A Ruthenium Dihydrogen Germylene Complex and the Catalytic Synthesis of Digermoxane
Smart, Katharine A.; Mothes-Martin, Emmanuelle; Vendier, Laure; Perutz, Robin N.; Grellier, Mary; Sabo-Etienne, Sylviane; Organometallics 34 (2015) 4158–; doi:10.1021/acs.organomet.5b00570

data_4086147
_publ_section_title
;
 A Ruthenium Dihydrogen Germylene Complex and the Catalytic Synthesis of
 Digermoxane
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4158
_journal_paper_doi               10.1021/acs.organomet.5b00570
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C64 H100 Ge2 O2 P2 Ru'
_chemical_formula_sum            'C64 H100 Ge2 O2.5 P2 Ru'
_chemical_formula_weight         1217.63
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-06-28T16:08:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.1010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7310(2)
_cell_length_b                   12.2590(3)
_cell_length_c                   21.6540(3)
_cell_measurement_reflns_used    10795
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.3534
_cell_measurement_theta_min      3.0667
_cell_measurement_wavelength     0.71073
_cell_volume                     3055.80(10)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0144471
_diffrn_orient_matrix_UB_12      0.0492794
_diffrn_orient_matrix_UB_13      -0.013861
_diffrn_orient_matrix_UB_21      0.0183319
_diffrn_orient_matrix_UB_22      0.0230022
_diffrn_orient_matrix_UB_23      0.0303433
_diffrn_orient_matrix_UB_31      0.0570028
_diffrn_orient_matrix_UB_32      -0.0198774
_diffrn_orient_matrix_UB_33      0.0007094
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24122
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_correction_T_min  0.9532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         10865
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+1.0370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                10088
_reflns_number_total             10865
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00570_si_003.cif
_cod_data_source_block           Germoxane2
_cod_depositor_comments
'Adding full bibliography for 4086145--4086147.cif.'
_cod_original_formula_sum        'C64 H100 Ge2 O2.50 P2 Ru'
_cod_database_code               4086147