#------------------------------------------------------------------------------
#$Date: 2019-11-25 12:38:52 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240879 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/04/4130448.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_4130448
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         '(C140 H140 Cl3 Co12 N76 O12) Co1.4 O1.4'
_chemical_formula_sum            'C140 H140 Cl3 Co14.4 N76 O14.4'
_chemical_formula_weight         4072.57
_chemical_name_common            Co-BDTriP-DMF
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_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            1
_cell_length_a                   18.8345(7)
_cell_length_b                   18.8345(7)
_cell_length_c                   18.8345(7)
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.174
_cell_measurement_theta_min      2.636
_cell_volume                     6681.3(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0696
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            97274
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         30.174
_diffrn_reflns_theta_min         2.358
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1253 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.9275.
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             1683
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0462
_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)+(0.0916P)²+6.3029P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1404
_reflns_number_total             1577
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b03680_si_001.cif
_cod_data_source_block           Co-BDTriP-DMF
_cod_original_cell_volume        6681.3(7)
_cod_original_formula_sum        'C140 H140 Cl3 Co14.40 N76 O14.40'
_cod_database_code               4130448
_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   0.911
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{N2, C1}
3. Uiso/Uaniso restraints and constraints
Co2 \\sim O2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(N2) = Uanis(C1)
4. Others
 Fixed Sof: C1(0.6667) H1(0.6667) Co2(0.05) O2(0.05) N2(0.3333)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C1(H1)
;
_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, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-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, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
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 0.36808(4) 0.0000 0.5000 0.0317(2) Uani 1 4 d S T P A .
Cl1 Cl 0.5000 0.0000 0.5000 0.0315(5) Uani 1 16 d S T P . .
O1 O 0.2488(2) 0.0000 0.5000 0.0596(11) Uani 1 4 d S T P . .
N1 N 0.37154(10) 0.07406(9) 0.57762(11) 0.0353(5) Uani 1 1 d . . . . .
C2 C 0.35155(13) 0.16474(16) 0.64845(13) 0.0348(7) Uani 1 2 d S T P . .
C3 C 0.32005(12) 0.22839(17) 0.67995(12) 0.0335(7) Uani 1 2 d S T P A .
C4 C 0.34951(18) 0.25930(12) 0.74070(12) 0.0340(7) Uani 1 2 d S T P . .
H4 H 0.3905 0.2385 0.7615 0.041 Uiso 1 2 calc RS T P A .
C1 C 0.32826(12) 0.12903(10) 0.58949(11) 0.0368(5) Uani 0.6667 1 d . . . A 1
H1 H 0.2880 0.1413 0.5617 0.044 Uiso 0.6667 1 calc R . . A 1
Co2 Co 0.2808(4) 0.1567(3) 0.5000 0.0558(14) Uani 0.1 2 d S TU P A 2
O2 O 0.1736(11) 0.1736(11) 0.5000 0.065(7) Uani 0.2 4 d S TU P A 2
N2 N 0.32826(12) 0.12903(10) 0.58949(11) 0.0368(5) Uani 0.3333 1 d . . . 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 0.0040 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 180.0 . .
N1 Co1 Cl1 88.16(6) 4_556 .
N1 Co1 Cl1 88.16(6) 27 .
N1 Co1 Cl1 88.16(6) . .
N1 Co1 Cl1 88.16(6) 26_556 .
N1 Co1 O1 91.84(6) 4_556 .
N1 Co1 O1 91.84(6) . .
N1 Co1 O1 91.84(6) 27 .
N1 Co1 O1 91.84(6) 26_556 .
N1 Co1 N1 87.26(10) 27 .
N1 Co1 N1 176.31(12) 4_556 .
N1 Co1 N1 87.26(10) 4_556 26_556
N1 Co1 N1 92.62(10) 26_556 .
N1 Co1 N1 92.62(10) 4_556 27
N1 Co1 N1 176.32(12) 27 26_556
Co1 Cl1 Co1 90.0 45_655 .
Co1 Cl1 Co1 90.0 . 21_556
Co1 Cl1 Co1 180.0 . 25_656
Co1 Cl1 Co1 90.0 25_656 21_556
Co1 Cl1 Co1 180.0 45_655 21_556
Co1 Cl1 Co1 90.0 45_655 25_656
N1 N1 Co1 122.28(5) 46_656 .
C1 N1 Co1 129.49(16) . .
C1 N1 N1 108.23(13) . 46_656
N2 N1 Co1 129.49(16) . .
N2 N1 N1 108.23(13) . 46_656
C1 C2 C3 126.93(14) 46_656 .
C1 C2 C3 126.93(14) . .
C1 C2 C1 106.1(3) 46_656 .
N2 C2 C3 126.93(14) . .
N2 C2 C3 126.93(14) 46_656 .
N2 C2 N2 106.1(3) 46_656 .
C4 C3 C2 120.79(16) 11_566 .
C4 C3 C2 120.79(16) . .
C4 C3 C4 118.4(3) . 11_566
C3 C4 C3 121.6(3) 8_656 .
C3 C4 H4 119.2 . .
C3 C4 H4 119.2 8_656 .
N1 C1 C2 108.7(2) . .
N1 C1 H1 125.7 . .
C2 C1 H1 125.7 . .
N2 Co2 O2 119.2(3) . .
N2 Co2 O2 119.2(3) 26_556 .
N2 Co2 N2 116.9(3) . 26_556
Co2 O2 Co2 108.0(13) . 13_556
N1 N2 C2 108.7(2) . .
N1 N2 Co2 109.7(2) . .
C2 N2 Co2 134.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 Cl1 2.4846(7) .
Co1 O1 2.248(5) .
Co1 N1 2.022(2) 26_556
Co1 N1 2.022(2) 27
Co1 N1 2.022(2) 4_556
Co1 N1 2.022(2) .
Cl1 Co1 2.4846(7) 45_655
Cl1 Co1 2.4846(7) 21_556
Cl1 Co1 2.4846(7) 25_656
N1 N1 1.355(4) 46_656
N1 C1 1.337(3) .
N1 N2 1.337(3) .
C2 C3 1.463(4) .
C2 C1 1.370(3) .
C2 C1 1.370(3) 46_656
C2 N2 1.370(3) 46_656
C2 N2 1.370(3) .
C3 C4 1.399(2) .
C3 C4 1.399(2) 11_566
C4 C3 1.399(2) 8_656
C4 H4 0.9500 .
C1 H1 0.9500 .
Co2 O2 2.044(18) .
Co2 N2 1.978(4) .
Co2 N2 1.978(4) 26_556
O2 Co2 2.044(18) 13_556
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 N1 C1 C2 -179.98(19) . .
Co1 N1 N2 C2 -179.98(19) . .
Co1 N1 N2 Co2 -24.1(3) . .
N1 N1 C1 C2 0.1(2) 46_656 .
N1 N1 N2 C2 0.1(2) 46_656 .
N1 N1 N2 Co2 156.0(2) 46_656 .
C2 C3 C4 C3 -179.9(2) . 8_656
C3 C2 C1 N1 179.6(3) . .
C3 C2 N2 N1 179.6(3) . .
C3 C2 N2 Co2 32.5(6) . .
C4 C3 C4 C3 -0.6(7) 11_566 8_656
C1 C2 C3 C4 -179.8(3) 46_656 11_566
C1 C2 C3 C4 0.5(5) . 11_566
C1 C2 C3 C4 179.8(3) . .
C1 C2 C3 C4 -0.5(5) 46_656 .
C1 C2 C1 N1 -0.1(4) 46_656 .
N2 C2 C3 C4 -179.8(3) 46_656 11_566
N2 C2 C3 C4 0.5(5) . 11_566
N2 C2 C3 C4 -0.5(5) 46_656 .
N2 C2 C3 C4 179.8(3) . .
N2 C2 N2 N1 -0.1(4) 46_656 .
N2 C2 N2 Co2 -147.2(3) 46_656 .
