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_4079657
_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         'C27 H17 F12 Fe Ge O4, C10 H16 N'
_chemical_formula_sum            'C37 H33 F12 Fe Ge N O4'
_chemical_formula_weight         912.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.267(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.703(2)
_cell_length_b                   18.313(5)
_cell_length_c                   20.760(5)
_cell_measurement_reflns_used    8952
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5029
_cell_measurement_theta_min      3.0085
_cell_volume                     3682.9(15)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 24.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.0216
              2theta: -19.9478
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 24.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.0216
              2theta: -19.9478

;
_diffrn_measurement_device
;
Saturn724 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0433
_diffrn_orient_matrix_UB_12      -0.0374
_diffrn_orient_matrix_UB_13      -0.0859
_diffrn_orient_matrix_UB_21      0.0074
_diffrn_orient_matrix_UB_22      -0.0481
_diffrn_orient_matrix_UB_23      0.0247
_diffrn_orient_matrix_UB_31      -0.0421
_diffrn_orient_matrix_UB_32      -0.0156
_diffrn_orient_matrix_UB_33      -0.0178
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27203
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    1.312
_exptl_absorpt_correction_T_max  0.7793
_exptl_absorpt_correction_T_min  0.6218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998),  private communication
;
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.908
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         8358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+9.1641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1463
_reflns_number_gt                6990
_reflns_number_total             8358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300915y_si_002.cif
_cod_data_source_block           gefebn20
_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_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4079657