Iron(II) Complexes with Scorpiand-Like Macrocyclic Polyamines: Kinetico-Mechanistic Aspects of Complex Formation and Oxidative Dehydrogenation of Coordinated Amines.
Clares, M. Paz; Acosta-Rueda, Laura; Castillo, Carmen E.; Blasco, Salvador; Jiménez, Hermas R; García-España, Enrique; Basallote, Manuel G.; Inorganic chemistry 56 (2017) 4400–4412; doi:10.1021/acs.inorgchem.6b03070

data_4345783
_publ_section_title
;
 Iron(II) Complexes with Scorpiand-Like Macrocyclic Polyamines:
 Kinetico-Mechanistic Aspects of Complex Formation and Oxidative
 Dehydrogenation of Coordinated Amines.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4400
_journal_page_last               4412
_journal_paper_doi               10.1021/acs.inorgchem.6b03070
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C19 H26 Fe N6, 2(Cl O4)'
_chemical_formula_sum            'C19 H26 Cl2 Fe N6 O8'
_chemical_formula_weight         593.21
_chemical_name_common            '[Fe(pytren-2pyH-1)](ClO4)2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-06-26
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5602(3)
_cell_length_b                   8.8480(2)
_cell_length_c                   18.2092(4)
_cell_measurement_reflns_used    3244
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2506.98(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0153
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5550
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.9065
_exptl_absorpt_correction_T_min  0.7394
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'shaped leaves'
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0824
_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^)+(0.1886P)^2^+2.1874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2639
_refine_ls_wR_factor_ref         0.2841
_reflns_number_gt                2382
_reflns_number_total             3053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b03070_si_002.cif
_cod_data_source_block           fepytren2py
_cod_database_code               4345783