A Synthetic Route to a Molecular Galloxane Dihydroxide and Its Group 4 Heterobimetallic Compounds
Erandi Bernabé-Pablo; Vojtech Jancik; Mónica Moya-Cabrera; Inorganic Chemistry 52 (2013) 6944–6950; doi:10.1021/ic4010054

data_4335294
_publ_section_title
;
 A Synthetic Route to a Molecular Galloxane Dihydroxide and Its Group 4
 Heterobimetallic Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6944
_journal_page_last               6950
_journal_paper_doi               10.1021/ic4010054
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C46 H58 Cl2 Ga2 N4 O'
_chemical_formula_sum            'C46 H58 Cl2 Ga2 N4 O'
_chemical_formula_weight         893.30
_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                   20.539(3)
_cell_length_b                   47.199(5)
_cell_length_c                   9.343(2)
_cell_measurement_reflns_used    6858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.16
_cell_volume                     9057(3)
_computing_cell_refinement       'Bruker AXS SAINT (v 7.34A, Bruker 2006)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'Bruker AXS SAINT (v 7.34A, Bruker 2006)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (v 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       'omega scan'
_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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9363
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.345
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Sheldrick 2008'
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             3728
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.344
_exptl_crystal_size_min          0.226
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3594
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0178P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0553
_reflns_number_gt                3441
_reflns_number_total             3594
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4010054_si_001_2.cif
_cod_data_source_block           Compound3
_cod_database_code               4335294