Post-assembly Modification of Tetrazine-Edged Fe(II)4L6 Tetrahedra.
Roberts, Derrick A.; Pilgrim, Ben S.; Cooper, Jonathan D.; Ronson, Tanya K.; Zarra, Salvatore; Nitschke, Jonathan R.; Journal of the American Chemical Society 137 (2015) 10068–10071; doi:10.1021/jacs.5b05080

data_4124264
_publ_section_title
;
 Post-assembly Modification of Tetrazine-Edged Fe(II)4L6 Tetrahedra.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10068
_journal_page_last               10071
_journal_paper_doi               10.1021/jacs.5b05080
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety
'C156 H96 F12 Fe4 N48, 0.25(C2 F6 N O4 S2), 7.75(B F4), 5(C2 H3 N)'
_chemical_formula_sum            'C166.5 H111 B7.75 F44.5 Fe4 N53.25 O S0.5'
_chemical_formula_weight         4042.29
_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   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                93.763(3)
_cell_angle_beta                 98.158(4)
_cell_angle_gamma                100.570(3)
_cell_formula_units_Z            2
_cell_length_a                   20.3453(14)
_cell_length_b                   20.5485(14)
_cell_length_c                   24.4033(17)
_cell_measurement_reflns_used    9796
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.351
_cell_measurement_theta_min      4.785
_cell_volume                     9883.4(12)
_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  0.0834
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            123164
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        21.260
_diffrn_reflns_theta_max         21.258
_diffrn_reflns_theta_min         0.981
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.4789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       block
_exptl_crystal_F_000             4084
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2542
_refine_ls_number_reflns         23905
_refine_ls_number_restraints     6212
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.1409
_refine_ls_R_factor_gt           0.1117
_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^+35.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3063
_refine_ls_wR_factor_ref         0.3314
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16330
_reflns_number_total             23905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b05080_si_001.cif
_cod_data_source_block           jdc224_sq_d
_cod_depositor_comments
'Adding full bibliography for 4124264--4124265.cif.'
_cod_original_formula_sum
'C166.50 H111 B7.75 F44.50 Fe4 N53.25 O S0.50'
_cod_database_code               4124264
_shelx_estimated_absorpt_t_min   0.996
_shelx_estimated_absorpt_t_max   0.996
_shelxl_version_number           2014/6
_shelx_res_checksum              62471
_shelx_hkl_checksum              10965