Synthesis and Stabilization of a Monomeric Iron(II) Hydroxo Complex via Intramolecular Hydrogen Bonding in the Secondary Coordination Sphere
Alexander J. Kendall; Lev N. Zakharov; John D. Gilbertson; Inorganic Chemistry 49 (2010) 8656–8658; doi:10.1021/ic101408e

data_4316658
_publ_section_title
;
 Synthesis and Stabilization of a Monomeric Iron(II) Hydroxo Complex via
 Intramolecular Hydrogen Bonding in the Secondary Coordination Sphere
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8656
_journal_page_last               8658
_journal_paper_doi               10.1021/ic101408e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C31 H49 Br2 F6 Fe N4 O0.5 P'
_chemical_formula_weight         846.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXLTL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.742(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   46.903(6)
_cell_length_b                   10.1167(13)
_cell_length_c                   15.678(2)
_cell_measurement_reflns_used    3758
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.10
_cell_measurement_theta_min      2.40
_cell_volume                     7308.9(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26671
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         0.88
_exptl_absorpt_coefficient_mu    2.703
_exptl_absorpt_correction_T_max  0.9479
_exptl_absorpt_correction_T_min  0.5632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                5681
_reflns_number_total             7935
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101408e_si_002_1.cif
_cod_data_source_block           gilb14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        7308.8(16)
_cod_original_formula_sum        'C31 H49 Br2 F6 Fe N4 O0.50 P'
_cod_database_code               4316658