#------------------------------------------------------------------------------
#$Date: 2019-11-25 12:38:52 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240879 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/04/4130450.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_4130450
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         'C109.02 H71.02 Cl3 Co13.44 N63.98 O5.04'
_chemical_formula_sum            'C109.02 H71.02 Cl3 Co13.44 N63.98 O5.04'
_chemical_formula_weight         3256.24
_chemical_name_common            Co-BDTriP
_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
_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                   18.6522(5)
_cell_length_b                   18.6522(5)
_cell_length_c                   18.6522(5)
_cell_measurement_reflns_used    9714
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.667
_cell_measurement_theta_min      2.442
_cell_volume                     6489.2(3)
_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 7.9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7753
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.544
_diffrn_source                   'microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0697 before and 0.0427 after correction.
The Ratio of minimum to maximum transmission is 0.8931.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    0.814
_exptl_crystal_description       cube
_exptl_crystal_F_000             1582
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         1208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0463
_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)+(0.0447P)²+13.2442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.000
_reflns_number_gt                926
_reflns_number_total             1208
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b03680_si_001.cif
_cod_data_source_block           Co-BDTriP-Activated
_cod_original_cell_volume        6489.2(5)
_cod_database_code               4130450
_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   0.915
_shelx_estimated_absorpt_t_min   0.915
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{C1, N2}
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(N2)
4. Others
 Fixed Sof: O1(0.105) Co2(0.03) N2(0.333) C1(0.667) H1(0.667)
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'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-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 0.5000 0.0000 0.37226(4) 0.0243(3) Uani 1 4 d S T P . .
Cl1 Cl 0.5000 0.0000 0.5000 0.0276(6) Uani 1 16 d S T P . .
O1 O 0.5000 0.0000 0.2460(10) 0.108(6) Uani 0.42 4 d S T P . .
N1 N 0.42456(12) 0.07238(11) 0.37319(12) 0.0236(5) Uani 1 1 d . . . . .
C2 C 0.35194(16) 0.1632(2) 0.35194(16) 0.0299(10) Uani 1 2 d S T P . .
C3 C 0.31974(15) 0.2279(2) 0.31974(15) 0.0277(9) Uani 1 2 d S T P . .
C4 C 0.25857(16) 0.25857(16) 0.3493(2) 0.0290(10) Uani 1 2 d S T P . .
H4 H 0.2373 0.2373 0.3904 0.035 Uiso 1 2 calc RS T P A .
Co2 Co 0.5000 0.1461(9) 0.2707(7) 0.062(4) Uani 0.06 2 d S T P A 2
N2 N 0.41188(14) 0.12768(14) 0.32927(15) 0.0292(6) Uani 0.333 1 d . . . A 2
C1 C 0.41188(14) 0.12768(14) 0.32927(15) 0.0292(6) Uani 0.667 1 d . . . A 3
H1 H 0.4401 0.1403 0.2888 0.035 Uiso 0.667 1 calc R . . A 3
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'
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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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 89.49(7) 33 .
N1 Co1 Cl1 89.49(7) 30_655 .
N1 Co1 Cl1 89.49(7) . .
N1 Co1 Cl1 89.49(7) 3_655 .
N1 Co1 O1 90.51(7) 33 .
N1 Co1 O1 90.51(7) . .
N1 Co1 O1 90.51(7) 30_655 .
N1 Co1 O1 90.51(7) 3_655 .
N1 Co1 N1 87.63(13) 33 .
N1 Co1 N1 87.63(13) 30_655 3_655
N1 Co1 N1 92.36(13) 33 3_655
N1 Co1 N1 92.36(13) 30_655 .
N1 Co1 N1 178.98(14) 33 30_655
N1 Co1 N1 178.98(14) 3_655 .
Co1 Cl1 Co1 180.0 32_655 8_556
Co1 Cl1 Co1 90.0 32_655 .
Co1 Cl1 Co1 90.0 8_556 25_656
Co1 Cl1 Co1 180.0 25_656 .
Co1 Cl1 Co1 90.0 8_556 .
Co1 Cl1 Co1 90.0 32_655 25_656
N1 N1 Co1 121.10(7) 48 .
N2 N1 Co1 130.97(19) . .
N2 N1 N1 107.93(15) . 48
C1 N1 Co1 130.97(19) . .
C1 N1 N1 107.93(15) . 48
N2 C2 C3 127.13(17) 48 .
N2 C2 C3 127.13(17) . .
N2 C2 N2 105.7(3) . 48
C1 C2 C3 127.13(17) 48 .
C1 C2 C3 127.13(17) . .
C1 C2 C1 105.7(3) . 48
C4 C3 C2 120.6(2) . .
C4 C3 C2 120.6(2) 11 .
C4 C3 C4 118.8(4) . 11
C3 C4 C3 121.2(4) 12 .
C3 C4 H4 119.4 12 .
C3 C4 H4 119.4 . .
N2 Co2 N2 110.3(6) 30_655 .
N1 N2 C2 109.2(2) . .
N1 N2 Co2 108.7(4) . .
C2 N2 Co2 139.2(5) . .
N1 C1 C2 109.2(2) . .
N1 C1 H1 125.4 . .
C2 C1 H1 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 2.3826(8) .
Co1 O1 2.354(19) .
Co1 N1 1.950(2) .
Co1 N1 1.950(2) 30_655
Co1 N1 1.950(2) 3_655
Co1 N1 1.950(2) 33
Cl1 Co1 2.3826(8) 32_655
Cl1 Co1 2.3826(8) 25_656
Cl1 Co1 2.3826(8) 8_556
N1 N1 1.355(4) 48
N1 N2 1.338(3) .
N1 C1 1.338(3) .
C2 C3 1.475(6) .
C2 N2 1.367(4) .
C2 N2 1.367(4) 48
C2 C1 1.367(4) .
C2 C1 1.367(4) 48
C3 C4 1.390(3) 11
C3 C4 1.390(3) .
C4 C3 1.390(3) 12
C4 H4 0.9500 .
Co2 N2 2.003(8) 30_655
Co2 N2 2.003(8) .
C1 H1 0.9500 .
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 N2 C2 179.7(2) . .
Co1 N1 N2 Co2 -15.6(6) . .
Co1 N1 C1 C2 179.7(2) . .
N1 N1 N2 C2 -0.4(3) 48 .
N1 N1 N2 Co2 164.2(5) 48 .
N1 N1 C1 C2 -0.4(3) 48 .
C2 C3 C4 C3 179.6(3) . 12
C3 C2 N2 N1 178.9(4) . .
C3 C2 N2 Co2 21.5(9) . .
C3 C2 C1 N1 178.9(4) . .
C4 C3 C4 C3 -1.5(9) 11 12
N2 C2 C3 C4 179.5(4) 48 11
N2 C2 C3 C4 1.7(7) . 11
N2 C2 C3 C4 -179.5(4) . .
N2 C2 C3 C4 -1.7(7) 48 .
N2 C2 N2 N1 0.7(5) 48 .
N2 C2 N2 Co2 -156.7(6) 48 .
C1 C2 C3 C4 -1.7(7) 48 .
C1 C2 C3 C4 1.7(7) . 11
C1 C2 C3 C4 179.5(4) 48 11
C1 C2 C3 C4 -179.5(4) . .
C1 C2 C1 N1 0.7(5) 48 .
