Crystal structure of di-μ-aqua-μ-(pyrazine <i>N</i>,<i>N</i>'-dioxide)-κ^2^<i>O</i>:<i>O</i>-bis(diaquasodium) tetraphenylborate dihydrate pyrazine <i>N</i>,<i>N</i>'-dioxide monosolvate
Boron, Elaine P.; Carter, Kelsey K.; Knaust, Jacqueline M.; Acta Crystallographica Section E 71 (2015) 1467–1470; doi:10.1107/S205698901502071X

data_2241278
_publ_section_title
;
 Crystal structure of di-\m-aqua-\m-(pyrazine
 <i>N</i>,<i>N</i>'-dioxide)-\k^2^<i>O</i>:<i>O</i>-bis(diaquasodium)
 tetraphenylborate dihydrate pyrazine <i>N</i>,<i>N</i>'-dioxide
 monosolvate
;
_journal_coeditor_code           WM5232
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1467
_journal_page_last               1470
_journal_paper_doi               10.1107/S205698901502071X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac
'[Na2 (C4 H4 N2 O2) (H2 O1)6]  (B C24 H20)2, C4 H4 N2 O2, 2H2 O'
_chemical_formula_moiety
'C4 H16 N2 Na2 O8 2+, 2(B C24 H20 -), C4 H4 N2 O2, 2(H2 O)'
_chemical_formula_sum            'C56 H64 B2 N4 Na2 O12'
_chemical_formula_weight         1052.71
_chemical_name_systematic
;Di-\m-aqua-\m-(pyrazine
<i>N</i>,<i>N</i>'-dioxide)-\k^2^<i>O</i>:<i>O</i>-bis(diaquasodium)
tetraphenylborate pyrazine <i>N</i>,<i>N</i>'-dioxide monosolvate dihydrate
;
_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           'form.cif (version 2.0)'
_cell_angle_alpha                90.00
_cell_angle_beta                 102.9470(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.4224(9)
_cell_length_b                   10.1950(4)
_cell_length_c                   27.2349(11)
_cell_measurement_reflns_used    14931
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      30.513
_cell_measurement_theta_min      2.244
_cell_volume                     5526.3(4)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
SMART (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
XSEED (Barbour, 2001)
;
_computing_publication_material
;
XSEED (Barbour, 2001)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      99(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\w 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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            32437
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.894364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2001)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         8464
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0739P)^2^+3.1014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1395
_reflns_number_gt                6996
_reflns_number_total             8464
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm5232sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2241278
_cod_database_fobs_code          2241278