Post-assembly Modification of Kinetically Metastable Fe(II)2L3 Triple Helicates.
Roberts, Derrick A.; Castilla, Ana M.; Ronson, Tanya K.; Nitschke, Jonathan R.; Journal of the American Chemical Society 136 (2014) 8201–8204; doi:10.1021/ja5042397

data_4122154
_publ_section_title
;
 Post-assembly Modification of Kinetically Metastable Fe(II)2L3 Triple
 Helicates.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8201
_journal_page_last               8204
_journal_paper_doi               10.1021/ja5042397
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C90 H66 Fe2 N24, 4(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C98 H72 F12 Fe2 N26 O12 S4'
_chemical_formula_weight         2273.75
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.401(2)
_cell_length_b                   34.672(2)
_cell_length_c                   21.1517(14)
_cell_measurement_reflns_used    9767
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      42.223
_cell_measurement_theta_min      4.467
_cell_volume                     22295(2)
_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 0.997
_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  0.0950
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            147206
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.150
_diffrn_reflns_theta_max         20.148
_diffrn_reflns_theta_min         0.863
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             9296
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1258
_refine_ls_number_reflns         11652
_refine_ls_number_restraints     1449
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.1185
_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^+60.0000P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3238
_refine_ls_wR_factor_ref         0.3397
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9090
_reflns_number_total             11652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5042397_si_001.cif
_cod_data_source_block           dr174_sq_d
_cod_original_cell_volume        22295(3)
_cod_database_code               4122154
_shelx_estimated_absorpt_t_min   0.992
_shelx_estimated_absorpt_t_max   0.998
_shelxl_version_number           2013-2
_shelx_res_checksum              95104
_shelx_hkl_checksum              92451