Isolation of Iron(II) Aqua and Hydroxyl Complexes Featuring a Tripodal H-bond Donor and Acceptor Ligand.
Matson, Ellen M.; Bertke, Jeffrey A.; Fout, Alison R.; Inorganic chemistry 53 (2014) 4450–4458; doi:10.1021/ic500102c

data_4338201
_publ_contact_author
; 
Alison R. Fout 
University of Illinois 
Department of Chemistry 
600 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Isolation of Iron(II) Aqua and Hydroxyl Complexes Featuring a Tripodal
 H-bond Donor and Acceptor Ligand.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4450
_journal_page_last               4458
_journal_paper_doi               10.1021/ic500102c
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
; 
C37 H51 F3 Fe N7 O3 S, C F3 O3 S, C4 H8 O 
;
_chemical_formula_sum            'C42 H59 F6 Fe N7 O7 S2'
_chemical_formula_weight         1007.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6938(11)
_cell_length_b                   16.2327(16)
_cell_length_c                   27.590(3)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    176(2)
_cell_measurement_theta_max      25.31
_cell_measurement_theta_min      2.40
_cell_volume                     4789.3(9)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
; 
SAINT V7.68A, XPREP V2005/2, SADABS V2008/2, TWINABS V2008/2 
(Bruker, 2005 & 2008) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      176(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cm77bas
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            59253
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.107
_diffrn_reflns_theta_min         1.455
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.9459
_exptl_absorpt_correction_T_min  0.8808
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2112
_exptl_crystal_id                cm77bas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (0 1 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.381
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
; 
 Flack x determined using 3815 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.011(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         10529
_refine_ls_number_restraints     570
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.8235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                9364
_reflns_number_total             10529
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500102c_si_003.cif
_cod_data_source_block           cm77bas_Compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 

 Adding full bibliography for 4338199--4338202.cif.
;
_cod_original_cell_volume        4789.3(8)
_cod_original_sg_symbol_H-M      'P2(1)2(1)2(1) '
_cod_database_code               4338201
_shelx_estimated_absorpt_t_min   0.827
_shelx_estimated_absorpt_t_max   0.935
_shelxl_version_number           2013-4
_shelx_res_checksum              21525
_shelx_hkl_checksum              72773