Inorganic Asymmetric Synthesis: Asymmetric Synthesis of a Two-Bladed Propeller, Octahedral Metal Complex
Warr, Rebecca J.; Willis, Anthony C.; Wild, S. Bruce; Inorganic Chemistry 45 (2006) 8618–8627; doi:10.1021/ic060856q

data_4332799
_publ_section_title
;
 Inorganic Asymmetric Synthesis:&#x00A0; Asymmetric Synthesis of a
 Two-Bladed Propeller, Octahedral Metal Complex
;
_journal_issue                   21
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8618
_journal_page_last               8627
_journal_paper_doi               10.1021/ic060856q
_journal_volume                  45
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_compound_source
;
?
;
_chemical_formula_moiety
' C31 H30 Fe N8 O6 S2 2+, 2(C6 H5 O3 S -), 2(C H4 O), 3(H2 O)'
_chemical_formula_sum            'C45 H54 Fe N8 O17 S2'
_chemical_formula_weight         1098.95
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-12-04
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2005-04-12 - Report on C45 H54 Fe N8 O17 S2 
             by Anthony C. Willis
             for Rebecca J. Warr and S. Bruce Wild

2005-04-12 - passes checkcif tests with minor warnings  

;
_cell_angle_alpha                90
_cell_angle_beta                 101.8508(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1842(1)
_cell_length_b                   19.8044(3)
_cell_length_c                   14.2977(2)
_cell_measurement_reflns_used    44977
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     2545.14(6)
_computing_cell_refinement
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
 COLLECT (Nonius BV, 1997) 
;
_computing_data_reduction
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_molecular_graphics
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
; 
Nonius Kappa CCD 
;
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            52078
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.638
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            ' red '
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             1148.0
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.48
_refine_ls_abs_structure_details 'Flack, 5664 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.010(11)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         8221
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.003790
_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: 
 1.24 0.651 0.982 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0458
_refine_ls_wR_factor_gt          0.0401
_refine_ls_wR_factor_ref         0.0401
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              25
_reflns_limit_k_min              -25
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                8221
_reflns_number_total             11626
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic060856qsup1.cif
_cod_data_source_block           rjw11
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        ' C45 H54 Fe N8 O17 S2 '
_cod_database_code               4332799