#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/83/2208388.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2208388
loop_
_publ_author_name
'Essehli, Rachid'
'El Bali, Brahim'
'Lachkar, Mohammed'
'Svoboda, Ingrid'
'Fuess, Hartmut'
_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 ω'
_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/[σ²(Fo²)+(0.0576P)²] where P = (Fo²+2Fc²)/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>2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Ni Ni1 1.0000 1.0000 0.0000 0.01252(15) Uani d S 1
P P1 1.22608(10) 0.71164(9) -0.14428(8) 0.01438(18) Uani d . 1
P P2 1.29920(9) 0.77543(9) 0.18040(7) 0.01297(17) Uani d . 1
O O1 1.0799(3) 0.8340(2) -0.1601(2) 0.0172(4) Uani d . 1
O O2 1.3634(3) 0.7589(3) 0.0369(2) 0.0185(4) Uani d . 1
O O3 1.1686(3) 0.9143(2) 0.17600(19) 0.0167(4) Uani d . 1
O O4 1.1143(3) 0.4999(3) -0.2013(2) 0.0242(5) Uani d . 1
O O5 1.3646(3) 0.7375(3) -0.2194(2) 0.0249(5) Uani d . 1
O O6 1.4931(3) 0.8490(3) 0.3223(2) 0.0204(4) Uani d . 1
O O7 1.1921(3) 0.5790(3) 0.1580(2) 0.0240(5) Uani d . 1
H H7 1.1009 0.5848 0.1852 0.029 Uiso calc R 1
O O8 1.2352(3) 1.2237(3) 0.0447(2) 0.0210(4) Uani d D 1
H H8A 1.219(4) 1.334(2) 0.068(3) 0.025 Uiso d D 1
H H8B 1.3578(18) 1.232(4) 0.092(3) 0.025 Uiso d D 1
N N1 0.8384(3) 0.8787(3) 0.2869(2) 0.0168(5) Uani d . 1
H H1A 0.8695 0.9718 0.2521 0.020 Uiso calc R 1
H H1C 0.7220 0.8776 0.2921 0.020 Uiso calc R 1
H H1B 0.8314 0.7695 0.2229 0.020 Uiso calc R 1
N N4 0.5620(3) 0.7615(3) 0.5911(2) 0.0196(5) Uani d . 1
H H4A 0.6775 0.8459 0.6437 0.024 Uiso calc R 1
H H4B 0.4951 0.7630 0.6501 0.024 Uiso calc R 1
H H4C 0.4928 0.7895 0.5071 0.024 Uiso calc R 1
C C2 0.9937(4) 0.9076(4) 0.4447(3) 0.0261(7) Uani d . 1
H H2A 1.1205 0.9081 0.4392 0.031 Uiso calc R 1
H H2B 0.9615 0.8049 0.4820 0.031 Uiso calc R 1
C C3 0.5962(4) 0.5730(4) 0.5451(3) 0.0256(6) Uani d . 1
H H3A 0.6726 0.5429 0.6366 0.031 Uiso calc R 1
H H3B 0.6716 0.5721 0.4827 0.031 Uiso calc R 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O3 Ni1 O3 . 2_775 180.0
O3 Ni1 O1 . 2_775 86.68(7)
O3 Ni1 O1 2_775 2_775 93.32(7)
O3 Ni1 O1 . . 93.32(7)
O3 Ni1 O1 2_775 . 86.68(7)
O1 Ni1 O1 2_775 . 180.00(8)
O3 Ni1 O8 . 2_775 87.67(8)
O3 Ni1 O8 2_775 2_775 92.33(8)
O1 Ni1 O8 2_775 2_775 88.94(7)
O1 Ni1 O8 . 2_775 91.06(7)
O3 Ni1 O8 . . 92.33(8)
O3 Ni1 O8 2_775 . 87.67(8)
O1 Ni1 O8 2_775 . 91.06(7)
O1 Ni1 O8 . . 88.94(7)
O8 Ni1 O8 2_775 . 180.0000(10)
O5 P1 O1 . . 116.41(11)
O5 P1 O4 . . 109.98(11)
O1 P1 O4 . . 109.98(11)
O5 P1 O2 . . 105.77(10)
O1 P1 O2 . . 108.27(10)
O4 P1 O2 . . 105.81(11)
O7 P2 O6 . . 113.18(11)
O7 P2 O3 . . 112.79(11)
O6 P2 O3 . . 111.81(10)
O7 P2 O2 . . 106.21(11)
O6 P2 O2 . . 104.25(10)
O3 P2 O2 . . 107.93(10)
P1 O1 Ni1 . . 132.24(11)
P1 O2 P2 . . 129.18(12)
P2 O3 Ni1 . . 131.55(10)
P2 O7 H7 . . 109.5
Ni1 O8 H8A . . 117.5(18)
Ni1 O8 H8B . . 126.7(19)
H8A O8 H8B . . 106.3(15)
C2 N1 H1A . . 109.5
C2 N1 H1C . . 109.5
H1A N1 H1C . . 109.5
C2 N1 H1B . . 109.5
H1A N1 H1B . . 109.5
H1C N1 H1B . . 109.5
C3 N4 H4A . . 109.5
C3 N4 H4B . . 109.5
H4A N4 H4B . . 109.5
C3 N4 H4C . . 109.5
H4A N4 H4C . . 109.5
H4B N4 H4C . . 109.5
N1 C2 C2 . 2_776 110.1(3)
N1 C2 H2A . . 109.6
C2 C2 H2A 2_776 . 109.6
N1 C2 H2B . . 109.6
C2 C2 H2B 2_776 . 109.6
H2A C2 H2B . . 108.2
N4 C3 C3 . 2_666 110.8(3)
N4 C3 H3A . . 109.5
C3 C3 H3A 2_666 . 109.5
N4 C3 H3B . . 109.5
C3 C3 H3B 2_666 . 109.5
H3A C3 H3B . . 108.1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 O3 . 2.0389(17) yes
Ni1 O3 2_775 2.0389(17) yes
Ni1 O1 2_775 2.0780(17) yes
Ni1 O1 . 2.0780(17) yes
Ni1 O8 2_775 2.1070(18) yes
Ni1 O8 . 2.1070(18) yes
P1 O5 . 1.4901(19) yes
P1 O1 . 1.5144(19) yes
P1 O4 . 1.5632(19) yes
P1 O2 . 1.6141(19) yes
P2 O7 . 1.5134(19) yes
P2 O6 . 1.5163(19) yes
P2 O3 . 1.5248(18) yes
P2 O2 . 1.6230(18) yes
O7 H7 . 0.8200 yes
O8 H8A . 0.848(10) yes
O8 H8B . 0.851(10) yes
N1 C2 . 1.502(4) yes
N1 H1A . 0.8900 yes
N1 H1C . 0.8900 yes
N1 H1B . 0.8900 yes
N4 C3 . 1.472(3) yes
N4 H4A . 0.8900 yes
N4 H4B . 0.8900 yes
N4 H4C . 0.8900 yes
C2 C2 2_776 1.515(5) yes
C2 H2A . 0.9700 yes
C2 H2B . 0.9700 yes
C3 C3 2_666 1.503(5) yes
C3 H3A . 0.9700 yes
C3 H3B . 0.9700 yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O7 H7 O4 2_765 0.82 1.73 2.501(3) 156
O8 H8A O7 1_565 0.848(10) 1.918(12) 2.756(3) 169(3)
O8 H8B O5 2_875 0.851(10) 1.947(11) 2.795(3) 174(3)
N1 H1A O1 2_775 0.89 1.96 2.846(3) 175
N1 H1C O6 1_455 0.89 1.84 2.718(3) 170
N1 H1B O4 2_765 0.89 2.10 2.888(3) 147
N4 H4A O3 2_776 0.89 2.04 2.816(3) 145
N4 H4B O5 1_456 0.89 1.89 2.779(3) 172
N4 H4C O6 1_455 0.89 1.96 2.748(3) 146
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
O5 P1 O1 Ni1 . -131.40(14)
O4 P1 O1 Ni1 . 102.69(15)
O2 P1 O1 Ni1 . -12.48(17)
O3 Ni1 O1 P1 . -5.38(15)
O3 Ni1 O1 P1 2_775 174.62(15)
O1 Ni1 O1 P1 2_775 9E1(10)
O8 Ni1 O1 P1 2_775 -93.10(15)
O8 Ni1 O1 P1 . 86.90(15)
O5 P1 O2 P2 . 173.42(14)
O1 P1 O2 P2 . 47.97(18)
O4 P1 O2 P2 . -69.90(17)
O7 P2 O2 P1 . 67.87(18)
O6 P2 O2 P1 . -172.34(15)
O3 P2 O2 P1 . -53.33(18)
O7 P2 O3 Ni1 . -93.67(16)
O6 P2 O3 Ni1 . 137.43(13)
O2 P2 O3 Ni1 . 23.35(17)
O3 Ni1 O3 P2 2_775 -13E1(10)
O1 Ni1 O3 P2 2_775 178.89(15)
O1 Ni1 O3 P2 . -1.11(15)
O8 Ni1 O3 P2 2_775 89.82(15)
O8 Ni1 O3 P2 . -90.18(15)
