#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/69/2226938.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_2226938
loop_
_publ_author_name
'Van der Merwe, Kina'
'Visser, Hendrik G.'
'Venter, J. A.'
_publ_section_title
;
 Pyridinium
 diaquabis(methylenediphosphonato-κ²O,O')chromate(III)
 tetrahydrate
;
_journal_coeditor_code           HY2333
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1011
_journal_page_last               m1012
_journal_paper_doi               10.1107/S1600536810028990
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C5 H6 N) [Cr (C H4 O6 P2)2 (H2 O)2], 4H2 O'
_chemical_formula_moiety         'C5 H6 N +, C2 H12 Cr O14 P4 -, 4(H2 O)'
_chemical_formula_sum            'C7 H26 Cr N O18 P4'
_chemical_formula_weight         588.17
_chemical_name_systematic
;
Pyridinium
diaquabis(methylenediphosphonato-κ²O,O')chromate(III)
tetrahydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                107.085(5)
_cell_angle_beta                 106.128(5)
_cell_angle_gamma                94.496(5)
_cell_formula_units_Z            1
_cell_length_a                   7.206(5)
_cell_length_b                   7.485(5)
_cell_length_c                   10.984(5)
_cell_measurement_reflns_used    6300
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.931
_cell_measurement_theta_min      0.843
_cell_volume                     535.7(6)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8784
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; (Bruker, 2001)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             303
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.623
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2632
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      3.952
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0240
_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/[σ²(Fo²)+(0.0342P)²+0.4874P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                2483
_reflns_number_total             2632
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2333.cif
_cod_data_source_block           I
_cod_database_code               2226938
_cod_database_fobs_code          2226938
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
Cr Cr1 0.5000 0.5000 0.5000 0.0082(3) Uani d S 1 . .
P P2 0.2173(2) 0.79359(19) 0.41325(14) 0.0086(4) Uani d D 1 . .
P P1 0.29362(19) 0.7622(2) 0.69142(14) 0.0085(4) Uani d . 1 . .
O O2 0.4491(6) 0.6457(6) 0.6635(4) 0.0110(8) Uani d D 1 . .
O O5 -0.0069(6) 0.7069(6) 0.3539(4) 0.0128(8) Uani d D 1 . .
O O3 0.3700(6) 0.8943(6) 0.8418(4) 0.0134(8) Uani d D 1 . .
H H3 0.4774 0.9569 0.8570 0.020 Uiso calc RD 1 . .
O O7 0.3373(6) 0.6353(6) 0.3947(4) 0.0113(8) Uani d . 1 . .
O O9 -0.0373(8) 0.7358(7) 0.8942(5) 0.0235(10) Uani d D 1 . .
O O1 0.7325(6) 0.6953(6) 0.5401(4) 0.0121(8) Uani d D 1 . .
C C1 0.2683(8) 0.9145(8) 0.5903(6) 0.0108(10) Uani d . 1 . .
H H4 0.3885 1.0063 0.6226 0.013 Uiso calc R 1 . .
H H5 0.1633 0.9841 0.6027 0.013 Uiso calc R 1 . .
O O4 0.0957(6) 0.6494(6) 0.6673(4) 0.0118(8) Uani d . 1 . .
O O8 0.2601(7) 0.9720(7) 1.1133(5) 0.0198(10) Uani d D 1 . .
N N1 0.381(7) 0.479(8) 0.070(5) 0.028(12) Uani d P 0.50 A 1
H H1 0.3025 0.4691 0.1145 0.034 Uiso calc PR 0.50 A 1
C C4 0.381(8) 0.466(10) 0.078(5) 0.024(10) Uani d PD 0.50 A 2
H H4A 0.3051 0.4405 0.1294 0.029 Uiso calc PR 0.50 A 2
C C3 0.5612(13) 0.5896(11) 0.1367(8) 0.0312(17) Uani d D 1 . .
H H3A 0.6025 0.6454 0.2295 0.037 Uiso calc R 1 A 1
C C2 0.3206(12) 0.3837(11) -0.0627(8) 0.0322(17) Uani d D 1 . .
H H2 0.2008 0.3014 -0.1034 0.039 Uiso calc R 1 A 1
O O6 0.2543(6) 0.9385(6) 0.3492(4) 0.0133(8) Uani d D 1 . .
H H8 0.193(16) 0.882(13) 1.042(9) 0.06(3) Uiso d D 1 . .
H H7 0.262(14) 0.950(13) 1.184(7) 0.03(2) Uiso d D 1 . .
H H1B 0.844(10) 0.677(12) 0.577(8) 0.03(2) Uiso d D 1 . .
H H1A 0.731(13) 0.806(9) 0.573(8) 0.025 Uiso d D 1 . .
H H6 -0.032(11) 0.597(8) 0.352(9) 0.03(3) Uiso d D 1 . .
H H9A 0.002(13) 0.710(13) 0.828(8) 0.03(2) Uiso d D 1 . .
H H10 -0.110(17) 0.817(16) 0.888(14) 0.07(4) 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 0.0033 0.0016 '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 0.0061 0.0033 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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
_geom_angle_publ_flag
O2 Cr1 O2 2_666 . 180.00(15) ?
O2 Cr1 O7 2_666 . 88.35(17) ?
O2 Cr1 O7 . . 91.65(17) ?
O2 Cr1 O7 2_666 2_666 91.65(17) ?
O2 Cr1 O7 . 2_666 88.35(17) ?
O7 Cr1 O7 . 2_666 180.0(2) ?
O2 Cr1 O1 2_666 2_666 90.51(17) ?
O2 Cr1 O1 . 2_666 89.49(17) ?
O7 Cr1 O1 . 2_666 90.81(18) ?
O7 Cr1 O1 2_666 2_666 89.19(18) ?
O2 Cr1 O1 2_666 . 89.49(17) ?
O2 Cr1 O1 . . 90.51(17) ?
O7 Cr1 O1 . . 89.19(18) ?
O7 Cr1 O1 2_666 . 90.81(18) ?
O1 Cr1 O1 2_666 . 180.0(3) ?
O6 P2 O7 . . 114.8(2) ?
O6 P2 O5 . . 107.8(2) ?
O7 P2 O5 . . 109.7(2) ?
O6 P2 C1 . . 108.2(3) ?
O7 P2 C1 . . 109.0(2) ?
O5 P2 C1 . . 107.1(2) ?
O4 P1 O2 1 . 115.5(2) ?
O4 P1 O2 . . 115.5(2) ?
O4 P1 O3 1 . 107.9(2) ?
O4 P1 O3 . . 107.9(2) ?
O2 P1 O3 . . 108.6(2) ?
O4 P1 C1 1 . 110.1(2) ?
O4 P1 C1 . . 110.1(2) ?
O2 P1 C1 . . 107.6(2) ?
O3 P1 C1 . . 106.9(3) ?
P1 O2 Cr1 . . 134.1(2) ?
P2 O5 H6 . . 114(5) ?
P1 O3 H3 . . 109.5 ?
P2 O7 Cr1 . . 140.0(3) ?
H9A O9 H10 . . 108(10) ?
Cr1 O1 H1B . . 119(6) ?
Cr1 O1 H1A . . 120(6) ?
H1B O1 H1A . . 107(9) ?
P1 C1 P2 . . 114.8(3) ?
P1 C1 H4 . . 108.6 ?
P2 C1 H4 . . 108.6 ?
P1 C1 H5 . . 108.6 ?
P2 C1 H5 . . 108.6 ?
H4 C1 H5 . . 107.5 ?
H8 O8 H7 . . 114(10) ?
C2 N1 C3 . . 123(4) ?
C2 N1 H1 . . 118.3 ?
C3 N1 H1 . . 118.3 ?
C3 C4 C2 . . 116(5) ?
C3 C4 H4A . . 122.1 ?
C2 C4 H4A . . 122.1 ?
N1 C3 C2 . 2_665 118(2) ?
C2 C3 C4 2_665 . 122(3) ?
N1 C3 H3A . . 121.1 ?
C2 C3 H3A 2_665 . 121.1 ?
C4 C3 H3A . . 116.7 ?
N1 C2 C3 . 2_665 119(2) ?
C3 C2 C4 2_665 . 122(2) ?
N1 C2 H2 . . 120.7 ?
C3 C2 H2 2_665 . 120.7 ?
C4 C2 H2 . . 117.1 ?
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
Cr1 O1 . 1.991(4) y
Cr1 O2 . 1.956(4) y
Cr1 O7 . 1.964(4) y
P2 O6 . 1.499(4) ?
P2 O7 . 1.519(4) ?
P2 O5 . 1.568(4) ?
P2 C1 . 1.804(6) ?
P1 O4 1 1.512(4) ?
P1 O4 . 1.512(4) ?
P1 O2 . 1.515(4) ?
P1 O3 . 1.568(4) ?
P1 C1 . 1.797(6) ?
O5 H6 . 0.83(5) ?
O3 H3 . 0.8200 ?
O9 H9A . 0.83(6) ?
O9 H10 . 0.84(7) ?
O1 H1B . 0.83(6) ?
O1 H1A . 0.80(6) ?
C1 H4 . 0.9700 ?
C1 H5 . 0.9700 ?
O8 H8 . 0.85(7) ?
O8 H7 . 0.83(6) ?
N1 C2 . 1.34(5) ?
N1 C3 . 1.36(4) ?
N1 H1 . 0.8600 ?
C4 C3 . 1.40(5) ?
C4 C2 . 1.41(5) ?
C4 H4A . 0.9300 ?
C3 C2 2_665 1.371(13) ?
C3 H3A . 0.9300 ?
C2 C3 2_665 1.371(13) ?
C2 H2 . 0.9300 ?
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
_geom_hbond_publ_flag
C1 H4 O6 2_676 0.97 2.49 3.346(7) 147 y
C4 H4A O9 2_566 0.93 2.16 2.93(7) 140 y
N1 H1 O9 2_566 0.86 2.32 3.03(5) 141 y
O1 H1A O6 2_676 0.80(6) 1.83(6) 2.634(6) 176(9) y
O1 H1B O4 1_655 0.83(6) 1.87(6) 2.704(6) 177(9) y
O3 H3 O8 2_677 0.82 1.83 2.629(6) 163 y
O5 H6 O4 2_566 0.83(5) 1.80(5) 2.619(6) 175(10) y
O8 H7 O6 1_556 0.83(6) 1.86(6) 2.687(6) 171(9) y
O8 H8 O9 1 0.85(7) 1.94(8) 2.748(7) 158(11) y
O9 H9A O4 1 0.83(6) 2.00(6) 2.833(6) 179(10) y
O9 H10 O8 2_577 0.84(7) 1.99(7) 2.820(7) 174(13) y
