Unexpected Formation of Ga4C2H4Heteroadamantane Cages by the Reaction of Carbon-Bridged Bis(dichlorogallium) Compounds withtert-Butyllithium
Uhl, Werner; Kovert, Dirk; Zemke, Sarina; Hepp, Alexander; Organometallics 30 (2011) 4736–; doi:10.1021/om200573g

data_4065120
_publ_section_exptl_refinement
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The weak completeness of X-ray data is a well-known phenomenon for these 
X-ray machines and particularly distinct for copper radiation. It has 
already been discussed in the respective internet forum. The problematic
measurements were partially carried out with copper radiation. The 
completeness in such measurements is generally even lower than those with
Mo radiation, particularly when the crystal symmetry (redundancy within 
the measurement) is low (triclinic in our case). Furthermore, the problem 
is aggravated when the measurement is carried out to angles in 2 theta 
well above the required minimum of 135 degrees. We always carry our Cu 
measurements to the physical maximum of 150&#x00B0;. When tested, our data 
showed a substantial increase in completeness when reduced to the 
required minimum in 2 theta. Since we are primarily interested in maximum 
crystallographic information, we used the complete measurement for the 
structure determination. 
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_publ_section_title
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 Unexpected Formation of Ga4C2H4Heteroadamantane Cages by the Reaction of
 Carbon-Bridged Bis(dichlorogallium) Compounds withtert-Butyllithium
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_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4736
_journal_paper_doi               10.1021/om200573g
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C58 H80 Ga4 Si2'
_chemical_formula_weight         1112.28
_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                105.1853(4)
_cell_angle_beta                 96.4344(4)
_cell_angle_gamma                108.6446(4)
_cell_formula_units_Z            2
_cell_length_a                   10.8708(3)
_cell_length_b                   13.5950(4)
_cell_length_c                   21.3470(6)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      31.91
_cell_measurement_theta_min      1.65
_cell_volume                     2817.99(14)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      153(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35340
_diffrn_reflns_theta_full        31.91
_diffrn_reflns_theta_max         31.91
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  0.8745
_exptl_absorpt_correction_T_min  0.8275
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         17779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                13420
_reflns_number_total             17779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200573g_si_004.cif
_cod_data_source_block           sad
_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        2817.98(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065120