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_4335295
_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         'C25 H35 Ga N2'
_chemical_formula_sum            'C25 H35 Ga N2'
_chemical_formula_weight         433.27
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   13.966(2)
_cell_length_b                   17.174(2)
_cell_length_c                   19.935(3)
_cell_measurement_reflns_used    9023
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.14
_cell_volume                     4781.5(11)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26518
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.163
_exptl_absorpt_correction_T_max  0.625
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Sheldrick 2008'
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.472
_exptl_crystal_size_mid          0.430
_exptl_crystal_size_min          0.412
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         8405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0234P)^2^+6.9671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                7139
_reflns_number_total             8405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4010054_si_001_3.cif
_cod_data_source_block           Compound5
_cod_database_code               4335295