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_4122157
_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
'C108 H81 Fe2 N21 O3, 3(F6 P), C F3 O3 S, 3(C2 H3 N)'
_chemical_formula_sum            'C115 H90 F21 Fe2 N24 O6 P3 S'
_chemical_formula_weight         2539.77
_chemical_name_systematic
;
 ?
;
_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-2013
_cell_angle_alpha                90
_cell_angle_beta                 96.0940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7077(3)
_cell_length_b                   21.2365(5)
_cell_length_c                   43.5084(10)
_cell_measurement_reflns_used    9399
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      58.72
_cell_measurement_theta_min      2.92
_cell_volume                     11675.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.975
_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  0.0480
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            53028
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        54.250
_diffrn_reflns_theta_max         54.236
_diffrn_reflns_theta_min         4.588
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.407
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       Block
_exptl_crystal_F_000             5192
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.345
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1604
_refine_ls_number_reflns         13896
_refine_ls_number_restraints     1758
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1403
_refine_ls_R_factor_gt           0.1054
_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^+35.0000P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2833
_refine_ls_wR_factor_ref         0.3081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9395
_reflns_number_total             13896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5042397_si_001.cif
_cod_data_source_block           jn1309_sq_d
_cod_database_code               4122157
_shelx_estimated_absorpt_t_min   0.428
_shelx_estimated_absorpt_t_max   0.796
_shelxl_version_number           2013-2
_shelx_res_checksum              93309
_shelx_hkl_checksum              14253