The 'globule‒globule' hybrid dicarbaborane‒polyoxometallate salt, [C2B10H11CH2NHCH(CH3)2]4[W10O32][H2O]2[(CH3)2CO]4
Macías, Ramón; Kennedy, John D.; Thornton-Pett, Mark; Román, Pascual; CrystEngComm 5 (2003) 93–; doi:10.1039/b302341a

data_7204621
_publ_section_title
;
 The 'globule--globule' hybrid dicarbaborane--polyoxometallate salt,
 [C2B10H11CH2NHCH(CH3)2]4[W10O32][H2O]2[(CH3)2CO]4
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              93
_journal_paper_doi               10.1039/b302341a
_journal_volume                  5
_journal_year                    2003
_chemical_formula_sum            'C18 H54 B20 N2 O19 W5'
_chemical_formula_weight         1738.08
_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                97.1960(6)
_cell_angle_beta                 106.0270(6)
_cell_angle_gamma                107.9160(6)
_cell_formula_units_Z            2
_cell_length_a                   11.5428(2)
_cell_length_b                   12.4850(2)
_cell_length_c                   18.4962(3)
_cell_measurement_temperature    150(2)
_cell_volume                     2372.42(7)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WC (Thornton-Pett, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
Detector set at 30mm from sample with different 2theta offsets 
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_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  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37855
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    12.142
_exptl_absorpt_correction_T_max  0.5820
_exptl_absorpt_correction_T_min  0.2812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.725
_refine_diff_density_min         -3.111
_refine_diff_density_rms         0.286
_refine_ls_extinction_coef       0.00088(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         9270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+2.4226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0980
_reflns_number_gt                8544
_reflns_number_total             9270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302341a.txt
_cod_data_source_block           rm65-2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204621