#------------------------------------------------------------------------------
#$Date: 2019-11-25 12:41:09 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240880 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/04/4130452.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_4130452
loop_
_publ_author_name
'Xiao, Dianne J.'
'Gonzalez, Miguel I.'
'Darago, Lucy E.'
'Vogiatzis, Konstantinos D.'
'Haldoupis, Emmanuel'
'Gagliardi, Laura'
'Long, Jeffrey R.'
_publ_section_title
;
 Selective, Tunable O2 Binding in Cobalt(II)-Triazolate/Pyrazolate
 Metal-Organic Frameworks.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7161
_journal_page_last               7170
_journal_paper_doi               10.1021/jacs.6b03680
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         '(C264 H264 Cl6 Co24 N168 O24) Co3'
_chemical_formula_sum            'C264 H264 Cl6 Co24 N168 O24'
_chemical_formula_weight         7978.06
_chemical_name_common            'Co-BTTri-DMF 100 K'
_space_group_crystal_system      cubic
_space_group_IT_number           226
_space_group_name_Hall           '-F 4a 2 3'
_space_group_name_H-M_alt        'F m -3 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-02-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.4139(16)
_cell_length_b                   37.4139(16)
_cell_length_c                   37.4139(16)
_cell_measurement_reflns_used    9310
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.035
_cell_measurement_theta_min      2.655
_cell_volume                     52372(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'channel-cut Si(111) crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            182403
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         30.204
_diffrn_reflns_theta_min         2.056
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0959 before and 0.0596 after correction.
The Ratio of minimum to maximum transmission is 0.9378.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.012
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             14040
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.436
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         2643
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0671
_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)+(0.1230P)²+463.8264P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1996
_refine_ls_wR_factor_ref         0.2164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2239
_reflns_number_total             2643
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b03680_si_002.cif
_cod_data_source_block           Co-BTTri-DMF-100K
_cod_original_cell_volume        52372(7)
_cod_original_sg_symbol_Hall     '-F 4c 2 3'
_cod_database_code               4130452
_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   0.922
_shelx_estimated_absorpt_t_min   0.922
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N4B-C5B \\sim N4A-C5A
 with sigma of 0.02
 O1-C5B \\sim O1-C5A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C5B \\sim C5A \\sim N4A \\sim N4B \\sim O1: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O1, N4A, C5A, N4B, C5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N4A(0.375) C5A(0.375) N4B(0.125) C5B(0.125)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y+1/2, x+1, -z+1'
'-y+1/2, -x+1, -z+1'
'y+1/2, -x+1, z+1'
'-y+1/2, x+1, z+1'
'x+1/2, z+1, -y+1'
'-x+1/2, z+1, y+1'
'-x+1/2, -z+1, -y+1'
'x+1/2, -z+1, y+1'
'z+1/2, y+1, -x+1'
'z+1/2, -y+1, x+1'
'-z+1/2, y+1, x+1'
'-z+1/2, -y+1, -x+1'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1, x+1/2, -z+1'
'-y+1, -x+1/2, -z+1'
'y+1, -x+1/2, z+1'
'-y+1, x+1/2, z+1'
'x+1, z+1/2, -y+1'
'-x+1, z+1/2, y+1'
'-x+1, -z+1/2, -y+1'
'x+1, -z+1/2, y+1'
'z+1, y+1/2, -x+1'
'z+1, -y+1/2, x+1'
'-z+1, y+1/2, x+1'
'-z+1, -y+1/2, -x+1'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1, x+1, -z+1/2'
'-y+1, -x+1, -z+1/2'
'y+1, -x+1, z+1/2'
'-y+1, x+1, z+1/2'
'x+1, z+1, -y+1/2'
'-x+1, z+1, y+1/2'
'-x+1, -z+1, -y+1/2'
'x+1, -z+1, y+1/2'
'z+1, y+1, -x+1/2'
'z+1, -y+1, x+1/2'
'-z+1, y+1, x+1/2'
'-z+1, -y+1, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-1/2, z-1/2'
'-y-1/2, x-1/2, -z-1/2'
'y-1/2, -x-1/2, -z-1/2'
'-x-1/2, -z-1/2, y-1/2'
'x-1/2, -z-1/2, -y-1/2'
'x-1/2, z-1/2, y-1/2'
'-x-1/2, z-1/2, -y-1/2'
'-z-1/2, -y-1/2, x-1/2'
'-z-1/2, y-1/2, -x-1/2'
'z-1/2, -y-1/2, -x-1/2'
'z-1/2, y-1/2, x-1/2'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y-1/2, -x, z'
'y-1/2, x, z'
'-y-1/2, x, -z'
'y-1/2, -x, -z'
'-x-1/2, -z, y'
'x-1/2, -z, -y'
'x-1/2, z, y'
'-x-1/2, z, -y'
'-z-1/2, -y, x'
'-z-1/2, y, -x'
'z-1/2, -y, -x'
'z-1/2, y, x'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'-y, -x-1/2, z'
'y, x-1/2, z'
'-y, x-1/2, -z'
'y, -x-1/2, -z'
'-x, -z-1/2, y'
'x, -z-1/2, -y'
'x, z-1/2, y'
'-x, z-1/2, -y'
'-z, -y-1/2, x'
'-z, y-1/2, -x'
'z, -y-1/2, -x'
'z, y-1/2, x'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y, -x, z-1/2'
'y, x, z-1/2'
'-y, x, -z-1/2'
'y, -x, -z-1/2'
'-x, -z, y-1/2'
'x, -z, -y-1/2'
'x, z, y-1/2'
'-x, z, -y-1/2'
'-z, -y, x-1/2'
'-z, y, -x-1/2'
'z, -y, -x-1/2'
'z, y, x-1/2'
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 0.5000 0.24617(2) 0.31633(2) 0.0311(3) Uani 1 2 d S T P . .
Cl1 Cl 0.5000 0.2500 0.2500 0.0375(5) Uani 1 8 d S T P . .
O1 O 0.5000 0.24525(11) 0.37403(11) 0.0490(9) Uani 1 2 d DS TU P . .
N2 N 0.53736(7) 0.31172(8) 0.29232(8) 0.0334(6) Uani 1 1 d . . . . .
N1 N 0.53752(7) 0.28479(8) 0.31631(7) 0.0323(6) Uani 1 1 d . . . . .
N3 N 0.56476(7) 0.33353(8) 0.29778(8) 0.0360(6) Uani 1 1 d . . . . .
C2 C 0.58313(9) 0.32014(9) 0.32616(9) 0.0339(7) Uani 1 1 d . . . . .
C1 C 0.56580(8) 0.28973(9) 0.33755(9) 0.0351(7) Uani 1 1 d . . . . .
H1 H 0.5727 0.2749 0.3570 0.042 Uiso 1 1 calc R . . . .
C3 C 0.61540(9) 0.33744(9) 0.34016(9) 0.0339(7) Uani 1 1 d . . . . .
C4 C 0.62962(9) 0.36758(9) 0.32359(9) 0.0342(7) Uani 1 1 d . . . . .
H4 H 0.6186 0.3767 0.3026 0.041 Uiso 1 1 calc R . . . .
N4A N 0.5000 0.2244(5) 0.4283(4) 0.174(6) Uani 0.75 2 d DS TU P A 2
C5A C 0.5169(5) 0.2299(5) 0.3933(5) 0.107(5) Uani 0.375 1 d D U . A 2
N4B N 0.5000 0.2667(16) 0.4318(11) 0.183(13) Uani 0.25 2 d DS TU P A 1
C5B C 0.5138(13) 0.2607(14) 0.3954(10) 0.117(9) Uani 0.125 1 d D U . A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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'
Cl Cl 0.1484 0.1585 '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 0.0080 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0140 0.0070 '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
O1 Co1 Cl1 177.61(11) . .
N2 Co1 Cl1 87.46(8) 68_454 .
N2 Co1 Cl1 87.46(8) 161_665 .
N2 Co1 O1 94.25(11) 68_454 .
N2 Co1 O1 94.25(11) 161_665 .
N2 Co1 N2 87.88(15) 161_665 68_454
N2 Co1 N1 175.06(12) 161_665 .
N2 Co1 N1 91.67(10) 68_454 .
N2 Co1 N1 91.67(10) 161_665 100_655
N2 Co1 N1 175.06(12) 68_454 100_655
N1 Co1 Cl1 87.60(8) 100_655 .
N1 Co1 Cl1 87.60(8) . .
N1 Co1 O1 90.69(11) . .
N1 Co1 O1 90.69(11) 100_655 .
N1 Co1 N1 88.36(15) . 100_655
Co1 Cl1 Co1 180.0 . 121_655
Co1 Cl1 Co1 180.00(3) 161_665 89_445
Co1 Cl1 Co1 90.0 89_445 .
Co1 Cl1 Co1 90.0 161_665 121_655
Co1 Cl1 Co1 90.0 89_445 121_655
Co1 Cl1 Co1 90.0 161_665 .
C5A O1 Co1 130.8(11) . .
C5A O1 Co1 130.8(11) 100_655 .
C5A O1 C5A 69(2) . 100_655
C5B O1 Co1 135(3) 100_655 .
C5B O1 Co1 135(3) . .
C5B O1 C5B 55(6) . 100_655
N1 N2 Co1 122.9(2) . 89_445
N3 N2 Co1 126.4(2) . 89_445
N3 N2 N1 110.7(3) . .
N2 N1 Co1 122.2(2) . .
C1 N1 Co1 130.6(2) . .
C1 N1 N2 107.2(3) . .
N2 N3 C2 106.5(3) . .
N3 C2 C1 107.9(3) . .
N3 C2 C3 122.2(3) . .
C1 C2 C3 129.9(3) . .
N1 C1 C2 107.6(3) . .
N1 C1 H1 126.2 . .
C2 C1 H1 126.2 . .
C4 C3 C2 120.8(3) . .
C4 C3 C2 120.1(3) 10_656 .
C4 C3 C4 119.1(3) . 10_656
C3 C4 C3 120.9(3) . 7_665
C3 C4 H4 119.6 . .
C3 C4 H4 119.6 7_665 .
C5A N4A C5A 51.0(14) 100_655 .
O1 C5A N4A 113.8(15) . .
C5B N4B C5B 41(4) 100_655 .
O1 C5B N4B 125(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 Cl1 2.4859(7) .
Co1 O1 2.159(4) .
Co1 N2 2.014(3) 161_665
Co1 N2 2.014(3) 68_454
Co1 N1 2.015(3) .
Co1 N1 2.015(3) 100_655
Cl1 Co1 2.4859(7) 121_655
Cl1 Co1 2.4859(7) 161_665
Cl1 Co1 2.4859(7) 89_445
O1 C5A 1.116(15) 100_655
O1 C5A 1.116(15) .
O1 C5B 1.11(2) .
O1 C5B 1.11(2) 100_655
N2 Co1 2.014(3) 89_445
N2 N1 1.349(4) .
N2 N3 1.326(4) .
N1 C1 1.336(4) .
N3 C2 1.360(4) .
C2 C1 1.377(5) .
C2 C3 1.467(5) .
C1 H1 0.9500 .
C3 C4 1.393(4) .
C3 C4 1.397(4) 10_656
C4 C3 1.397(4) 7_665
C4 H4 0.9500 .
N4A C5A 1.47(2) 100_655
N4A C5A 1.47(2) .
N4B C5B 1.48(3) 100_655
N4B C5B 1.48(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Co1 O1 C5A N4A -155.4(10) . .
Co1 O1 C5B N4B 153(4) . .
Co1 N2 N1 Co1 -0.3(3) 89_445 .
Co1 N2 N1 C1 179.5(2) 89_445 .
Co1 N2 N3 C2 -179.4(2) 89_445 .
Co1 N1 C1 C2 179.7(2) . .
N2 N1 C1 C2 -0.2(4) . .
N2 N3 C2 C1 -0.2(4) . .
N2 N3 C2 C3 -179.8(3) . .
N1 N2 N3 C2 0.1(4) . .
N3 N2 N1 Co1 -179.8(2) . .
N3 N2 N1 C1 0.1(3) . .
N3 C2 C1 N1 0.2(4) . .
N3 C2 C3 C4 177.1(3) . 10_656
N3 C2 C3 C4 -3.3(5) . .
C2 C3 C4 C3 178.4(2) . 7_665
C1 C2 C3 C4 -2.5(6) . 10_656
C1 C2 C3 C4 177.1(4) . .
C3 C2 C1 N1 179.8(3) . .
C4 C3 C4 C3 -2.0(7) 10_656 7_665
C5A O1 C5A N4A -29(2) 100_655 .
C5A N4A C5A O1 26(2) 100_655 .
C5B O1 C5B N4B 31(8) 100_655 .
C5B N4B C5B O1 -29(7) 100_655 .
