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_4122156
_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
'C102 H90 Fe2 N18 O3, 4(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C110 H96 F12 Fe2 N20 O15 S4'
_chemical_formula_weight         2406.00
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 92.370(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   47.203(3)
_cell_length_b                   12.9869(9)
_cell_length_c                   39.414(3)
_cell_measurement_reflns_used    9257
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      46.655
_cell_measurement_theta_min      4.475
_cell_volume                     24141(3)
_computing_cell_refinement
;
Rigaku CrystalClear-SM Expert 3.1 b27
;
_computing_data_collection
;
Rigaku CrystalClear-SM Expert 3.1 b27
;
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0796
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            47106
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        19.800
_diffrn_reflns_theta_max         19.782
_diffrn_reflns_theta_min         2.940
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.395
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.4791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       Blade
_exptl_crystal_F_000             9920
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1402
_refine_ls_number_reflns         10712
_refine_ls_number_restraints     1336
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.0981
_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^)+(0.1735P)^2^+114.2665P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2715
_refine_ls_wR_factor_ref         0.2880
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7339
_reflns_number_total             10712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5042397_si_001.cif
_cod_data_source_block           dr2118_sq_d
_cod_database_code               4122156
_shelx_estimated_absorpt_t_min   0.918
_shelx_estimated_absorpt_t_max   0.996
_shelxl_version_number           2013-2
_shelx_res_checksum              47211
_shelx_hkl_checksum              64747