Synthesis, Characterization, and Structures of Divalent Europium and Ytterbium N,N-Dimethylaminodiboranates
Scott R. Daly; Gregory S. Girolami; Inorganic Chemistry 49 (2010) 4578–4585; doi:10.1021/ic100292u

data_4315512
_publ_contact_author_address
;Department of Chemistry, Box 4-6
University of Illinois at Urbana-Champaign
600 South Mathews
Urbana, IL 61801
;
_publ_contact_author_email       girolami@scs.illinois.edu
_publ_contact_author_fax         '(217) 333-2685'
_publ_contact_author_name        'Gregory S. Girolami'
_publ_contact_author_phone       '(217) 333-2729'
_publ_section_title
;
 Synthesis, Characterization, and Structures of Divalent Europium and
 Ytterbium N,N-Dimethylaminodiboranates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4578
_journal_page_last               4585
_journal_paper_doi               10.1021/ic100292u
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C12 H44 B4 Eu N2 O4'
_chemical_formula_weight         475.69
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 103.552(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4304(11)
_cell_length_b                   14.3523(15)
_cell_length_c                   16.6107(18)
_cell_measurement_reflns_used    9781
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      1.90
_cell_volume                     2417.4(4)
_computing_cell_refinement       'Bruker APEX'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_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      193(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'psi and omega 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  0.0869
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33520
_diffrn_reflns_theta_full        27.13
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    2.608
_exptl_absorpt_correction_T_max  0.79196
_exptl_absorpt_correction_T_min  0.54414
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XPREP/SHELXTL
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.393
_exptl_crystal_size_mid          0.303
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         5347
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0227
_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^)+(0.0210P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0548
_reflns_number_gt                4417
_reflns_number_total             5347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100292u_si_001_2.cif
_cod_data_source_block           ba68i2m_face
_cod_database_code               4315512