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_4338199
_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_absolute_configuration ad
_chemical_formula_moiety         'C36 H48 Fe N7'
_chemical_formula_sum            'C42 H54 Fe N7'
_chemical_formula_weight         712.77
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           159
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   13.4323(5)
_cell_length_b                   13.4323(5)
_cell_length_c                   11.6144(4)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.48
_cell_volume                     1814.80(11)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2013/3, SADABS V2012/1, TWINABS V2012/1 
(Bruker, 2012 & 2013) 
;
_computing_molecular_graphics
; 
SHELXTL v2013-4 (Bruker, 2013), CrystalMaker v2.7.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2013-1 (Bruker, 2013)'
_computing_structure_refinement  'SHELX-2013-4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELX-2013-4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd67fsaq
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            28387
_diffrn_reflns_theta_full        27.14
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.97380
_exptl_absorpt_correction_T_min  0.95025
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS v2012/1 (Bruker, 2012)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             762
_exptl_crystal_id                cd67fsaq
_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 0 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.104
_platon_squeeze_details
; 
Each unit has a benzene molecule that is highly disordered over
a three fold symmetry. 
We squeezed the benzene molecule out because it was poorly modeled.  
The 49 elec consistant with one benzene molecule per unit cell 
as predicted by the original 
;
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack (1983),  1269 Friedels'
_refine_ls_abs_structure_Flack   0.005(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2620
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.3508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                2552
_reflns_number_total             2620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500102c_si_003.cif
_cod_data_source_block           cd67fsaq_compound2
_cod_depositor_comments
'Adding full bibliography for 4338199--4338202.cif.'
_cod_database_code               4338199