A Schrock-Type Germylene Complex: (η5-C5H4Et)2(PMe3)Hf═Ge(SiMetBu2)2
Nakata, Norio; Aoki, Shinji; Lee, Vladimir Ya.; Sekiguchi, Akira; Organometallics 34 (2015) 2699–; doi:10.1021/om501134a

data_4085355
_publ_section_title
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 A Schrock-Type Germylene Complex:
 (\h5-C5H4Et)2(PMe3)Hf&#x2550;Ge(SiMetBu2)2
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_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2699
_journal_paper_doi               10.1021/om501134a
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C35 H69 Ge Hf P Si2'
_chemical_formula_sum            'C35 H69 Ge Hf P Si2'
_chemical_formula_weight         828.13
_chemical_name_common            'Hf=Ge complex'
_chemical_name_systematic
; 
 Hf-germylene complex 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 118.260(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.1620(5)
_cell_length_b                   11.8050(5)
_cell_length_c                   19.6810(9)
_cell_measurement_reflns_used    6581
_cell_measurement_temperature    120(2)
_cell_volume                     3921.3(3)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'MacScience DIP2030 Image plate'
_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  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6581
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    3.535
_exptl_absorpt_correction_T_max  0.6191
_exptl_absorpt_correction_T_min  0.5383
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.006
_refine_diff_density_min         -3.609
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0961P)^2^+3.7346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1259
_reflns_number_gt                6220
_reflns_number_total             6581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501134a_si_002.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4085355.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4085355