#------------------------------------------------------------------------------
#$Date: 2019-11-03 15:04:13 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221712 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/86/4128631.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_4128631
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             2018-10-29
_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                   15.487(3)
_cell_length_b                   15.520(2)
_cell_length_c                   18.108(3)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      29.43
_cell_measurement_theta_min      2.61
_cell_volume                     4352.4(12)
_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 0.997
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0215
_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       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35183
_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         27.994
_diffrn_reflns_theta_min         2.856
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1232 before and 0.0523 after correction.
The Ratio of minimum to maximum transmission is 0.7785.
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    1.179
_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         0.178
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         5240
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0307
_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)+(0.0378P)²+1.0490P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0922
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3816
_reflns_number_total             5240
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            VT_dry_ZIF-4_Co_300K.cif
_cod_data_source_block           mo_zif-4_co_300k
_cod_original_cell_volume        4352.5(12)
_cod_database_code               4128631
_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   0.624
_shelx_estimated_absorpt_t_min   0.501
_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 0.50642(2) 0.33964(2) 0.31254(2) 0.06553(10) Uani 1 1 d . . . .
Co2 Co 0.20269(2) 0.14079(2) 0.40493(2) 0.06734(11) Uani 1 1 d . . . .
N11 N 0.44283(12) 0.23795(12) 0.35082(11) 0.0752(5) Uani 1 1 d . . . .
N12 N 0.32735(13) 0.16374(12) 0.38822(11) 0.0735(5) Uani 1 1 d . . . .
N21 N 0.59649(12) 0.37062(14) 0.38566(10) 0.0783(5) Uani 1 1 d D . . .
N22 N 0.67160(13) 0.37835(14) 0.49065(10) 0.0813(5) Uani 1 1 d D . . .
N31 N 0.42092(12) 0.43439(11) 0.30518(9) 0.0697(4) Uani 1 1 d . . . .
N32 N 0.33608(12) 0.54164(12) 0.34424(10) 0.0722(5) Uani 1 1 d . . . .
N41 N 0.56160(12) 0.31648(12) 0.21561(10) 0.0728(5) Uani 1 1 d . . . .
N42 N 0.63792(12) 0.24190(12) 0.13328(10) 0.0723(5) Uani 1 1 d . . . .
C11 C 0.35761(14) 0.23569(14) 0.35812(12) 0.0736(6) Uani 1 1 d . . . .
H11 H 0.3212 0.2817 0.3431 0.088 Uiso 1 1 calc R . . .
C21 C 0.60414(14) 0.34942(14) 0.45513(12) 0.0726(6) Uani 1 1 d . . . .
H21 H 0.5623 0.3143 0.4789 0.087 Uiso 1 1 calc R . . .
C22A C 0.6800(6) 0.3919(8) 0.3679(6) 0.136(5) Uani 0.5 1 d D P A 1
H22A H 0.7017 0.4026 0.3198 0.163 Uiso 0.5 1 calc R P A 1
C23A C 0.7261(6) 0.3948(8) 0.4323(5) 0.142(5) Uani 0.5 1 d D P A 1
H23A H 0.7861 0.4064 0.4361 0.171 Uiso 0.5 1 calc R P A 1
C31 C 0.40151(14) 0.48916(14) 0.35861(12) 0.0708(5) Uani 1 1 d . . . .
H31 H 0.4322 0.4908 0.4040 0.085 Uiso 1 1 calc R . . .
C32 C 0.36296(19) 0.45406(17) 0.25139(15) 0.0968(8) Uani 1 1 d . . . .
H32 H 0.3590 0.4267 0.2046 0.116 Uiso 1 1 calc R . . .
C33 C 0.31203(19) 0.51860(18) 0.27518(16) 0.0989(9) Uani 1 1 d . . . .
H33 H 0.2663 0.5440 0.2478 0.119 Uiso 1 1 calc R . . .
C41 C 0.59200(15) 0.24095(15) 0.19478(12) 0.0737(6) Uani 1 1 d . . . .
H41 H 0.5817 0.1896 0.2220 0.088 Uiso 1 1 calc R . . .
C42 C 0.5903(2) 0.37054(18) 0.16383(16) 0.1142(11) Uani 1 1 d . . . .
H42 H 0.5802 0.4309 0.1626 0.137 Uiso 1 1 calc R . . .
C43 C 0.6363(2) 0.32551(19) 0.11329(16) 0.1171(12) Uani 1 1 d . . . .
H43 H 0.6631 0.3491 0.0706 0.140 Uiso 1 1 calc R . . .
C13A C 0.39941(19) 0.11684(19) 0.40171(18) 0.1077(10) Uani 1 1 d . . . .
H13A H 0.4005 0.0613 0.4238 0.129 Uiso 1 1 calc R . . .
C12A C 0.4697(2) 0.16141(19) 0.3789(2) 0.1122(10) Uani 1 1 d . . . .
H12A H 0.5279 0.1423 0.3819 0.135 Uiso 1 1 calc R . . .
C22B C 0.6490(6) 0.4434(7) 0.3834(5) 0.122(4) Uani 0.5 1 d . P A 2
H22B H 0.6520 0.4835 0.3438 0.147 Uiso 0.5 1 calc R P A 2
C23B C 0.6950(6) 0.4476(6) 0.4463(6) 0.122(3) Uani 0.5 1 d . P A 2
H23B H 0.7363 0.4905 0.4584 0.146 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 107.98(8) . .
N21 Co1 N31 109.56(8) . .
N21 Co1 N41 109.36(8) . .
N31 Co1 N11 106.36(8) . .
N31 Co1 N41 111.25(7) . .
N41 Co1 N11 112.23(8) . .
N12 Co2 N42 107.23(8) . 6_556
N22 Co2 N12 114.21(8) 4_456 .
N22 Co2 N32 109.88(8) 4_456 8_655
N22 Co2 N42 109.23(8) 4_456 6_556
N32 Co2 N12 110.41(8) 8_655 .
N32 Co2 N42 105.48(8) 8_655 6_556
C11 N11 Co1 123.32(16) . .
C11 N11 C12A 104.2(2) . .
C12A N11 Co1 132.38(18) . .
C11 N12 Co2 123.79(16) . .
C11 N12 C13A 103.6(2) . .
C13A N12 Co2 132.61(17) . .
C21 N21 Co1 130.26(16) . .
C21 N21 C22A 101.6(5) . .
C21 N21 C22B 100.4(4) . .
C22A N21 Co1 124.4(5) . .
C22B N21 Co1 126.0(4) . .
C21 N22 Co2 127.95(15) . 4_556
C21 N22 C23A 100.1(5) . .
C21 N22 C23B 100.9(4) . .
C23A N22 Co2 127.9(5) . 4_556
C23B N22 Co2 127.3(5) . 4_556
C31 N31 Co1 125.40(14) . .
C31 N31 C32 103.28(19) . .
C32 N31 Co1 130.96(16) . .
C31 N32 Co2 126.80(15) . 8_665
C31 N32 C33 103.27(19) . .
C33 N32 Co2 129.32(16) . 8_665
C41 N41 Co1 124.59(15) . .
C41 N41 C42 103.82(19) . .
C42 N41 Co1 130.61(17) . .
C41 N42 Co2 123.81(16) . 6_656
C41 N42 C43 103.1(2) . .
C43 N42 Co2 132.58(17) . 6_656
N11 C11 N12 114.5(2) . .
N21 C21 N22 117.4(2) . .
C23A C22A N21 107.5(7) . .
C22A C23A N22 109.1(7) . .
N31 C31 N32 115.15(19) . .
C33 C32 N31 109.0(2) . .
C32 C33 N32 109.3(2) . .
N41 C41 N42 115.0(2) . .
N41 C42 C43 109.0(2) . .
N42 C43 C42 109.0(2) . .
N12 C13A C12A 109.4(2) . .
C13A C12A N11 108.3(3) . .
C23B C22B N21 108.9(7) . .
C22B C23B N22 108.3(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N11 1.9853(18) .
Co1 N21 1.9824(19) .
Co1 N31 1.9833(18) .
Co1 N41 1.9850(18) .
Co2 N12 1.986(2) .
Co2 N22 1.9737(19) 4_456
Co2 N32 1.9841(18) 8_655
Co2 N42 1.9867(18) 6_556
N11 C11 1.327(3) .
N11 C12A 1.357(3) .
N12 C11 1.328(3) .
N12 C13A 1.354(3) .
N21 C21 1.306(3) .
N21 C22A 1.372(8) .
N21 C22B 1.393(10) .
N22 Co2 1.9737(19) 4_556
N22 C21 1.306(3) .
N22 C23A 1.376(8) .
N22 C23B 1.389(9) .
N31 C31 1.322(3) .
N31 C32 1.359(3) .
N32 Co2 1.9841(18) 8_665
N32 C31 1.326(3) .
N32 C33 1.353(3) .
N41 C41 1.318(3) .
N41 C42 1.335(3) .
N42 Co2 1.9867(18) 6_656
N42 C41 1.322(3) .
N42 C43 1.347(3) .
C22A C23A 1.368(14) .
C32 C33 1.346(3) .
C42 C43 1.354(4) .
C13A C12A 1.355(4) .
C22B C23B 1.345(14) .
