Synthesis and structural studies of germyl and germyl/stannyl substituted tungstenocenes
Khalimon, Andrey Yu.; Dorogov, Konstantin Yu.; Churakov, Andrei V.; Kuzmina, Lyudmila G.; Lemenovskii, Dmitry A.; Howard, Judith A. K.; Nikonov, Georgii I.; Dalton Transactions  (2007) 2440–; doi:10.1039/b618806k

data_7005273
_publ_section_title
;
 Synthesis and structural studies of germyl and germyl/stannyl
 substituted tungstenocenes
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              2440
_journal_paper_doi               10.1039/b618806k
_journal_year                    2007
_chemical_formula_moiety         'C16 H26 Br1.71 Cl0.29 Ge Sn W'
_chemical_formula_sum            'C16 H26 Br1.71 Cl0.29 Ge Sn W'
_chemical_formula_weight         740.42
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 90.741(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5322(3)
_cell_length_b                   8.7717(2)
_cell_length_c                   14.2873(2)
_cell_measurement_reflns_used    7509
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.000
_cell_measurement_theta_min      2.623
_cell_volume                     1946.39(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART 6K'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10353
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.246
_exptl_absorpt_correction_T_max  0.2166
_exptl_absorpt_correction_T_min  0.1308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    2.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1371
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.224
_refine_diff_density_min         -4.672
_refine_diff_density_rms         0.281
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         4906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0620P)^2^+24.9074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1171
_reflns_number_gt                4540
_reflns_number_total             4906
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b618806k.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7005273