A novel heterocyclic compound: <i>catena</i>-poly[[[diaquasodium(I)]-di-μ-aqua] hemi(1,5-dihydroxy-4,8,9-trioxa-2,6-diazabicyclo[3.3.1]nona-2,6-diene-3,7-diolate)]
Fang, Rui-Qin; Xiao, Zhu-Ping; Cao, Ping; Shi, Da-Hua; Zhu, Hai-Liang; Acta Crystallographica Section C 63 (2007) m193–m194; doi:10.1107/S0108270107001977

data_2015946
_publ_section_title
;A novel heterocyclic compound:
 <i>catena</i>-poly[[[diaquasodium(I)]-di-\m-aqua]
 hemi(1,5-dihydroxy-4,8,9-trioxa-2,6-diazabicyclo[3.3.1]nona-2,6-diene-3,7-diolate)]
;
_journal_coeditor_code           GD3082
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m193
_journal_page_last               m194
_journal_paper_doi               10.1107/S0108270107001977
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Na (H2 O1)4]2 (C4 H2 N2 O7)'
_chemical_formula_moiety         '2(H8 Na O4 +), C4 H2 N2 O7 2-'
_chemical_formula_sum            'C4 H18 N2 Na2 O15'
_chemical_formula_weight         380.18
_chemical_name_systematic
;
bis(tetraaquasodium)
1,5-dihydroxy-4,8,9-trioxa-2,6-diazabicyclo[3.3.1]nona-2,6-diene-3,7-diolate
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.634(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.935(7)
_cell_length_b                   10.709(6)
_cell_length_c                   12.277(7)
_cell_measurement_reflns_used    986
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.32
_cell_measurement_theta_min      2.80
_cell_volume                     1503.5(15)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3719
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.9620
_exptl_absorpt_correction_T_min  0.9318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.812
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1333
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0659
_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^)+(0.1475P)^2^+3.8784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2174
_refine_ls_wR_factor_ref         0.2246
_reflns_number_gt                1146
_reflns_number_total             1333
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3082.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_hydrogen_treatment' value 'refu' changed to 'refU' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'refu' changed to 'refU'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1503.5(16)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2015946
_cod_database_fobs_code          2015946