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_4335297
_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         'C54 H78 Ga2 Hf N6 O3, 0.5 (C7 H8)'
_chemical_formula_sum            'C57.5 H82 Ga2 Hf N6 O3'
_chemical_formula_weight         1223.22
_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                95.800(1)
_cell_angle_beta                 90.452(1)
_cell_angle_gamma                112.275(1)
_cell_formula_units_Z            2
_cell_length_a                   10.4382(3)
_cell_length_b                   13.4996(4)
_cell_length_c                   21.7611(7)
_cell_measurement_reflns_used    9348
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.35
_cell_volume                     2819.48(15)
_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      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            85263
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         0.94
_exptl_absorpt_coefficient_mu    2.832
_exptl_absorpt_correction_T_max  0.8575
_exptl_absorpt_correction_T_min  0.4959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2, Sheldrick'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       plate
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         9973
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0174
_refine_ls_R_factor_gt           0.0162
_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^)+(0.0196P)^2^+2.3293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0404
_refine_ls_wR_factor_ref         0.0410
_reflns_number_gt                9527
_reflns_number_total             9973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4010054_si_001_5.cif
_cod_data_source_block           Compound8
_cod_original_formula_sum        'C57.50 H82 Ga2 Hf N6 O3'
_cod_database_code               4335297