 125.1(2) . .
C11 N12 C13 103.8(3) . .
C13 N12 Co2 131.1(3) . .
C21 N21B Co1 124.1(8) . .
C21 N21B C22B 107.8(9) . .
C22B N21B Co1 126.6(8) . .
C21 N21A Co1 134.5(9) . .
C21 N21A C22A 99.3(10) . .
C22A N21A Co1 126.1(8) . .
C21 N22B Co2 122.7(7) . 4_556
C21 N22B C23B 107.6(8) . .
C23B N22B Co2 128.4(7) . 4_556
C21 N22A Co2 129.8(8) . 4_556
C21 N22A C23A 97.9(9) . .
C23A N22A Co2 132.1(8) . 4_556
C31 N31 Co1 125.1(2) . .
C31 N31 C32 103.3(3) . .
C32 N31 Co1 131.4(3) . .
C31 N32 Co2 126.7(3) . 8_665
C31 N32 C33 102.3(3) . .
C33 N32 Co2 130.5(3) . 8_665
C41 N41 Co1 126.3(2) . .
C41 N41 C42 102.9(3) . .
C42 N41 Co1 130.3(3) . .
C41 N42 Co2 124.9(2) . 6_656
C41 N42 C43 103.0(3) . .
C43 N42 Co2 131.9(3) . 6_656
N11 C11 N12 115.6(3) . .
N11 C12 C17 128.7(6) . .
C13 C12 N11 108.4(4) . .
C13 C12 C17 121.9(6) . .
N12 C13 C12 108.5(4) . .
N12 C13 C14 130.9(6) . .
C12 C13 C14 119.8(6) . .
C15 C14 C13 119.5(9) . .
C14 C15 C16 119.0(10) . .
C15 C16 C17 122.1(10) . .
C12 C17 C16 117.1(9) . .
N21B C21 N22B 110.7(8) . .
N22A C21 N21A 121.9(9) . .
N21A C22A C23A 108.7(8) . .
N21B C22B C23B 106.7(9) . .
N21B C22B C27B 130.7(11) . .
C23B C22B C27B 119.1(12) . .
N22A C23A C22A 111.9(8) . .
N22B C23B C22B 105.2(9) . .
N22B C23B C24B 134.4(11) . .
C22B C23B C24B 118.8(12) . .
C25B C24B C23B 123.2(16) . .
C26B C25B C24B 115.5(16) . .
C25B C26B C27B 122.9(17) . .
C26B C27B C22B 119.5(16) . .
N32 C31 N31 115.8(3) . .
C33 C32 N31 108.5(4) . .
C32 C33 N32 110.0(4) . .
N42 C41 N41 115.5(3) . .
N41 C42 C43 109.8(4) . .
C42 C43 N42 108.8(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N11 1.971(3) .
Co1 N21B 2.046(12) .
Co1 N21A 1.907(13) .
Co1 N31 1.970(3) .
Co1 N41 1.963(3) .
Co2 N12 1.957(3) .
Co2 N22B 2.013(11) 4_456
Co2 N22A 1.937(12) 4_456
Co2 N32 1.977(3) 8_655
Co2 N42 1.981(3) 6_556
N11 C11 1.312(4) .
N11 C12 1.369(5) .
N12 C11 1.317(4) .
N12 C13 1.360(5) .
N21B C21 1.310(11) .
N21B C22B 1.337(12) .
N21A C21 1.320(11) .
N21A C22A 1.353(13) .
N22B Co2 2.013(11) 4_556
N22B C21 1.318(10) .
N22B C23B 1.352(11) .
N22A Co2 1.937(12) 4_556
N22A C21 1.298(10) .
N22A C23A 1.355(12) .
N31 C31 1.315(4) .
N31 C32 1.339(5) .
N32 Co2 1.977(3) 8_665
N32 C31 1.308(4) .
N32 C33 1.344(5) .
N41 C41 1.322(4) .
N41 C42 1.326(5) .
N42 Co2 1.981(3) 6_656
N42 C41 1.302(4) .
N42 C43 1.348(5) .
C12 C13 1.360(5) .
C12 C17 1.383(9) .
C13 C14 1.417(9) .
C14 C15 1.368(11) .
C15 C16 1.390(11) .
C16 C17 1.398(11) .
C22A C23A 1.347(13) .
C22B C23B 1.424(10) .
C22B C27B 1.476(13) .
C23B C24B 1.470(13) .
C24B C25B 1.462(14) .
C25B C26B 1.433(14) .
C26B C27B 1.448(14) .
C32 C33 1.335(6) .
C42 C43 1.335(6) .
