Oxidation triggers guest dissociation during reorganization of an FeII4L6 twisted parallelogram
Plajer, Alex J.; Rizzuto, Felix; von Krbek, Larissa K. S.; Gisbert, Yohan; Martínez-Agramunt, Víctor; Nitschke, Jonathan; Chemical Science  (2020) –; doi:10.1039/D0SC04352D

data_1559031
_publ_section_title
;
 Oxidation triggers guest dissociation during reorganization of an FeII4L6
 twisted parallelogram
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC04352D
_journal_year                    2020
_chemical_formula_moiety
'C192 H144 Fe10 N36, 8(C2 F6 N O4 S2), 5(C2 H3 N)'
_chemical_formula_sum            'C218 H159 F48 Fe10 N49 O32 S16'
_chemical_formula_weight         5960.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-05-30 deposited with the CCDC.	2020-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.81(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.651(5)
_cell_length_b                   27.050(5)
_cell_length_c                   36.959(7)
_cell_measurement_reflns_used    16196
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.1087
_cell_measurement_theta_min      1.1461
_cell_volume                     26330(9)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.8.1-g1afca60c-release-hotfix1'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.8.1-g1afca60c-release-hotfix1
pointless (Evans, P., 2006)
XIA2 0.5.474-gb1e580cd-dials-1.8 (Winter, G., 2010)
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Diamond Light Source Beamline I19-1'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1258
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            98034
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        18.248
_diffrn_reflns_theta_max         18.248
_diffrn_reflns_theta_min         1.046
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9524
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.046: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       block
_exptl_crystal_F_000             12056
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3364
_refine_ls_number_reflns         20709
_refine_ls_number_restraints     7475
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1792
_refine_ls_R_factor_gt           0.1492
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+400.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3261
_refine_ls_wR_factor_ref         0.3409
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12914
_reflns_number_total             20709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04352d2.cif
_cod_data_source_block           P21C_A_SQ
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1559031
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.894
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              28818
_shelx_fab_checksum              4703