#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/86/2238653.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_2238653
loop_
_publ_author_name
'Elboulali, Adel'
'Akriche, Samah'
'Rzaigui, Mohamed'
_publ_section_title
;
 m-Xylylenediaminium diaquabis[dihydrogen
 diphosphato(2{-})]cobaltate(II) dihydrate
;
_journal_coeditor_code           LH5650
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m545
_journal_page_last               m546
_journal_paper_doi               10.1107/S160053681302535X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac
'(C8 H14 N2) [Co (H2 P2 O7)2 (H2 O)2] , 2H2 O'
_chemical_formula_moiety         'C8 H14 N2 , Co H8 O16 P4 , 2(H2 O)'
_chemical_formula_sum            'C8 H26 Co N2 O18 P4'
_chemical_formula_weight         621.12
_chemical_name_systematic
;
m-Xylylenediaminium
diaquabis[dihydrogen diphosphato(2-)]cobaltate(II)
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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.20(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.933(2)
_cell_length_b                   9.132(4)
_cell_length_c                   21.441(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      9
_cell_volume                     2292.0(11)
_computing_cell_refinement       'CAD-4 Express (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 Express (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1996)'
_computing_molecular_graphics
;
Ortep-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg & Putz,
2005)
;
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            7386
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.412
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         5609
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0354
_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/[σ²(Fo²)+(0.0412P)²+1.1740P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                4197
_reflns_number_total             5609
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh5650.cif
_cod_data_source_block           I
_cod_original_cell_volume        2291.8(11)
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               2238653
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
_atom_site_symmetry_multiplicity
Co Co1 0.2500 0.2500 0.5000 0.01705(6) Uani d S 1 2
P P1 0.02843(3) 0.22128(4) 0.571350(18) 0.01809(7) Uani d . 1 1
P P2 -0.02421(3) 0.29251(4) 0.435477(17) 0.01764(7) Uani d . 1 1
O O1 0.14860(8) 0.19560(13) 0.56463(5) 0.0244(2) Uani d . 1 1
O O2 0.01855(10) 0.34054(12) 0.62180(6) 0.0295(2) Uani d . 1 1
H H2O2 0.0510 0.4153 0.6137 0.044 Uiso calc R 1 1
O O3 -0.03555(9) 0.08962(12) 0.58755(6) 0.0272(2) Uani d . 1 1
O O4 -0.04173(9) 0.29279(16) 0.50765(6) 0.0343(3) Uani d . 1 1
O O5 0.10009(8) 0.30371(12) 0.43469(5) 0.02264(19) Uani d . 1 1
O O6 -0.10026(8) 0.41352(11) 0.40494(5) 0.0240(2) Uani d . 1 1
O O7 -0.07639(9) 0.14643(13) 0.40722(7) 0.0373(3) Uani d . 1 1
H H7 -0.0275 0.0822 0.4135 0.056 Uiso calc R 1 1
O O1W 0.25749(9) 0.47229(13) 0.52445(7) 0.0317(3) Uani d D 1 1
H H1W1 0.2077(14) 0.501(3) 0.5446(10) 0.050 Uiso d D 1 1
H H2W1 0.3230(10) 0.503(3) 0.5427(10) 0.050 Uiso d D 1 1
O O2W 0.31653(13) 0.3286(2) 0.17868(8) 0.0503(4) Uani d D 1 1
H H1W2 0.3666(14) 0.365(3) 0.1596(10) 0.050 Uiso d D 1 1
H H2W2 0.2488(10) 0.355(3) 0.1618(10) 0.050 Uiso d D 1 1
N N1 0.20006(11) 0.51928(16) 0.36481(7) 0.0286(3) Uani d . 1 1
H H1A 0.1506 0.5933 0.3594 0.043 Uiso calc R 1 1
H H1B 0.2686 0.5518 0.3836 0.043 Uiso calc R 1 1
H H1C 0.1768 0.4511 0.3891 0.043 Uiso calc R 1 1
C C1 0.09999(15) 0.3728(2) 0.27477(8) 0.0336(3) Uani d . 1 1
C C2 0.0986(2) 0.2211(3) 0.27536(10) 0.0499(5) Uani d . 1 1
H H2 0.1644 0.1696 0.2929 0.060 Uiso calc R 1 1
C C3 0.0000 0.1464(4) 0.2500 0.0578(9) Uani d S 1 2
H H3 0.0000 0.0446 0.2500 0.069 Uiso calc SR 1 2
C C4 0.0000 0.4479(3) 0.2500 0.0305(4) Uani d S 1 2
H H4 0.0000 0.5497 0.2500 0.037 Uiso calc SR 1 2
C C5 0.20697(16) 0.4554(3) 0.30225(10) 0.0477(5) Uani d . 1 1
H H5A 0.2719 0.3896 0.3070 0.057 Uiso calc R 1 1
H H5B 0.2186 0.5330 0.2733 0.057 Uiso calc R 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3050 0.6296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 4 8
4 2 10
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
O1 Co1 O1 7_556 . 180.0
O1 Co1 O1W 7_556 7_556 93.85(5)
O1 Co1 O1W . 7_556 86.15(5)
O1 Co1 O1W 7_556 . 86.15(5)
O1 Co1 O1W . . 93.85(5)
O1W Co1 O1W 7_556 . 180.00(8)
O1 Co1 O5 7_556 . 91.75(4)
O1 Co1 O5 . . 88.25(4)
O1W Co1 O5 7_556 . 94.01(5)
O1W Co1 O5 . . 85.99(5)
O1 Co1 O5 7_556 7_556 88.25(4)
O1 Co1 O5 . 7_556 91.75(4)
O1W Co1 O5 7_556 7_556 85.99(5)
O1W Co1 O5 . 7_556 94.01(5)
O5 Co1 O5 . 7_556 180.00(5)
O1 P1 O3 . . 116.07(7)
O1 P1 O2 . . 112.49(7)
O3 P1 O2 . . 106.82(7)
O1 P1 O4 . . 109.69(6)
O3 P1 O4 . . 108.66(7)
O2 P1 O4 . . 102.15(7)
O5 P2 O6 . . 117.67(6)
O5 P2 O7 . . 112.39(7)
O6 P2 O7 . . 107.56(7)
O5 P2 O4 . . 109.15(7)
O6 P2 O4 . . 103.86(7)
O7 P2 O4 . . 105.19(8)
P1 O1 Co1 . . 136.65(7)
P1 O2 H2O2 . . 109.5
P1 O4 P2 . . 132.91(7)
P2 O5 Co1 . . 134.09(7)
P2 O7 H7 . . 109.5
Co1 O1W H1W1 . . 115.7(17)
Co1 O1W H2W1 . . 114.9(17)
H1W1 O1W H2W1 . . 109.9(18)
H1W2 O2W H2W2 . . 112.3(18)
C5 N1 H1A . . 109.5
C5 N1 H1B . . 109.5
H1A N1 H1B . . 109.5
C5 N1 H1C . . 109.5
H1A N1 H1C . . 109.5
H1B N1 H1C . . 109.5
C2 C1 C4 . . 119.07(19)
C2 C1 C5 . . 120.64(19)
C4 C1 C5 . . 120.3(2)
C3 C2 C1 . . 120.2(2)
C3 C2 H2 . . 119.9
C1 C2 H2 . . 119.9
C2 C3 C2 2 . 120.6(3)
C2 C3 H3 2 . 119.7
C2 C3 H3 . . 119.7
C1 C4 C1 2 . 120.8(2)
C1 C4 H4 2 . 119.6
C1 C4 H4 . . 119.6
N1 C5 C1 . . 111.18(15)
N1 C5 H5A . . 109.4
C1 C5 H5A . . 109.4
N1 C5 H5B . . 109.4
C1 C5 H5B . . 109.4
H5A C5 H5B . . 108.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 O1 7_556 2.0695(11)
Co1 O1 . 2.0695(11)
Co1 O1W 7_556 2.0940(15)
Co1 O1W . 2.0940(14)
Co1 O5 . 2.1044(11)
Co1 O5 7_556 2.1044(11)
P1 O1 . 1.4873(10)
P1 O3 . 1.5007(12)
P1 O2 . 1.5554(12)
P1 O4 . 1.5965(12)
P2 O5 . 1.4901(10)
P2 O6 . 1.4975(11)
P2 O7 . 1.5452(13)
P2 O4 . 1.6012(13)
O2 H2O2 . 0.8200
O7 H7 . 0.8200
O1W H1W1 . 0.843(9)
O1W H2W1 . 0.849(9)
O2W H1W2 . 0.853(9)
O2W H2W2 . 0.855(9)
N1 C5 . 1.480(3)
N1 H1A . 0.8900
N1 H1B . 0.8900
N1 H1C . 0.8900
C1 C2 . 1.385(3)
C1 C4 . 1.389(2)
C1 C5 . 1.501(3)
C2 C3 . 1.377(3)
C2 H2 . 0.9300
C3 C2 2 1.377(3)
C3 H3 . 0.9300
C4 C1 2 1.389(2)
C4 H4 . 0.9300
C5 H5A . 0.9700
C5 H5B . 0.9700
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
O2 H2O2 O6 5_566 0.82 1.74 2.5574(18) 171.5
O7 H7 O3 5_556 0.82 1.74 2.5268(18) 159.6
O1W H1W1 O6 5_566 0.843(9) 1.988(10) 2.8289(17) 174(2)
O1W H2W1 O3 3 0.849(9) 1.944(10) 2.7891(17) 174(2)
O2W H1W2 O3 8 0.853(9) 2.151(12) 2.972(2) 162(2)
O2W H2W2 O6 2 0.855(9) 2.118(12) 2.946(2) 163(2)
N1 H1A O2 5_566 0.89 2.22 2.9694(18) 141.9
N1 H1A O2W 4 0.89 2.36 2.969(3) 125.9
N1 H1B O7 3 0.89 2.01 2.8893(18) 167.3
N1 H1C O5 . 0.89 1.99 2.8701(19) 170.8
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_site_symmetry_4
_geom_torsion
O3 P1 O1 Co1 . . 132.63(10)
O2 P1 O1 Co1 . . -103.92(11)
O4 P1 O1 Co1 . . 9.04(13)
O1 Co1 O1 P1 7_556 . 112.8(17)
O1W Co1 O1 P1 7_556 . -109.69(11)
O1W Co1 O1 P1 . . 70.31(11)
O5 Co1 O1 P1 . . -15.56(11)
O5 Co1 O1 P1 7_556 . 164.44(11)
O1 P1 O4 P2 . . 23.46(15)
O3 P1 O4 P2 . . -104.38(13)
O2 P1 O4 P2 . . 142.97(12)
O5 P2 O4 P1 . . -38.26(15)
O6 P2 O4 P1 . . -164.55(12)
O7 P2 O4 P1 . . 82.55(13)
O6 P2 O5 Co1 . . 142.47(8)
O7 P2 O5 Co1 . . -91.76(11)
O4 P2 O5 Co1 . . 24.54(12)
O1 Co1 O5 P2 7_556 . 175.43(10)
O1 Co1 O5 P2 . . -4.57(10)
O1W Co1 O5 P2 7_556 . 81.45(10)
O1W Co1 O5 P2 . . -98.55(10)
O5 Co1 O5 P2 7_556 . -4E1(10)
C4 C1 C2 C3 . . 1.9(3)
C5 C1 C2 C3 . . -179.98(16)
C1 C2 C3 C2 . 2 -0.95(14)
C2 C1 C4 C1 . 2 -0.93(14)
C5 C1 C4 C1 . 2 -179.09(18)
C2 C1 C5 N1 . . -104.4(2)
C4 C1 C5 N1 . . 73.8(2)
