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_4132607
_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
'C432 H408 Fe8 N72 O24, 2(C16 H36 N), 18(F6 P1), 4(C6 H6), (C2 H3 N)'
_chemical_formula_sum            'C490 H507 F108 Fe8 N75 O24 P18'
_chemical_formula_weight         10886.94
_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-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 95.956(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.2842(7)
_cell_length_b                   36.3797(6)
_cell_length_c                   49.0016(9)
_cell_measurement_reflns_used    67064
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.2460
_cell_measurement_theta_min      1.5350
_cell_volume                     64333(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'GDA 8.44; generic data acquisition software'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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_detector_area_resol_mean 0
_diffrn_detector_type            'Dectris Pilatus 2M'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       '\f rotation with 0.2 degree frames'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Diamond Light Source Beamline I19'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0957
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            310835
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        19.245
_diffrn_reflns_theta_max         19.245
_diffrn_reflns_theta_min         1.541
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_T_max  0.7444
_exptl_absorpt_correction_T_min  0.4572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_description       prism
_exptl_crystal_F_000             22456
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3216
_refine_ls_number_reflns         29307
_refine_ls_number_restraints     7288
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.1796
_refine_ls_R_factor_gt           0.1607
_refine_ls_shift/su_max          0.000
_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^+600.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4251
_refine_ls_wR_factor_ref         0.4404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22751
_reflns_number_total             29307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05082_si_004.cif
_cod_data_source_block           dr7142_sq
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4132607
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.994
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              36904
_shelx_hkl_checksum              56957
_shelx_fab_checksum              49845