Synthesis, Structure, and Reactivity of Tungsten Acetylide‒Germylene Complexes
Sakaba, Hiroyuki; Arai, Yasuhiro; Suganuma, Kensei; Kwon, Eunsang; Organometallics 32 (2013) 5038–; doi:10.1021/om4000264

data_4081214
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Tungsten Acetylide--Germylene
 Complexes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5038
_journal_paper_doi               10.1021/om4000264
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C32 H40 Ge O3 Si W'
_chemical_formula_sum            'C32 H40 Ge O3 Si W'
_chemical_formula_weight         757.19
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 114.918(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   19.491(5)
_cell_length_b                   8.503(2)
_cell_length_c                   20.556(5)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.27
_cell_measurement_theta_min      2.40
_cell_volume                     3089.7(13)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44278
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.765
_exptl_absorpt_correction_T_max  0.538
_exptl_absorpt_correction_T_min  0.377
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1504.00
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.870
_refine_diff_density_min         -0.680
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     343
_refine_ls_number_reflns         7071
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0318P)^2^+3.5391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                6640
_reflns_number_total             7074
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om4000264_si_002.cif
_cod_data_source_block           complex8a
_cod_original_cell_volume        3089.8(13)
_cod_database_code               4081214