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_4307504
_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_sum            'C71 H122 F6 Fe4 N12 Na O35 P'
_chemical_formula_weight         2095.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.229(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4915(6)
_cell_length_b                   16.5318(6)
_cell_length_c                   36.239(2)
_cell_measurement_temperature    100(2)
_cell_volume                     9801.5(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius Kappa-CCD'
_diffrn_measurement_method
'1673 images at 0.5 deg. stepwise rotation in omega and phi, 30 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            115757
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.9464
_exptl_absorpt_correction_T_min  0.8452
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             4384
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1219
_refine_ls_number_reflns         17196
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0980
_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^)+(0.0477P)^2^+89.1320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2135
_refine_ls_wR_factor_ref         0.2203
_reflns_number_gt                14763
_reflns_number_total             17196
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062001jsi20070105_015228_2.cif
_cod_data_source_block           17
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' 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 

2023-09-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C35.5 H61 F3 Fe2 N6 Na0.5 O17.5 P0.5'
_cod_original_formula_weight         1047.59
_cod_original_formula_units_Z            8
_cod_database_code               4307504