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_4081215
_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         'C33 H40 Ge O3 W '
_chemical_formula_sum            'C33 H40 Ge O3 W'
_chemical_formula_weight         741.12
_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'
_cell_angle_alpha                90.0000
_cell_angle_beta                 115.429(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   19.088(6)
_cell_length_b                   8.558(2)
_cell_length_c                   20.428(6)
_cell_measurement_reflns_used    7861
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3013.7(15)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_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            43036
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    4.846
_exptl_absorpt_correction_T_max  0.379
_exptl_absorpt_correction_T_min  0.263
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472.00
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.41
_refine_diff_density_min         -2.28
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6868
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1181P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1830
_reflns_number_gt                5942
_reflns_number_total             6868
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om4000264_si_002.cif
_cod_data_source_block           complex8b
_cod_original_cell_volume        3013.9(15)
_cod_original_formula_sum        'C33 H40 Ge O3 W '
_cod_database_code               4081215