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_4124265
_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
'C180 H144 Fe4 N36, 6(C2 F6 N O4 S2), 2(B F4), 9.5(C2 H3 N)'
_chemical_formula_sum            'C211 H172.5 B2 F44 Fe4 N51.5 O24 S12'
_chemical_formula_weight         5279.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90.871(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.1666(11)
_cell_length_b                   25.5055(9)
_cell_length_c                   37.0688(15)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      79.031
_cell_measurement_theta_min      5.457
_cell_volume                     23791.2(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0857
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            63012
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        40.057
_diffrn_reflns_theta_max         39.967
_diffrn_reflns_theta_min         2.384
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.849
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.6039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       needle
_exptl_crystal_F_000             10772
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3096
_refine_ls_number_reflns         14345
_refine_ls_number_restraints     7005
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1357
_refine_ls_R_factor_gt           0.0896
_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^)+(0.1468P)^2^+149.7923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2245
_refine_ls_wR_factor_ref         0.2510
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9391
_reflns_number_total             14345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b05080_si_002.cif
_cod_data_source_block           jn1438_sq_d
_cod_depositor_comments
'Adding full bibliography for 4124264--4124265.cif.'
_cod_original_formula_sum        'C211 H172.50 B2 F44 Fe4 N51.50 O24 S12'
_cod_database_code               4124265
_shelx_estimated_absorpt_t_min   0.424
_shelx_estimated_absorpt_t_max   0.941
_shelxl_version_number           2014/6
_shelx_res_checksum              14924
_shelx_hkl_checksum              98475