Linking iron(iii) carboxylates into high-nuclearity complexes by using Bis-tris
Ferguson, Alan; McGregor, Julie; Parkin, Andrew; Murrie, Mark; Dalton Transactions  (2008) 731–733; doi:10.1039/b715932c

data_7003402
_publ_section_title
;
 Linking iron(iii) carboxylates into high-nuclearity complexes by using
 Bis-tris
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              731
_journal_page_last               733
_journal_paper_doi               10.1039/b715932c
_journal_year                    2008
_chemical_formula_moiety
'C83 H157 Cl4 Fe10 N2 Na1 O44. 0.5CH2Cl2 . 0.625H2O'
_chemical_formula_sum            'C83.5 H159.25 Cl5 Fe10 N2 Na O44.625'
_chemical_formula_weight         2664.14
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2n'
_symmetry_space_group_name_H-M   'P n a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-08-31
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6011(11)
_cell_length_b                   23.6529(18)
_cell_length_c                   29.306(2)
_cell_measurement_reflns_used    10447
_cell_measurement_temperature    120
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     12200.6(15)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    Mercury
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.101
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            53691
_diffrn_reflns_theta_full        25.120
_diffrn_reflns_theta_max         27.605
_diffrn_reflns_theta_min         2.915
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.45
_exptl_crystal_description       rod
_exptl_crystal_F_000             5440
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.92
_refine_diff_density_min         -1.82
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9936
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         13376
_refine_ls_number_restraints     252
_refine_ls_R_factor_all          0.1696
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.007563
_refine_ls_structure_factor_coef Fsqd
_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:
867. 718. 152. -7.72
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1147
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.1147
_reflns_limit_h_max              22
_reflns_limit_h_min              0
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              38
_reflns_limit_l_min              0
_reflns_number_gt                5641
_reflns_number_total             24131
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.9554(18)
_cod_data_source_file            b715932c.txt
_cod_data_source_block           2006src0286
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 n a m '
_cod_original_formula_sum        'C83.5 H159.25 Cl5 Fe10 N2 Na1 O44.625'
_cod_database_code               7003402