Synthesis of Fe‒H/Si‒H and Fe‒H/Ge‒H Bifunctional Complexes and Their Catalytic Hydrogenation Reactions toward Nonpolar Unsaturated Organic Molecules
Kamitani, Masahiro; Nishiguchi, Yoshinori; Tada, Ryosuke; Itazaki, Masumi; Nakazawa, Hiroshi; Organometallics 33 (2014) 1532–; doi:10.1021/om5000562

data_4082868
_publ_section_title
;
 Synthesis of Fe--H/Si--H and Fe--H/Ge--H Bifunctional Complexes and Their
 Catalytic Hydrogenation Reactions toward Nonpolar Unsaturated Organic
 Molecules
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1532
_journal_paper_doi               10.1021/om5000562
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety
'C49 H41 Fe N O3 Si2, 0.5(C6 H14), 0.25(C H2 Cl2)'
_chemical_formula_sum            'C52.25 H48.5 Cl0.5 Fe N O3 Si2'
_chemical_formula_weight         868.18
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                73.409(5)
_cell_angle_beta                 90.112(8)
_cell_angle_gamma                78.748(6)
_cell_formula_units_Z            4
_cell_length_a                   13.7402(5)
_cell_length_b                   18.28100(10)
_cell_length_c                   19.4265(5)
_cell_measurement_reflns_used    11288
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.0112
_cell_volume                     4578.0(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
scan:
    Number of images: 600
               Slice: -80.0000 - 100.0000
         Image width: 0.3000
            Exp time: 7.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 45.2736
              2theta: 19.7962
scan:
    Number of images: 160
               Slice: -20.0000 - 28.0000
         Image width: 0.3000
            Exp time: 7.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 45.2736
              2theta: 19.7962
scan:
    Number of images: 160
               Slice: -20.0000 - 28.0000
         Image width: 0.3000
            Exp time: 7.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 45.2736
              2theta: 19.7962
scan:
    Number of images: 160
               Slice: -20.0000 - 28.0000
         Image width: 0.3000
            Exp time: 7.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 45.2736
              2theta: 19.7962
scan:
    Number of images: 160
               Slice: -20.0000 - 28.0000
         Image width: 0.3000
            Exp time: 7.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 270.0000
                 XTD: 45.2736
              2theta: 19.7962

;
_diffrn_measurement_device       'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_device_details 'AFC7: Eulerian 3-circle'
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\w or \f'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0742
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37091
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.01
_diffrn_source_current           280.0000
_diffrn_source_power             16.8000
_diffrn_source_voltage           60.0000
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_T_max  0.9350
_exptl_absorpt_correction_T_min  0.8949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1822
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 200(2) K'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.573
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         20705
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0835
_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^)+(0.0881P)^2^+7.1395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.2121
_reflns_number_gt                16225
_reflns_number_total             20705
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5000562_si_001.cif
_cod_data_source_block           KAM1237
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4082868.cif.
;
_cod_original_cell_volume        4578.0(2)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C52.25 H48.50 Cl0.50 Fe N O3 Si2'
_cod_database_code               4082868