Covalent Post-assembly Modification Triggers Multiple Structural Transformations of a Tetrazine-Edged Fe<sub>4</sub>L<sub>6</sub> Tetrahedron.
Roberts, Derrick A.; Pilgrim, Ben S.; Sirvinskaite, Giedre; Ronson, Tanya K.; Nitschke, Jonathan R.; Journal of the American Chemical Society 140 (2018) 9616–9623; doi:10.1021/jacs.8b05082

data_4132606
_publ_section_title
;
 Covalent Post-assembly Modification Triggers Multiple Structural
 Transformations of a Tetrazine-Edged Fe<sub>4</sub>L<sub>6</sub>
 Tetrahedron.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9616
_journal_page_last               9623
_journal_paper_doi               10.1021/jacs.8b05082
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety
'C408 H336 F24 Fe8 N72, 3(C16 H36 N), 19(F6 P), 27(C6 H6), 11(C2 H3 N)'
_chemical_formula_sum            'C640 H639 F138 Fe8 N86 P19'
_chemical_formula_weight         13192.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 96.856(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   49.486(10)
_cell_length_b                   28.207(6)
_cell_length_c                   48.662(9)
_cell_measurement_reflns_used    9011
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.431
_cell_measurement_theta_min      4.426
_cell_volume                     67439(2)
_computing_cell_refinement
;
'Bruker SAINT' 
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
'Bruker SAINT' 
;
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0956
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            257100
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        21.350
_diffrn_reflns_theta_max         21.351
_diffrn_reflns_theta_min         0.803
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             27264
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.463
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3858
_refine_ls_number_reflns         41237
_refine_ls_number_restraints     8532
_refine_ls_restrained_S_all      1.276
_refine_ls_R_factor_all          0.1679
_refine_ls_R_factor_gt           0.1279
_refine_ls_shift/su_max          0.002
_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^+350.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3491
_refine_ls_wR_factor_ref         0.3932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28648
_reflns_number_total             41237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05082_si_003.cif
_cod_data_source_block           bsp325_sq
_cod_original_cell_volume        67437(23)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4132606
_shelx_estimated_absorpt_t_min   0.991
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2014/6
_shelx_res_checksum              86270
_shelx_hkl_checksum              68908
_shelx_fab_checksum              86074