Bis(hydrazin-1-ium) bis(μ~2~-pyridazine-3,6-dicarboxylato)bis(aqualithiate) octaaquabis(μ~3~-pyridazine-3,6-dicarboxylato)tetralithium
Starosta, Wojciech; Leciejewicz, Janusz; Acta Crystallographica Section E 68 (2012) m324–m325; doi:10.1107/S1600536812007192

data_2233913
_publ_section_title
;
 Bis(hydrazin-1-ium)
 bis(\m~2~-pyridazine-3,6-dicarboxylato)bis(aqualithiate)
 octaaquabis(\m~3~-pyridazine-3,6-dicarboxylato)tetralithium
;
_journal_coeditor_code           KP2385
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m324
_journal_page_last               m325
_journal_paper_doi               10.1107/S1600536812007192
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'(N2 H5)2 [Li2 (C6 H2 N2 O4)2 (H2 O)2] , [Li4 (C6 H2 N2 O4)2 (H2 O)8]'
_chemical_formula_moiety
'2(H5 N2 +), C12 H8 Li2 N4 O10 2-, C12 H20 Li4 N4 O16'
_chemical_formula_sum            'C24 H38 Li6 N12 O26'
_chemical_formula_weight         952.30
_chemical_name_systematic
;
Bis(hydrazin-1-ium) bis(\m~2~-pyridazine-3,6-dicarboxylato)bis(aqualithiate)
octaaquabis(\m~3~-pyridazine-3,6-dicarboxylato)tetralithium
;
_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           SHELXL97
_cell_angle_alpha                86.40(3)
_cell_angle_beta                 87.68(3)
_cell_angle_gamma                61.49(3)
_cell_formula_units_Z            1
_cell_length_a                   7.0999(14)
_cell_length_b                   7.2390(14)
_cell_length_c                   22.608(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      6
_cell_volume                     1019.0(5)
_computing_cell_refinement       'KM-4 Software (Kuma, 1996)'
_computing_data_collection       'KM-4 Software (Kuma, 1996)'
_computing_data_reduction        'DATAPROC (Kuma, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_device_type  'Kuma KM-4 four-circle'
_diffrn_measurement_method       'profile data from \w/2\q 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  0.0898
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            5515
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        5.81
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  0.9851
_exptl_absorpt_correction_T_min  0.9701
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.722
_exptl_crystal_size_mid          0.346
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.413
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0539
_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^)+(0.1491P)^2^+0.1309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.2038
_reflns_number_gt                3362
_reflns_number_total             5058
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp2385.cif
_cod_data_source_block           I
_cod_original_cell_volume        1018.9(3)
_cod_database_code               2233913
_cod_database_fobs_code          2233913