Synthesis and properties of stable 2-metallanaphthalenes of heavier group 14 elements
Mizuhata, Yoshiyuki; Sasamori, Takahiro; Nagahora, Noriyoshi; Watanabe, Yasuaki; Furukawa, Yukio; Tokitoh, Norihiro; Dalton Transactions  (2008) 4409–4418; doi:10.1039/b718193k

data_7003666
_publ_section_title
;
 Synthesis and properties of stable 2-metallanaphthalenes of heavier
 group 14 elements
;
_journal_issue                   33
_journal_name_full               'Dalton Transactions'
_journal_page_first              4409
_journal_page_last               4418
_journal_paper_doi               10.1039/b718193k
_journal_year                    2008
_chemical_formula_moiety         'C40 H74 Ge Si6'
_chemical_formula_sum            'C40 H74 Ge Si6'
_chemical_formula_weight         796.12
_chemical_name_common            2-germanaphthalene
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.2068(3)
_cell_length_b                   22.3394(7)
_cell_length_c                   45.9538(19)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.88
_cell_volume                     9451.5(6)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'RIGAKU Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            96496
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.9599
_exptl_absorpt_correction_T_min  0.8863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.611
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.303
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8303
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.302
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.1103
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+55.2113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2453
_refine_ls_wR_factor_ref         0.2572
_reflns_number_gt                6275
_reflns_number_total             8303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718193k.txt
_cod_data_source_block           2genp
_cod_original_sg_symbol_Hall     ' -P 2ac 2ab'
_cod_database_code               7003666