Coordination Equilibria Between Seven- and Five-coordinate Iron(II) Complexes
Michaela Grau; Jason England; Rafael Torres Martin de Rosales; Henry S. Rzepa; Andrew J. P. White; George J. P. Britovsek; Inorganic Chemistry 52 (2013) 11867–11874; doi:10.1021/ic401416h

data_4336427
_publ_section_title
;
 Coordination Equilibria Between Seven- and Five-coordinate Iron(II)
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11867
_journal_page_last               11874
_journal_paper_doi               10.1021/ic401416h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C21 H25 Fe N5, 2(C F3 O3 S)'
_chemical_formula_sum            'C23 H25 F6 Fe N5 O6 S2'
_chemical_formula_weight         701.45
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 129.267(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.4112(9)
_cell_length_b                   10.5689(2)
_cell_length_c                   15.0745(6)
_cell_measurement_reflns_used    9408
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.5625
_cell_measurement_theta_min      4.1608
_cell_volume                     2764.4(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 15.9863
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0119
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13890
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         32.64
_diffrn_reflns_theta_min         4.23
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       tablets
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.4275
_exptl_crystal_size_mid          0.4100
_exptl_crystal_size_min          0.1819
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0990P)^2^+1.3233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1409
_reflns_number_gt                4436
_reflns_number_total             4741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401416h_si_001_3.cif
_cod_data_source_block           '[Fe(1)](OTf)2'
_cod_database_code               4336427