Synthesis and Characterization of an Amidinate-Stabilized Bisgermylene Oxide and Sulfide
Zhang, Shu-Hua; So, Cheuk-Wai; Organometallics 30 (2011) 2059–; doi:10.1021/om101194f

data_4064231
_publ_section_title
;
 Synthesis and Characterization of an Amidinate-Stabilized Bisgermylene
 Oxide and Sulfide
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2059
_journal_paper_doi               10.1021/om101194f
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C66 H102 Ge2 N4 O2 S'
_chemical_formula_weight         1160.76
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.213(5)
_cell_angle_beta                 100.902(5)
_cell_angle_gamma                109.631(3)
_cell_formula_units_Z            2
_cell_length_a                   13.4937(15)
_cell_length_b                   13.5639(10)
_cell_length_c                   19.802(2)
_cell_measurement_reflns_used    4194
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      23.38
_cell_measurement_theta_min      2.36
_cell_volume                     3267.5(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1235
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14916
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  0.9070
_exptl_absorpt_correction_T_min  0.6916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   twinabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.199
_refine_diff_density_min         -1.713
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         14916
_refine_ls_number_restraints     274
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.0885
_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^)+(0.1084P)^2^+14.3325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2153
_refine_ls_wR_factor_ref         0.2387
_reflns_number_gt                9693
_reflns_number_total             14916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101194f_si_001.cif
_cod_data_source_block           scw273s_3m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3267.6(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064231