Synthesis and characterization of iron trisphenolate complexes with hydrogen-bonding cavities.
Adelhardt, Mario; Chalkley, Matthew J.; Heinemann, Frank W.; Sutter, Jörg; Scheurer, Andreas; Meyer, Karsten; Inorganic chemistry 53 (2014) 2763–2765; doi:10.1021/ic5002286

data_4337725
_publ_section_title
;
 Synthesis and characterization of iron trisphenolate complexes with
 hydrogen-bonding cavities.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2763
_journal_page_last               2765
_journal_paper_doi               10.1021/ic5002286
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C48 H69 N4 O6 Zn, C4 H12 N, 3.5(C5 H5 N)'
_chemical_formula_sum            'C69.5 H98.5 N8.5 O6 Zn'
_chemical_formula_weight         1214.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.772(3)
_cell_length_b                   23.772(3)
_cell_length_c                   23.772(3)
_cell_measurement_reflns_used    9718
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.38
_cell_measurement_theta_min      2.84
_cell_volume                     13434(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            71099
_diffrn_reflns_theta_full        27.09
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2008'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5224
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4936
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+10.4401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1202
_reflns_number_gt                3873
_reflns_number_total             4936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5002286_si_002.cif
_cod_data_source_block           ma1311
_cod_original_sg_symbol_Hall     -P_2ac_2ab_3
_cod_original_sg_symbol_H-M      Pa-3
_cod_original_formula_sum        'C69.50 H98.50 N8.50 O6 Zn'
_cod_database_code               4337725