Iron Complexes of New Pentadentate Ligands Containing the 1,4,7-Triazacyclononane-1,4-diacetate Motif. Spectroscopic, Electro-, and Photochemical Studies
Yu-Fei Song; John F. Berry; Eckhard Bill; Eberhard Bothe; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 46 (2007) 2208–2219; doi:10.1021/ic062001j

data_4307505
_publ_contact_author_address
;  Department of Chemistry
   University of Glasgow
   G12, 8QQ, Glasgow
   UK
;
_publ_contact_author_email       ysong@chem.gla.ac.uk
_publ_contact_author_name        'Y.-F. Song'
_publ_section_title
;
Iron Complexes of New Pentadentate Ligands Containing the
1,4,7-Triazacyclononane-1,4-diacetate Motif. Spectroscopic, Electro-, and
Photochemical Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2208
_journal_page_last               2219
_journal_paper_doi               10.1021/ic062001j
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '[C17 H23 Cl Fe N3 O4], 0.5 EtOH, 0.5 H2O'
_chemical_formula_sum            'C18 H27 Cl Fe N3 O5'
_chemical_formula_weight         456.73
_chemical_name_systematic
; 
 ? 
;
_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                73.25(1)
_cell_angle_beta                 89.24(1)
_cell_angle_gamma                88.90(1)
_cell_formula_units_Z            4
_cell_length_a                   8.3266(6)
_cell_length_b                   13.0757(9)
_cell_length_c                   19.1902(12)
_cell_measurement_reflns_used    68458
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.00
_cell_measurement_theta_min      2.91
_cell_volume                     2000.3(3)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker-Nonius Kappa-CCD'
_diffrn_measurement_method
'773 images at 1.0 deg. stepwise rotation in omega and phi, 15 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40720
_diffrn_reflns_theta_full        31.01
_diffrn_reflns_theta_max         31.01
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent plate'
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.387
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         12673
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          1.502
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+2.6841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                11040
_reflns_number_total             12673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062001jsi20070105_015228_3.cif
_cod_data_source_block           18
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+2.6841P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+2.6841P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2000.3(2)
_cod_database_code               4307505