Synthesis, structures and catalytic properties of iron(iii) complexes with asymmetric N-capped tripodal NO3 ligands and a pentadentate N2O3 ligand
Tong, Lok H.; Wong, Yee-Lok; Pascu, Sofia I.; Dilworth, Jonathan R.; Dalton Transactions  (2008) 4784–4791; doi:10.1039/b804414g

data_7004218
_publ_section_title
;
 Synthesis, structures and catalytic properties of iron(iii) complexes
 with asymmetric N-capped tripodal NO3 ligands and a pentadentate N2O3
 ligand
;
_journal_issue                   35
_journal_name_full               'Dalton Transactions'
_journal_page_first              4784
_journal_page_last               4791
_journal_paper_doi               10.1039/b804414g
_journal_year                    2008
_chemical_formula_moiety         'C40.36 H54.43 Cl1 Fe1 N3 O3.36'
_chemical_formula_sum            'C40.36 H54.43 Cl Fe N3 O3.36'
_chemical_formula_weight         726.63
_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
_audit_creation_date             07-11-09
_audit_creation_method           CRYSTALS_ver_12.80
_cell_angle_alpha                94.0494(11)
_cell_angle_beta                 94.7940(11)
_cell_angle_gamma                112.5924(11)
_cell_formula_units_Z            2
_cell_length_a                   11.2778(2)
_cell_length_b                   13.6398(3)
_cell_length_c                   14.0391(3)
_cell_measurement_reflns_used    27291
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     1974.47(7)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius (1997-2001). COLLECT.'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27291
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.437
_diffrn_reflns_theta_min         5.124
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            darkbrown
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       block
_exptl_crystal_F_000             774.859
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.16
_refine_diff_density_min         -1.05
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0417
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6725
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.003125
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
6.28 2.13 5.46
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0670
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0655
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                6725
_reflns_number_total             8924
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          1.389(3)
_cod_data_source_file            b804414g.txt
_cod_data_source_block           3
_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 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C40.36 H54.43 Cl1 Fe1 N3 O3.36'
_cod_database_code               7004218