Soft scorpionate coordination at alkali metals
Rajesekharan-Nair, Rajeev; Lutta, Samuel T.; Kennedy, Alan R.; Reglinski, John; Spicer, Mark D.; Acta Crystallographica Section C 70 (2014) 421–427; doi:10.1107/S2053229614005737

data_2019576
_publ_section_title
;
 Soft scorpionate coordination at alkali metals
;
_journal_coeditor_code           OV3047
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              421
_journal_page_last               427
_journal_paper_doi               10.1107/S2053229614005737
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[Na2 (C18 H28 B N6 S3)2 (C H4 O)4] , 0.3333C4 H10 O1 , 0.0833C1 H4 O1'
_chemical_formula_moiety
'(C40 H72 B2 N12 Na2 O4 S6), 0.3333(C4 H10 O1), 0.0833(C1 H4 O1)'
_chemical_formula_sum            'C41.3333 H75.3333 B2 N12 Na2 O4.42 S6'
_chemical_formula_weight         1072.43
_chemical_name_systematic
'Bis-\m-methanol-\k^4^<i>O</i>:<i>O</i>-bis{[hydrotris(3-isopropyl-2-sulfanylidene-2,3-dihydro-1<i>H</i>-1,3-imidazol-1-yl)borato-\k^3^<i>H</i>,<i>S</i>,<i>S</i>'](methanol-\k<i>O</i>)sodium(I)}--diethyl ether--methanol (1/0.3333/0.0833)'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.256(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   53.903(2)
_cell_length_b                   14.4391(4)
_cell_length_c                   22.9832(4)
_cell_measurement_reflns_used    11902
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.3034
_cell_measurement_theta_min      3.0084
_cell_volume                     17781.5(9)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Xcalibur E'
_diffrn_measurement_method       \w
_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  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_h_min       -66
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33618
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut fragment'
_exptl_crystal_F_000             6858
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.133
_refine_diff_density_min         -0.643
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1011
_refine_ls_number_reflns         17425
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0928P)^2^+46.3515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1762
_reflns_number_gt                12925
_reflns_number_total             17425
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ov3047sup1.cif
_cod_data_source_block           rajpri
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2019576
_cod_database_fobs_code          2019576