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_7004219
_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         'C48 H73 Fe1 N2 O3'
_chemical_formula_sum            'C48 H73 Fe N2 O3'
_chemical_formula_weight         781.97
_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
_audit_creation_date             07-11-09
_audit_creation_method           CRYSTALS_ver_12.80
_cell_angle_alpha                90
_cell_angle_beta                 115.7166(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4928(3)
_cell_length_b                   19.4211(4)
_cell_length_c                   16.9802(4)
_cell_measurement_reflns_used    40111
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     4603.07(17)
_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 0.990
_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  0.053
_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            40111
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         5.103
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.46
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0735
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         7378
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.000515
_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:
3.45 -0.465 2.82
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0474
_refine_ls_wR_factor_gt          0.0453
_refine_ls_wR_factor_ref         0.0453
_reflns_limit_h_max              18
_reflns_limit_h_min              -20
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                7378
_reflns_number_total             10776
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.7962(10)
_cod_data_source_file            b804414g.txt
_cod_data_source_block           5
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C48 H73 Fe1 N2 O3'
_cod_database_code               7004219