Bis(ethylenediammonium) diaquabis[hydrogendiphosphato(3–)]nickelate(II): structure and vibrational spectroscopy
Essehli, Rachid; El Bali, Brahim; Lachkar, Mohammed; Svoboda, Ingrid; Fuess, Hartmut; Acta Crystallographica Section E 62 (2006) m538–m541; doi:10.1107/S1600536806004399

data_2208388
_publ_section_title
;
 Bis(ethylenediammonium)
 diaquabis[hydrogendiphosphato(3--)]nickelate(II): structure and
 vibrational spectroscopy
;
_journal_coeditor_code           NC6053
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m538
_journal_page_last               m541
_journal_paper_doi               10.1107/S1600536806004399
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C2 H10 N2)2 [Ni (H P 2O7)2 (H2 O)2]'
_chemical_formula_moiety         '2C2 H10 N2 2+ , H6 Ni O16 P4 4-'
_chemical_formula_structural     '(C2 H10 N2)2 [Ni (H P 2O7)2 (H2 O)2]'
_chemical_formula_sum            'C4 H26 N4 Ni O16 P4'
_chemical_formula_weight         568.88
_chemical_name_systematic
;
bis(ethylenediammonium) diaquabis[hydrogendiphosphato(3-)]nickel(II)
;
_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                103.876(9)
_cell_angle_beta                 111.1900(10)
_cell_angle_gamma                97.711(8)
_cell_formula_units_Z            1
_cell_length_a                   7.4898(9)
_cell_length_b                   7.5517(7)
_cell_length_c                   9.77800(10)
_cell_measurement_reflns_used    1929
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      29.183
_cell_measurement_theta_min      2.970
_cell_volume                     485.48(8)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2002)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type
;
Oxford Xcalibur diffractometer with Sapphire CCD area detector
;
_diffrn_measurement_method       'Rotation method data acquisition using \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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3240
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.12
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.415
_exptl_absorpt_correction_T_max  0.9199
_exptl_absorpt_correction_T_min  0.7847
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2002)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.946
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             294
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.722
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1930
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0576P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0888
_reflns_number_gt                1662
_reflns_number_total             1930
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            nc6053.cif
_cod_data_source_block           I
_cod_original_cell_volume        485.48(9)
_cod_database_code               2208388
_cod_database_fobs_code          2208388