Pyrene-Edged Fe(II)4L6 Cages Adaptively Reconfigure During Guest Binding.
Ronson, Tanya K.; League, Aaron B.; Gagliardi, Laura; Cramer, Christopher J.; Nitschke, Jonathan R.; Journal of the American Chemical Society 136 (2014) 15615–15624; doi:10.1021/ja507617h

data_4122866
_publ_section_title
;
 Pyrene-Edged Fe(II)4L6 Cages Adaptively Reconfigure During Guest Binding.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15615
_journal_page_last               15624
_journal_paper_doi               10.1021/ja507617h
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety
'C240 H156 Fe4 N24, 8(F6 P), 2.5(C6 H6), 0.5(C2 H3 N)'
_chemical_formula_sum            'C256 H172.5 F48 Fe4 N24.5 P8'
_chemical_formula_weight         4974.83
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                82.922(3)
_cell_angle_beta                 66.366(4)
_cell_angle_gamma                72.449(3)
_cell_formula_units_Z            2
_cell_length_a                   24.4345(15)
_cell_length_b                   25.6731(16)
_cell_length_c                   28.6611(17)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.462
_cell_measurement_theta_min      4.466
_cell_volume                     15704.5(17)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Rigaku Saturn 724+ detector on Crystal Logic diffractometer'
_diffrn_measurement_method       '\w  scans'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_source         'Diamond beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0998
_diffrn_reflns_av_unetI/netI     0.1020
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            107323
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.000
_diffrn_reflns_theta_max         19.737
_diffrn_reflns_theta_min         2.041
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.6133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_description       block
_exptl_crystal_F_000             5072
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2834
_refine_ls_number_reflns         30894
_refine_ls_number_restraints     2272
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1417
_refine_ls_R_factor_gt           0.1016
_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^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2795
_refine_ls_wR_factor_ref         0.3111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18375
_reflns_number_total             30894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja507617h_si_002.cif
_cod_data_source_block           tkr68_sq_d
_cod_depositor_comments          'Adding full bibliography for 4122866.cif.'
_cod_original_formula_sum        'C256 H172.50 F48 Fe4 N24.50 P8'
_cod_database_code               4122866
_shelx_estimated_absorpt_t_min   0.997
_shelx_estimated_absorpt_t_max   0.997
_shelxl_version_number           2013-2
_shelx_res_checksum              9757
_shelx_hkl_checksum              83047