Anionic Iron Complexes with a Bond between an Ate-Type Pentacoordinated Germanium and an Iron Atom
Kano, Naokazu; Yoshinari, Naohito; Shibata, Yusuke; Miyachi, Mariko; Kawashima, Takayuki; Enomoto, Masaya; Okazawa, Atsushi; Kojima, Norimichi; Guo, Jing-Dong; Nagase, Shigeru; Organometallics 31 (2012) 8059–; doi:10.1021/om300915y

data_4079656
_publ_section_title
;
 Anionic Iron Complexes with a Bond between an Ate-Type Pentacoordinated
 Germanium and an Iron Atom
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8059
_journal_paper_doi               10.1021/om300915y
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C39 H41 F12 Fe Ge Na O7'
_chemical_formula_sum            'C39 H41 F12 Fe Ge Na O7'
_chemical_formula_weight         1001.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.17(7)
_cell_angle_beta                 76.90(7)
_cell_angle_gamma                77.94(7)
_cell_formula_units_Z            2
_cell_length_a                   9.547(10)
_cell_length_b                   11.309(13)
_cell_length_c                   20.59(2)
_cell_measurement_reflns_used    4915
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0817
_cell_volume                     2094(4)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 14.5666
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
scan:
    Number of images: 600
               Slice: -70.0000 - 110.0000
         Image width: 0.3000
            Exp time: 22.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.2007
              2theta: 19.3994
scan:
    Number of images: 600
               Slice: -70.0000 - 110.0000
         Image width: 0.3000
            Exp time: 22.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.2007
              2theta: 19.3994

;
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC8: Eulerian 3-circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0897
_diffrn_orient_matrix_UB_12      0.0379
_diffrn_orient_matrix_UB_13      -0.0495
_diffrn_orient_matrix_UB_21      0.0222
_diffrn_orient_matrix_UB_22      -0.0884
_diffrn_orient_matrix_UB_23      0.0077
_diffrn_orient_matrix_UB_31      -0.0319
_diffrn_orient_matrix_UB_32      -0.0037
_diffrn_orient_matrix_UB_33      -0.0389
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_sigmaI/netI    0.1193
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13764
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  0.8915
_exptl_absorpt_correction_T_min  0.7989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Rigaku, private communication
;
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         7183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1447
_reflns_number_gt                4816
_reflns_number_total             7183
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300915y_si_002.cif
_cod_data_source_block           gefe2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_database_code               4079656