Structural Evidence of the Epoxide Oxygen Propensity to Double Coordination
Janusz Lewiński; Janusz Zachara; Paweł Horeglad; Daniel Glinka; Janusz Lipkowski; Iwona Justyniak; Inorganic Chemistry 40 (2001) 6086–6087; doi:10.1021/ic015572e

data_4320623
_publ_contact_author
;
   Dr. Janusz Lewinski,
   Department of Chemistry
   Warsaw University of Technology,
   Noakowskiego 3,
   PL-00-664 Warszawa
   Poland
;
_publ_contact_author_email       lewin@ch.pw.edu.pl
_publ_contact_author_fax         '048 22 6607279'
_publ_contact_author_phone       '048 22 6607315'
_publ_section_title
;
 Structural Evidence of the Epoxide Oxygen Propensity to Double
 Coordination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6086
_journal_page_last               6087
_journal_paper_doi               10.1021/ic015572e
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C16 H40 Ga4 O4'
_chemical_formula_structural     '[Ga(CH3)2(C3H5O2)Ga(CH3)3]2'
_chemical_formula_sum            'C16 H40 Ga4 O4'
_chemical_formula_weight         575.36
_chemical_name_systematic
; 
 bis(\m~3~-Glycidolato-O,O')-decamethyl-tetragallium
;
_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                84.9523(11)
_cell_angle_beta                 79.4490(11)
_cell_angle_gamma                63.9269(16)
_cell_formula_units_Z            1
_cell_length_a                   7.5689(2)
_cell_length_b                   7.8002(2)
_cell_length_c                   12.2351(5)
_cell_measurement_reflns_used    2841
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     637.84(4)
_computing_cell_refinement       'Denzo & Scalepak (Otwinowski, Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction        'Denzo & Scalepak (Otwinowski, Minor, 1997)'
_computing_molecular_graphics
;
ORTEP III (Burnett, Johnson, 1996) & DIAMOND v2.1 (Brandenburg, 1999)
;
_computing_publication_material
;
SHELXL-97 (Sheldrick, 1997) & PLATON99 (Spek, 1999)'
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 18.2
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
 181 frames, \f rotation 2.0\% per frame (120s per frame)
  19 frames, \w rotation 2.0\% per frame (120s per frame)
  54 frames, \w rotation 2.0\% per frame (120s per frame)
  30 frames, \w rotation 2.0\% per frame (120s per frame)
  28 frames, \w rotation 2.0\% per frame (120s per frame)
  21 frames, \w rotation 2.0\% per frame (120s per frame)
  46 frames, \w rotation 2.0\% per frame (120s per frame)
  15 frames, \w rotation 2.0\% per frame (120s per frame)
;
_diffrn_measurement_device       '\k-geometry diffractometr'
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'area detector \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  0.068
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4596
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    4.192
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'Scalepak (Otwinowski, Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flattened prism'
_exptl_crystal_F_000             292
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       0.010(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0511P)^2^+1.710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                2516
_reflns_number_total             2898
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic015572e_s1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_Hall     -P_1
_cod_database_code               4320623