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_4081213
_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         'C29 H34 Ge O2 Si W'
_chemical_formula_sum            'C29 H34 Ge O2 Si W'
_chemical_formula_weight         699.11
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.460(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.654(3)
_cell_length_b                   18.836(5)
_cell_length_c                   12.897(4)
_cell_measurement_reflns_used    9126
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.16
_cell_volume                     2828.5(14)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0418
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40521
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.196
_exptl_absorpt_correction_T_max  0.354
_exptl_absorpt_correction_T_min  0.202
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1376.00
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.700
_refine_diff_density_min         -1.350
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6465
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0277P)^2^+1.5697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0516
_reflns_number_gt                6280
_reflns_number_total             6465
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om4000264_si_002.cif
_cod_data_source_block           complex7a
_cod_original_cell_volume        2828.4(13)
_cod_database_code               4081213