Trans-selective hydrogermylation of alkynes promoted by methyliron and bis(germyl)hydridoiron complexes as a catalyst precursor
Masumi Itazaki; Masahiro Kamitani; Hiroshi Nakazawa; Chem.Commun. 47 (2011) 7854–; doi:10.1039/c1cc12530c

data_7106622
_publ_section_title
;
 Trans-selective hydrogermylation of alkynes promoted by methyliron and
 bis(germyl)hydridoiron complexes as a catalyst precursor
;
_journal_name_full               Chem.Commun.
_journal_page_first              7854
_journal_paper_doi               10.1039/c1cc12530c
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C42 H36 Fe Ge2 O'
_chemical_formula_sum            'C42 H36 Fe Ge2 O'
_chemical_formula_weight         757.74
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.061(9)
_cell_angle_beta                 87.698(8)
_cell_angle_gamma                74.396(7)
_cell_formula_units_Z            4
_cell_length_a                   12.931(2)
_cell_length_b                   14.400(2)
_cell_length_c                   19.151(3)
_cell_measurement_reflns_used    14656
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.0511
_cell_volume                     3430.9(9)
_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_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31455
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         4.05
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  0.8107
_exptl_absorpt_correction_T_min  0.5791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.269
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         13765
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+55.1293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.1877
_reflns_number_gt                12351
_reflns_number_total             13765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12530c.txt
_cod_data_source_block           KAM356
_cod_original_cell_volume        3431.0(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7106622