#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/37/2223749.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_2223749
loop_
_publ_author_name
'Selmi, Ahmed'
'Akriche, Samah'
'Rzaigui, Mohamed'
_publ_section_title
;
 Bis(2-methylanilinium)
 diaquabis[dihydrogendiphosphato(2{-})]cobaltate(II)
;
_journal_coeditor_code           FL2278
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1487
_journal_paper_doi               10.1107/S1600536809044079
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '(C7 H10 N)2 [Co (H2 P2 O7)2 (H2 O)2]'
_chemical_formula_moiety         '2(C7 H10 N +), H8 Co O16 P4 2-'
_chemical_formula_sum            'C14 H28 Co N2 O16 P4'
_chemical_formula_weight         663.19
_chemical_name_systematic
;
Bis(2-methylanilinium) diaquabis[dihydrogendiphosphato(2-)]cobaltate(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           SHELXL-97
_cell_angle_alpha                91.92(3)
_cell_angle_beta                 94.09(5)
_cell_angle_gamma                104.67(2)
_cell_formula_units_Z            1
_cell_length_a                   7.440(4)
_cell_length_b                   7.455(2)
_cell_length_c                   11.747(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11
_cell_measurement_theta_min      9
_cell_volume                     627.8(4)
_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, 1997) and DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'WinGX  (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_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 CAD-4'
_diffrn_measurement_method       'Non-profiled ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Agk\a
_diffrn_radiation_wavelength     0.56085
_diffrn_reflns_av_R_equivalents  0.0083
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4678
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        7
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             341
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4486
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0277
_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)+(0.0409P)²+0.209P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                3911
_reflns_number_total             4486
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fl2278.cif
_cod_data_source_block           I
_cod_database_code               2223749
_cod_database_fobs_code          2223749
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.5000 0.5000 0.5000 0.01548(6) Uani d S 1 . .
P P1 0.21765(4) 0.73669(4) 0.39318(3) 0.01617(7) Uani d . 1 . .
P P2 0.27309(4) 0.74457(4) 0.64170(3) 0.01643(7) Uani d . 1 . .
O O1 0.37007(14) 0.64107(14) 0.38682(8) 0.02204(18) Uani d . 1 . .
O O2 0.29044(15) 0.94783(14) 0.37491(11) 0.0272(2) Uani d . 1 . .
H H2 0.4017 0.9718 0.3647 0.041 Uiso calc R 1 . .
O O3 0.04241(14) 0.65899(15) 0.31845(9) 0.0253(2) Uani d . 1 . .
O O4 0.15097(14) 0.73056(16) 0.52080(9) 0.02389(19) Uani d . 1 . .
O O5 0.39173(14) 0.61111(14) 0.63563(8) 0.02138(18) Uani d . 1 . .
O O6 0.11785(15) 0.68728(15) 0.72493(9) 0.0258(2) Uani d . 1 . .
H H6 0.0630 0.5776 0.7116 0.039 Uiso calc R 1 . .
O O7 0.37403(15) 0.94287(14) 0.67018(10) 0.0275(2) Uani d . 1 . .
O O8 0.25633(15) 0.27064(15) 0.49415(11) 0.0291(2) Uani d D 1 . .
N N1 0.29299(18) 0.25923(18) 0.76160(10) 0.0234(2) Uani d . 1 . .
H H1A 0.3161 0.1554 0.7340 0.035 Uiso calc R 1 . .
H H1B 0.3821 0.3566 0.7445 0.035 Uiso calc R 1 . .
H H1C 0.1832 0.2687 0.7308 0.035 Uiso calc R 1 . .
C C1 0.2890(2) 0.2541(2) 0.88612(12) 0.0242(3) Uani d . 1 . .
C C2 0.4492(2) 0.2523(2) 0.95316(14) 0.0313(3) Uani d . 1 . .
C C3 0.4354(3) 0.2471(3) 1.07075(16) 0.0469(5) Uani d . 1 . .
H H3 0.5407 0.2471 1.1184 0.056 Uiso calc R 1 . .
C C4 0.2716(4) 0.2419(4) 1.11818(16) 0.0550(6) Uani d . 1 . .
H H4 0.2668 0.2390 1.1970 0.066 Uiso calc R 1 . .
C C5 0.1146(3) 0.2411(4) 1.04945(18) 0.0579(6) Uani d . 1 . .
H H5 0.0026 0.2356 1.0815 0.069 Uiso calc R 1 . .
C C6 0.1229(3) 0.2486(3) 0.93204(15) 0.0439(5) Uani d . 1 . .
H H6A 0.0173 0.2499 0.8849 0.053 Uiso calc R 1 . .
C C7 0.6297(3) 0.2562(4) 0.90335(19) 0.0530(6) Uani d . 1 . .
H H7A 0.6174 0.1429 0.8587 0.079 Uiso calc R 1 . .
H H7B 0.7264 0.2685 0.9639 0.079 Uiso calc R 1 . .
H H7C 0.6609 0.3596 0.8555 0.079 Uiso calc R 1 . .
H H2W 0.266(3) 0.174(2) 0.458(2) 0.052(7) Uiso d D 1 . .
H H1W 0.149(2) 0.287(4) 0.481(2) 0.070(9) Uiso d D 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'
Co Co 0.3050 0.6296 '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'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-1 -3 -5
3 -2 -5
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
_geom_angle_publ_flag
O1 Co1 O1 . 2_666 180.00(4) ?
O1 Co1 O5 . . 90.50(5) ?
O1 Co1 O5 2_666 . 89.50(5) ?
O1 Co1 O5 . 2_666 89.50(5) ?
O1 Co1 O5 2_666 2_666 90.50(5) ?
O5 Co1 O5 . 2_666 180.00(3) ?
O1 Co1 O8 . . 91.82(6) ?
O1 Co1 O8 2_666 . 88.18(6) ?
O5 Co1 O8 . . 86.64(6) ?
O5 Co1 O8 2_666 . 93.36(6) ?
O1 Co1 O8 . 2_666 88.18(6) ?
O1 Co1 O8 2_666 2_666 91.82(6) ?
O5 Co1 O8 . 2_666 93.36(6) ?
O5 Co1 O8 2_666 2_666 86.64(6) ?
O8 Co1 O8 . 2_666 180.0 ?
O1 P1 O3 . . 117.53(7) ?
O1 P1 O2 . . 110.90(7) ?
O3 P1 O2 . . 109.47(7) ?
O1 P1 O4 . . 109.65(7) ?
O3 P1 O4 . . 104.33(7) ?
O2 P1 O4 . . 103.91(7) ?
O5 P2 O7 . . 115.99(7) ?
O5 P2 O6 . . 112.76(7) ?
O7 P2 O6 . . 108.25(7) ?
O5 P2 O4 . . 108.51(6) ?
O7 P2 O4 . . 108.93(7) ?
O6 P2 O4 . . 101.36(7) ?
P1 O1 Co1 . . 134.55(7) ?
P1 O2 H2 . . 109.5 ?
P1 O4 P2 . . 129.26(7) ?
P2 O5 Co1 . . 132.40(6) ?
P2 O6 H6 . . 109.5 ?
Co1 O8 H2W . . 114.2(17) ?
Co1 O8 H1W . . 121(2) ?
H2W O8 H1W . . 111(2) ?
C1 N1 H1A . . 109.5 ?
C1 N1 H1B . . 109.5 ?
H1A N1 H1B . . 109.5 ?
C1 N1 H1C . . 109.5 ?
H1A N1 H1C . . 109.5 ?
H1B N1 H1C . . 109.5 ?
C6 C1 C2 . . 122.21(15) ?
C6 C1 N1 . . 118.02(14) ?
C2 C1 N1 . . 119.77(14) ?
C1 C2 C3 . . 116.73(17) ?
C1 C2 C7 . . 122.34(15) ?
C3 C2 C7 . . 120.94(17) ?
C4 C3 C2 . . 122.00(18) ?
C4 C3 H3 . . 119.0 ?
C2 C3 H3 . . 119.0 ?
C3 C4 C5 . . 119.95(18) ?
C3 C4 H4 . . 120.0 ?
C5 C4 H4 . . 120.0 ?
C4 C5 C6 . . 119.9(2) ?
C4 C5 H5 . . 120.1 ?
C6 C5 H5 . . 120.1 ?
C1 C6 C5 . . 119.22(18) ?
C1 C6 H6A . . 120.4 ?
C5 C6 H6A . . 120.4 ?
C2 C7 H7A . . 109.5 ?
C2 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
C2 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
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
Co1 O1 . 2.0574(12) ?
Co1 O1 2_666 2.0574(12) ?
Co1 O5 . 2.0752(12) ?
Co1 O5 2_666 2.0752(12) ?
Co1 O8 . 2.1491(14) ?
Co1 O8 2_666 2.1491(14) ?
P1 O1 . 1.4892(11) ?
P1 O3 . 1.4919(14) ?
P1 O2 . 1.5570(11) ?
P1 O4 . 1.6108(12) ?
P2 O5 . 1.4909(11) ?
P2 O7 . 1.4933(12) ?
P2 O6 . 1.5529(13) ?
P2 O4 . 1.6160(13) ?
O2 H2 . 0.8200 ?
O6 H6 . 0.8200 ?
O8 H2W . 0.842(9) ?
O8 H1W . 0.842(9) ?
N1 C1 . 1.4667(18) ?
N1 H1A . 0.8900 ?
N1 H1B . 0.8900 ?
N1 H1C . 0.8900 ?
C1 C6 . 1.375(2) ?
C1 C2 . 1.384(2) ?
C2 C3 . 1.394(2) ?
C2 C7 . 1.496(3) ?
C3 C4 . 1.368(3) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.371(3) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.387(3) ?
C5 H5 . 0.9300 ?
C6 H6A . 0.9300 ?
C7 H7A . 0.9600 ?
C7 H7B . 0.9600 ?
C7 H7C . 0.9600 ?
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
O6 H6 O3 2_566 0.82 1.75 2.5712(17) 176.8
O2 H2 O7 2_676 0.82 1.71 2.522(2) 169.0
O8 H2W O2 1_545 0.842(9) 1.978(10) 2.8199(18) 179(3)
O8 H1W O4 2_566 0.842(9) 2.202(13) 3.020(2) 164(3)
N1 H1A O7 1_545 0.89 1.89 2.7788(18) 176.9
N1 H1B O5 . 0.89 2.31 3.0083(19) 135.0
N1 H1B O1 2_666 0.89 2.48 3.105(2) 127.3
N1 H1C O3 2_566 0.89 1.94 2.821(2) 167.7
