Synthesis and Structural Characterization of an Unprecedented Nonmetal Cation Polyborate Salt Containing Two Different "Isolated" Polyborate Anions: [H2en]2[B4O5(OH)4][B7O9(OH)5].3H2O (en = H2NCH2CH2NH2)
Michael A. Beckett; Peter N. Horton; Simon J. Coles; David W. Martin; Inorganic Chemistry 50 (2011) 12215–12218; doi:10.1021/ic202144f

data_4327050
_publ_section_title
;
 Synthesis and Structural Characterization of an Unprecedented Nonmetal
 Cation Polyborate Salt Containing Two Different "Isolated" Polyborate
 Anions: [H2en]2[B4O5(OH)4][B7O9(OH)5].3H2O (en = H2NCH2CH2NH2)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12215
_journal_page_last               12218
_journal_paper_doi               10.1021/ic202144f
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C4 H35 B11 N4 O26'
_chemical_formula_weight         674.27
_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                80.415(5)
_cell_angle_beta                 84.057(5)
_cell_angle_gamma                86.438(6)
_cell_formula_units_Z            2
_cell_length_a                   8.3270(7)
_cell_length_b                   8.6970(9)
_cell_length_c                   19.164(2)
_cell_measurement_reflns_used    3676
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     1359.7(2)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16004
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.9984
_exptl_absorpt_correction_T_min  0.9845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       Plate
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.215
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         4734
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1334
_refine_ls_R_factor_gt           0.0896
_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^)+(0.0293P)^2^+7.5191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.1976
_reflns_number_gt                3306
_reflns_number_total             4734
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic202144f_si_001.cif
_cod_data_source_block           2011src0323
_cod_database_code               4327050