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_7003403
_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         'C86 H163.00 Fe10 N7 O44.00'
_chemical_formula_sum            'C86 H163 Fe10 N7 O44'
_chemical_formula_weight         2557.73
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-07-27
_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                   23.6467(11)
_cell_length_b                   24.0903(12)
_cell_length_c                   20.2106(10)
_cell_measurement_reflns_used    7435
_cell_measurement_temperature    100
_cell_measurement_theta_max      32
_cell_measurement_theta_min      2
_cell_volume                     11513.1(10)
_computing_cell_refinement       APEXII
_computing_data_collection       'APEXII (Bruker, 2006)'
_computing_data_reduction        APEXII
_computing_molecular_graphics    MERCURY
_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      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15509
_diffrn_reflns_theta_full        29.158
_diffrn_reflns_theta_max         29.158
_diffrn_reflns_theta_min         1.207
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       block
_exptl_crystal_F_000             5360
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.41
_refine_diff_density_min         -1.00
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0722
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         15509
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001278
_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:
314. 524. 326. 148. 37.6
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1434
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.1434
_reflns_limit_h_max              32
_reflns_limit_h_min              0
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                8577
_reflns_number_total             73922
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.21
_oxford_diffrn_Wilson_scale      148.55
_oxford_refine_ls_scale          0.3133(2)
_oxford_structure_analysis_title 'jm8 in Pccn'
_cod_data_source_file            b715932c.txt
_cod_data_source_block           jm8
_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 c c n '
_cod_original_formula_sum        'C86 H163.00 Fe10 N7 O44.00'
_cod_database_code               7003403