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_4338202
_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_sum            'C40 H59 Fe N7 O2'
_chemical_formula_weight         725.79
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.254(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.764(3)
_cell_length_b                   9.222(3)
_cell_length_c                   42.281(12)
_cell_measurement_temperature    172(2)
_cell_volume                     3807(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker, 2005)'
_computing_molecular_graphics    'SHELX-2013-4 (Sheldrick, 2013)'
_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      172(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            34190
_diffrn_reflns_theta_full        27.22
_diffrn_reflns_theta_max         27.22
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  0.9698
_exptl_absorpt_correction_T_min  0.7977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0310P)^2^+1.6631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0859
_reflns_number_gt                6758
_reflns_number_total             8441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500102c_si_003.cif
_cod_data_source_block           cm07das_compound5
_cod_depositor_comments
'Adding full bibliography for 4338199--4338202.cif.'
_cod_original_cell_volume        3807.1(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4338202