Reversible CO Scavenging via Adsorbate-Dependent Spin State Transitions in an Iron(II)-Triazolate Metal-Organic Framework.
Reed, Douglas A.; Xiao, Dianne J.; Gonzalez, Miguel I.; Darago, Lucy E.; Herm, Zoey R.; Grandjean, Fernande; Long, Jeffrey R.; Journal of the American Chemical Society 138 (2016) 5594–5602; doi:10.1021/jacs.6b00248

data_4130102
_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         '(C264 H240 Cl6 Fe24 N168 O24) Fe3'
_chemical_formula_sum            'C264 H240 Cl6 Fe27 N168 O24'
_chemical_formula_weight         7870.49
_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             2015-10-21
_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                   38.0680(11)
_cell_length_b                   38.0680(11)
_cell_length_c                   38.0680(11)
_cell_measurement_reflns_used    9591
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.252
_cell_measurement_theta_min      2.609
_cell_volume                     55167(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
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS diffractometer'
_diffrn_measurement_method       '\w/\q scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            264419
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         35.322
_diffrn_reflns_theta_min         2.021
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.9582
_exptl_absorpt_correction_T_min  0.8856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1064 before and 0.0648 after correction.
The Ratio of minimum to maximum transmission is 0.9242.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.948
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             14040
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.465
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         4188
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0505
_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/[\s^2^(Fo^2^)+(0.0983P)^2^+182.7640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3583
_reflns_number_total             4188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b00248_si_002.cif
_cod_data_source_block           djx014s
_cod_original_cell_volume        55167(5)
_cod_original_sg_symbol_Hall     '-F 4c 2 3'
_cod_database_code               4130102
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.950
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O003-C6 \\sim O003-C11
 with sigma of 0.02
 N14-C6 \\sim N4-C11
 with sigma of 0.02
3. Rigid bond restraints
 O003, C6, N4, C11, N14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O003 \\sim C6 \\sim N4 \\sim C11 \\sim N14: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
5. Others
 Fixed Sof: C6(0.4) H6(0.4) N4(0.1) C11(0.1) H11(0.1) N14(0.4)
6.a Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C4(H4), C6(H6), C11(H11)
;
_shelx_res_checksum              85865
_shelx_hkl_checksum              49456
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'