Inorganic Asymmetric Synthesis: Diastereoselective Syntheses of Mono- and Dinuclear Complexes Containing Octahedral, Two-Bladed Propeller, Bis(pyridine-2-aldehyde 2'-pyridylhydrazone)iron(II) Stereocenters
Rebecca J. Warr; Anthony C. Willis; S. Bruce Wild; Inorganic Chemistry 47 (2008) 9351–9362; doi:10.1021/ic800936d

data_4306003
_publ_contact_author_address
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email       ' sbw@rsc.anu.edu.au '
_publ_contact_author_fax         ' 61 2 6125 0750 '
_publ_contact_author_name        ' S. Bruce Wild '
_publ_contact_author_phone       ' 61 2 6125 4236 '
_publ_section_title
;
Inorganic Asymmetric Synthesis: Diastereoselective Syntheses of Mono- and
Dinuclear Complexes Containing Octahedral, Two-Bladed Propeller,
Bis(pyridine-2-aldehyde 2'-pyridylhydrazone)iron(II) Stereocenters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9351
_journal_page_last               9362
_journal_paper_doi               10.1021/ic800936d
_journal_volume                  47
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C47 H44 N8 O4, 2.5(C H Cl3)'
_chemical_formula_sum            'C49.5 H46.5 Cl7.5 N8 O4'
_chemical_formula_weight         1083.36
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             04-27-08
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2004-09-07 - Report on C47 H44 N8 O4, 2.5(C H Cl3)
             by Anthony C. Willis
             for Rebecca J. Warr and S. Bruce Wild

2004-09-07 - passes checkcif tests with minor warnings  
2008-05-20 - start to put 3 cifs together for paper

;
_cell_angle_alpha                90
_cell_angle_beta                 100.813(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.4763(8)
_cell_length_b                   16.5010(7)
_cell_length_c                   11.2234(4)
_cell_measurement_reflns_used    30854
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     5543.9(3)
_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 0.99
_diffrn_measured_fraction_theta_max 0.986
_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       31
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24875
_diffrn_reflns_theta_full        25.
_diffrn_reflns_theta_max         25.097
_diffrn_reflns_theta_min         2.722
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             2236
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.69
_refine_ls_abs_structure_details 'Flack, 3788 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.10(11)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0675
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         6405
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.005780
_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: 
 2.91 1.21 2.28 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0823
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0755
_reflns_limit_h_max              35
_reflns_limit_h_min              -36
_reflns_limit_k_max              19
_reflns_limit_k_min              -17
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                6405
_reflns_number_total             8930
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic800936d_si_001_1.cif
_cod_data_source_block           rjw5a
_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      'C 1 2 1 '
_cod_original_formula_sum        ' C49.5 H46.5 Cl7.5 N8 O4 '
_cod_database_code               4306003