Iron(ii) complexes of new hexadentate 1,1,1-tris-(iminomethyl)ethane podands, and their 7-methyl-1,3,5-triazaadamantane rearrangement products.
Diener, Sara A.; Santoro, Amedeo; Kilner, Colin A.; Loughrey, Jonathan J.; Halcrow, Malcolm A.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 3731–3739; doi:10.1039/c2dt11911k

data_7018386
_publ_section_title
;
 Iron(ii) complexes of new hexadentate 1,1,1-tris-(iminomethyl)ethane
 podands, and their 7-methyl-1,3,5-triazaadamantane rearrangement
 products.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3731
_journal_page_last               3739
_journal_paper_doi               10.1039/c2dt11911k
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C17 H21 Fe N9, 2[Cl O4], 0.7[H2 O]'
_chemical_formula_sum            'C17 H22.4 Cl2 Fe N9 O8.7'
_chemical_formula_weight         618.79
_chemical_name_systematic
;
[1,1,1-Tris(1H-imidazol-2-ylmethyleneaminomethyl)ethane]iron(II)
diperchlorate hydrate (1/0.7)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.037(5)
_cell_angle_beta                 87.449(7)
_cell_angle_gamma                75.601(4)
_cell_formula_units_Z            4
_cell_length_a                   10.1387(13)
_cell_length_b                   12.1897(13)
_cell_length_c                   21.549(3)
_cell_measurement_reflns_used    91511
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.27
_cell_measurement_theta_min      0.97
_cell_volume                     2503.0(5)
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            91511
_diffrn_reflns_theta_full        30.27
_diffrn_reflns_theta_max         30.27
_diffrn_reflns_theta_min         0.97
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of
G/ottingen, Germany.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         14631
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0389P)^2^+1.7567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                12096
_reflns_number_total             14632
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt11911k.txt
_cod_data_source_block           sd19
_cod_original_formula_sum        'C17 H22.40 Cl2 Fe N9 O8.70'
_cod_database_code               7018386