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_2019575
_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 (C27 H22 B N6 S3)2 (C H4 O)4]'
_chemical_formula_moiety         'C58 H60 B2 N12 Na2 O4 S6'
_chemical_formula_sum            'C58 H60 B2 N12 Na2 O4 S6'
_chemical_formula_weight         1249.14
_chemical_name_systematic
Bis-\m-methanol-\k^4^<i>O</i>:<i>O</i>-bis{[hydrotris(3-phenyl-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)}
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.777(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6969(5)
_cell_length_b                   19.4915(6)
_cell_length_c                   13.2609(4)
_cell_measurement_reflns_used    8166
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.8227
_cell_measurement_theta_min      3.0920
_cell_volume                     3003.3(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.967
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18722
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.27
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'fragment from large block'
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6679
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0312P)^2^+1.0836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                5282
_reflns_number_total             6679
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ov3047sup1.cif
_cod_data_source_block           slligand
_cod_original_cell_volume        3003.27(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2019575
_cod_database_fobs_code          2019575