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_4122155
_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         'C96 H78 Fe2 N18 O3, 4(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C104 H84 F12 Fe2 N20 O15 S4'
_chemical_formula_weight         2321.85
_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                 96.757(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0651(4)
_cell_length_b                   20.7223(6)
_cell_length_c                   45.3163(14)
_cell_measurement_reflns_used    7063
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.116
_cell_measurement_theta_min      4.445
_cell_volume                     11251.1(6)
_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 0.956
_diffrn_measured_fraction_theta_max 0.955
_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  0.0737
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            123184
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        23.000
_diffrn_reflns_theta_max         23.043
_diffrn_reflns_theta_min         1.984
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.2388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       plate
_exptl_crystal_F_000             4768
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1386
_refine_ls_number_reflns         16526
_refine_ls_number_restraints     1495
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.1684
_refine_ls_R_factor_gt           0.1070
_refine_ls_shift/su_max          0.020
_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^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2999
_refine_ls_wR_factor_ref         0.3242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7369
_reflns_number_total             16526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5042397_si_001.cif
_cod_data_source_block           dr2104
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               4122155
_shelx_estimated_absorpt_t_min   0.992
_shelx_estimated_absorpt_t_max   0.996
_shelxl_version_number           2013-2
_shelx_res_checksum              9029
_shelx_hkl_checksum              48228