#------------------------------------------------------------------------------
#$Date: 2019-11-25 10:27:58 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240675 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/01/4130101.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_4130101
loop_
_publ_author_name
'Reed, Douglas A.'
'Xiao, Dianne J.'
'Gonzalez, Miguel I.'
'Darago, Lucy E.'
'Herm, Zoey R.'
'Grandjean, Fernande'
'Long, Jeffrey R.'
_publ_section_title
;
 Reversible CO Scavenging via Adsorbate-Dependent Spin State Transitions
 in an Iron(II)-Triazolate Metal-Organic Framework.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5594
_journal_page_last               5602
_journal_paper_doi               10.1021/jacs.6b00248
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         '(C216 H96 Cl6 Fe24 N144 O24) Fe3'
_chemical_formula_sum            'C216 H96 Cl6 Fe27 N144 O24'
_chemical_formula_weight         6812.64
_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             2015-10-07
_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                   37.2012(9)
_cell_length_b                   37.2012(9)
_cell_length_c                   37.2012(9)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.75
_cell_measurement_theta_min      2.67
_cell_volume                     51484(2)
_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
_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       'ω/θ scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            155474
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.753
_diffrn_reflns_theta_max         26.753
_diffrn_reflns_theta_min         2.388
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  0.9582
_exptl_absorpt_correction_T_min  0.8579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1350 before and 0.0680 after correction.
The Ratio of minimum to maximum transmission is 0.8953.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.857
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             13272
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.208
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0405
_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)+(0.0883P)²+114.3153P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1292
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1646
_reflns_number_total             1873
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b00248_si_001.cif
_cod_data_source_block           dar002s
_cod_original_cell_volume        51484(4)
_cod_original_sg_symbol_Hall     '-F 4c 2 3'
_cod_database_code               4130101
_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   0.934
_shelx_estimated_absorpt_t_min   0.934
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.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
Fe1 Fe 0.68398(2) 0.74486(2) 0.5000 0.0226(2) Uani 1 2 d S T P
Cl1 Cl 0.7500 0.7500 0.5000 0.0218(4) Uani 1 8 d S T P
O1 O 0.60770(9) 0.73774(9) 0.5000 0.0522(8) Uani 1 2 d S T P
N1 N 0.71707(5) 0.68337(5) 0.46256(5) 0.0197(5) Uani 1 1 d . . .
N2 N 0.68990(5) 0.70733(5) 0.46283(5) 0.0191(4) Uani 1 1 d . . .
N3 N 0.66791(5) 0.70182(5) 0.43544(5) 0.0221(5) Uani 1 1 d . . .
C1 C 0.71187(6) 0.66225(6) 0.43398(6) 0.0223(5) Uani 1 1 d . . .
H1 H 0.7268 0.6429 0.4267 0.027 Uiso 1 1 calc R . .
C2 C 0.68120(6) 0.67339(6) 0.41702(6) 0.0210(5) Uani 1 1 d . . .
C3 C 0.66345(6) 0.65967(6) 0.38420(6) 0.0219(5) Uani 1 1 d . . .
C4 C 0.63290(6) 0.67675(6) 0.37066(6) 0.0216(5) Uani 1 1 d . . .
H4 H 0.6238 0.6976 0.3823 0.026 Uiso 1 1 calc R . .
C5 C 0.63651(13) 0.74033(10) 0.5000 0.0356(9) Uani 1 2 d S T P
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 0.1690 0.1900 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3680 0.9950 '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
N1 Fe1 Cl1 87.48(6) 160_576 .
N1 Fe1 Cl1 87.48(6) 63_464 .
N1 Fe1 N1 89.04(10) 160_576 63_464
N2 Fe1 Cl1 86.78(6) 98_556 .
N2 Fe1 Cl1 86.78(6) . .
N2 Fe1 N1 90.83(7) 98_556 160_576
N2 Fe1 N1 174.27(8) . 160_576
N2 Fe1 N1 90.83(7) . 63_464
N2 Fe1 N1 174.26(8) 98_556 63_464
N2 Fe1 N2 88.73(11) . 98_556
C5 Fe1 Cl1 178.99(12) . .
C5 Fe1 N1 93.24(10) . 63_464
C5 Fe1 N1 93.24(10) . 160_576
C5 Fe1 N2 92.50(10) . .
C5 Fe1 N2 92.50(10) . 98_556
Fe1 Cl1 Fe1 180.0 135_756 63_464
Fe1 Cl1 Fe1 90.0 135_756 .
Fe1 Cl1 Fe1 180.0 169_666 .
Fe1 Cl1 Fe1 90.0 169_666 135_756
Fe1 Cl1 Fe1 90.000(1) 169_666 63_464
Fe1 Cl1 Fe1 89.998(1) 63_464 .
N2 N1 Fe1 121.46(14) . 135_756
C1 N1 Fe1 131.92(16) . 135_756
C1 N1 N2 106.62(18) . .
N1 N2 Fe1 123.75(14) . .
N3 N2 Fe1 125.41(15) . .
N3 N2 N1 110.84(17) . .
N2 N3 C2 106.57(17) . .
N1 C1 H1 126.0 . .
N1 C1 C2 108.0(2) . .
C2 C1 H1 126.0 . .
N3 C2 C1 107.93(19) . .
N3 C2 C3 121.63(19) . .
C1 C2 C3 130.4(2) . .
C4 C3 C2 120.3(2) . .
C4 C3 C2 120.0(2) 11_566 .
C4 C3 C4 119.7(2) 11_566 .
C3 C4 C3 120.3(2) 8_656 .
C3 C4 H4 119.8 . .
C3 C4 H4 119.8 8_656 .
O1 C5 Fe1 179.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 Cl1 2.4633(5) .
Fe1 N1 1.9861(19) 160_576
Fe1 N1 1.9861(19) 63_464
Fe1 N2 1.9774(19) .
Fe1 N2 1.9775(19) 98_556
Fe1 C5 1.774(5) .
Cl1 Fe1 2.4632(5) 135_756
Cl1 Fe1 2.4632(5) 63_464
Cl1 Fe1 2.4632(5) 169_666
O1 C5 1.076(5) .
N1 Fe1 1.9862(19) 135_756
N1 N2 1.348(3) .
N1 C1 1.336(3) .
N2 N3 1.323(3) .
N3 C2 1.354(3) .
C1 H1 0.9500 .
C1 C2 1.368(3) .
C2 C3 1.479(3) .
C3 C4 1.386(3) 11_566
C3 C4 1.396(3) .
C4 C3 1.386(3) 8_656
C4 H4 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
Fe1 N1 N2 Fe1 -1.0(2) 135_756 .
Fe1 N1 N2 N3 179.93(14) 135_756 .
Fe1 N1 C1 C2 179.78(16) 135_756 .
Fe1 N2 N3 C2 -178.83(15) . .
N1 N2 N3 C2 0.3(2) . .
N1 C1 C2 N3 0.6(3) . .
N1 C1 C2 C3 179.5(2) . .
N2 N1 C1 C2 -0.4(3) . .
N2 N3 C2 C1 -0.5(3) . .
N2 N3 C2 C3 -179.5(2) . .
N3 C2 C3 C4 -176.6(2) . 11_566
N3 C2 C3 C4 2.2(3) . .
C1 N1 N2 Fe1 179.20(15) . .
C1 N1 N2 N3 0.1(2) . .
C1 C2 C3 C4 -176.6(3) . .
C1 C2 C3 C4 4.6(4) . 11_566
C2 C3 C4 C3 -178.62(16) . 8_656
C4 C3 C4 C3 0.2(5) 11_566 8_656
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 -0.265 -0.107 -0.996 25059.7 826.1
2 0.250 0.250 0.250 930.2 123.1
3 0.250 0.250 0.750 930.2 129.8
4 0.250 0.750 0.250 930.2 129.8
5 0.250 0.750 0.750 930.2 123.1
6 0.750 0.250 0.250 930.2 129.8
7 0.750 0.250 0.750 930.2 123.1
8 0.750 0.750 0.250 930.2 123.1
9 0.750 0.750 0.750 930.2 129.8
