Digermylene Oxide Complexes: Facile Synthesis and Reactivity
Rahul Kumar Siwatch; Dhirendra Yadav; Goutam Mukherjee; Gopalan Rajaraman; Selvarajan Nagendran; Inorganic Chemistry 52 (2013) 13384–13391; doi:10.1021/ic401720e

data_4336812
_publ_contact_author_address
; 
      Department of Chemistry 
      Indian Institute of Technology
      Hauz Khas, New Delhi 110016
      India
;
_publ_contact_author_email       sisn@chemistry.iitd.ac.in
_publ_contact_author_fax         +91-11-26582277
_publ_contact_author_name        'S. Nagendran and R. K. Siwatch'
_publ_contact_author_phone       +91-11-26591523
_publ_section_title
;
 Digermylene Oxide Complexes: Facile Synthesis and Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13384
_journal_page_last               13391
_journal_paper_doi               10.1021/ic401720e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C30 H46 Ge2 N4 O Se2'
_chemical_formula_sum            'C30 H46 Ge2 N4 O Se2'
_chemical_formula_weight         781.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                   26.138(6)
_cell_length_b                   27.882(6)
_cell_length_c                   9.316(2)
_cell_measurement_reflns_used    3348
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.44
_cell_volume                     6789(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8721
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    3.943
_exptl_absorpt_correction_T_max  0.522
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       Block
_exptl_crystal_F_000             3152.0
_exptl_crystal_size_max          0.531
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.183
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2613
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0333P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                1594
_reflns_number_total             1600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401720e_si_001_4.cif
_cod_data_source_block           6
_cod_original_sg_symbol_Hall     'F 2 -2d '
_cod_database_code               4336812