#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/48/2214889.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_2214889
loop_
_publ_author_name
'Boudraa, Mhamed'
'Merazig, Hocine'
'Bouacida, Sofiane'
'Benard-Rocherulle, Patricia'
'Roisnel, Thierry'
_publ_section_title
;
 The solid solution Co~4.32~Mn~2.68~(HPO₄)₄(PO₄)₂
;
_journal_coeditor_code           WM2131
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i168
_journal_page_last               i169
_journal_paper_doi               10.1107/S1600536807031352
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'Co4.32 Mn2.68 (H P O4)4 (P O4)2'
_chemical_formula_structural     '(Co4.32 Mn2.68) (H P O4)4 (P O4)2'
_chemical_formula_sum            'Co4.32 H4 Mn2.68 O24 P6'
_chemical_formula_weight         974.07
_chemical_name_systematic
;
cobalt manganese tetrakis(hydrogen phosphate) bis(phosphate)
;
_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                104.428(3)
_cell_angle_beta                 109.1800(10)
_cell_angle_gamma                101.389(3)
_cell_formula_units_Z            1
_cell_length_a                   6.5119(12)
_cell_length_b                   7.9623(12)
_cell_length_c                   9.5799(10)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40.10
_cell_measurement_theta_min      2.41
_cell_volume                     432.64(11)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker, 2003)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (Burla et al.,  2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10685
_diffrn_reflns_theta_full        40.36
_diffrn_reflns_theta_max         40.36
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    6.648
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             469.6
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.818
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         5484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0676P)²+0.8077P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                4111
_reflns_number_total             5484
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm2131.cif
_cod_data_source_block           I
_cod_database_code               2214889
_cod_database_fobs_code          2214889
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
Co Co3 0.38449(3) 0.45668(3) 0.10926(2) 0.00799(5) Uani d P 0.796(12)
Mn Mn3 0.38449(3) 0.45668(3) 0.10926(2) 0.00799(5) Uani d P 0.204(12)
Co Co1 0.05082(4) 0.71421(3) 0.51524(2) 0.00797(5) Uani d P 0.729(12)
Mn Mn1 0.05082(4) 0.71421(3) 0.51524(2) 0.00797(5) Uani d P 0.271(12)
Co Co2 0.0000 0.0000 0.0000 0.00878(7) Uani d SP 0.418(16)
Mn Mn2 0.0000 0.0000 0.0000 0.00878(7) Uani d SP 0.582(16)
Co Co4 0.28343(4) 0.81332(3) 0.28480(3) 0.00936(6) Uani d P 0.424(12)
Mn Mn4 0.28343(4) 0.81332(3) 0.28480(3) 0.00936(6) Uani d P 0.576(12)
P P1 0.22577(6) 0.14388(5) -0.22339(4) 0.00662(7) Uani d . 1
P P3 -0.08771(6) 0.42078(5) 0.17407(4) 0.00616(7) Uani d . 1
P P2 0.41114(6) 1.23356(5) 0.37360(5) 0.00817(7) Uani d . 1
O O4 0.22221(19) 0.18779(14) -0.05752(13) 0.00969(18) Uani d . 1
O O2 0.44797(18) 0.24541(14) -0.22778(13) 0.00928(18) Uani d . 1
O O6 0.4801(2) 1.38550(15) 0.31163(14) 0.0130(2) Uani d . 1
O O7 0.27261(19) 1.29718(16) 0.47367(14) 0.0125(2) Uani d D 1
O O5 0.61929(19) 1.20780(16) 0.48908(14) 0.0124(2) Uani d . 1
O O3 0.2064(2) -0.06486(14) -0.27465(13) 0.01030(19) Uani d D 1
O O8 0.26319(19) 1.05504(14) 0.24010(13) 0.0118(2) Uani d . 1
O O10 0.12308(18) 0.53885(14) 0.16495(13) 0.00955(18) Uani d . 1
O O9 -0.30343(17) 0.46328(14) 0.08719(13) 0.00871(18) Uani d . 1
O O11 -0.05564(19) 0.45695(14) 0.34663(12) 0.00933(18) Uani d . 1
O O12 -0.1130(2) 0.21731(14) 0.09879(14) 0.0118(2) Uani d . 1
O O1 0.01773(19) 0.16985(14) -0.33822(13) 0.00999(18) Uiso d . 1
H H1P 0.184(5) -0.105(4) -0.205(3) 0.050 Uiso d D 1
H H2P 0.341(5) 1.401(2) 0.545(3) 0.050 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
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
H H 0.0000 0.0000 '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
O9 M3 O6 2_565 1_545 177.41(4)
O9 M3 O9 2_565 1_655 84.92(4)
O6 M3 O9 1_545 1_655 93.39(4)
O9 M3 O10 2_565 . 91.88(4)
O6 M3 O10 1_545 . 89.13(5)
O9 M3 O10 1_655 . 161.97(4)
O9 M3 O4 2_565 . 84.43(4)
O6 M3 O4 1_545 . 97.60(4)
O9 M3 O4 1_655 . 91.92(4)
O10 M3 O4 . . 105.44(4)
O9 M3 O2 2_565 2_665 81.10(4)
O6 M3 O2 1_545 2_665 96.76(4)
O9 M3 O2 1_655 2_665 83.03(4)
O10 M3 O2 . 2_665 78.94(4)
O4 M3 O2 . 2_665 165.03(4)
O9 M3 M3 2_565 2_665 42.81(3)
O6 M3 M3 1_545 2_665 135.46(4)
O9 M3 M3 1_655 2_665 42.10(3)
O10 M3 M3 . 2_665 132.14(3)
O4 M3 M3 . 2_665 87.57(3)
O2 M3 M3 2_665 2_665 79.23(3)
O11 M1 O3 . 1_566 163.60(4)
O11 M1 O1 . 2_565 90.18(4)
O3 M1 O1 1_566 2_565 105.01(4)
O11 M1 O11 . 2_566 78.20(5)
O3 M1 O11 1_566 2_566 87.39(4)
O1 M1 O11 2_565 2_566 166.41(4)
O11 M1 O7 . 2_576 96.03(4)
O3 M1 O7 1_566 2_576 89.65(4)
O1 M1 O7 2_565 2_576 92.17(5)
O11 M1 O7 2_566 2_576 82.20(4)
O11 M1 O5 . 2_676 94.92(4)
O3 M1 O5 1_566 2_676 82.07(5)
O1 M1 O5 2_565 2_676 79.53(4)
O11 M1 O5 2_566 2_676 108.19(4)
O7 M1 O5 2_576 2_676 166.27(5)
O12 M2 O12 . 2 180.00(6)
O12 M2 O4 . 2 90.32(4)
O12 M2 O4 2 2 89.68(4)
O12 M2 O4 . . 89.68(4)
O12 M2 O4 2 . 90.32(4)
O4 M2 O4 2 . 180.00(5)
O12 M2 O8 . 1_545 89.04(4)
O12 M2 O8 2 1_545 90.96(4)
O4 M2 O8 2 1_545 85.96(4)
O4 M2 O8 . 1_545 94.04(4)
O12 M2 O8 . 2_565 90.96(4)
O12 M2 O8 2 2_565 89.04(4)
O4 M2 O8 2 2_565 94.04(4)
O4 M2 O8 . 2_565 85.96(4)
O8 M2 O8 1_545 2_565 180.00(6)
O10 M4 O8 . . 136.28(5)
O10 M4 O2 . 2_665 83.06(4)
O8 M4 O2 . 2_665 105.04(4)
O10 M4 O5 . 2_676 95.67(5)
O8 M4 O5 . 2_676 123.79(5)
O2 M4 O5 2_665 2_676 100.18(4)
O10 M4 O1 . 2_565 88.72(4)
O8 M4 O1 . 2_565 83.01(4)
O2 M4 O1 2_665 2_565 171.24(4)
O5 M4 O1 2_676 2_565 77.56(4)
O1 P1 O2 . . 111.62(6)
O1 P1 O4 . . 110.72(6)
O2 P1 O4 . . 114.57(6)
O1 P1 O3 . . 108.54(6)
O2 P1 O3 . . 106.78(6)
O4 P1 O3 . . 104.08(6)
O9 P3 O11 . . 108.96(6)
O9 P3 O10 . . 110.59(6)
O11 P3 O10 . . 110.28(6)
O9 P3 O12 . . 109.91(6)
O11 P3 O12 . . 108.53(6)
O10 P3 O12 . . 108.55(6)
O8 P2 O6 . . 111.66(7)
O8 P2 O5 . . 111.13(7)
O6 P2 O5 . . 111.70(7)
O8 P2 O7 . . 109.60(6)
O6 P2 O7 . . 107.40(7)
O5 P2 O7 . . 105.06(7)
P1 O4 M3 . . 120.45(6)
P1 O4 M2 . . 122.03(6)
M3 O4 M2 . . 116.38(5)
P1 O2 M4 . 2_665 138.88(6)
P1 O2 M4 . 2_665 138.88(6)
P1 O2 M3 . 2_665 123.34(6)
M4 O2 M3 2_665 2_665 96.67(4)
M4 O2 M3 2_665 2_665 96.67(4)
P1 O2 M3 . 2_665 123.34(6)
M4 O2 M3 2_665 2_665 96.67(4)
P2 O6 M3 . 1_565 141.22(7)
P2 O7 M1 . 2_576 148.04(7)
P2 O7 H2P . . 114(2)
M1 O7 H2P 2_576 . 94(2)
M1 O7 H2P 2_576 . 94(2)
P2 O5 M4 . 2_676 136.06(7)
P2 O5 M1 . 2_676 121.90(7)
M4 O5 M1 2_676 2_676 98.92(5)
P2 O5 M1 . 2_676 121.90(7)
M4 O5 M1 2_676 2_676 98.92(5)
P1 O3 M1 . 1_544 135.93(7)
P1 O3 M1 . 1_544 135.93(7)
P1 O3 H1P . . 107.8(19)
M1 O3 H1P 1_544 . 106(2)
M1 O3 H1P 1_544 . 106(2)
P2 O8 M4 . . 117.24(7)
P2 O8 M2 . 1_565 131.08(7)
M4 O8 M2 . 1_565 111.53(5)
M4 O8 M2 . 1_565 111.53(5)
P3 O10 M4 . . 126.48(6)
P3 O10 M3 . . 128.41(6)
M4 O10 M3 . . 101.20(5)
P3 O9 M3 . 2_565 129.37(6)
P3 O9 M3 . 1_455 135.51(7)
M3 O9 M3 2_565 1_455 95.08(4)
P3 O9 M3 . 1_455 135.51(7)
M3 O9 M3 2_565 1_455 95.08(4)
P3 O11 M1 . . 124.87(6)
P3 O11 M1 . 2_566 132.69(6)
M1 O11 M1 . 2_566 101.80(5)
M1 O11 M1 . 2_566 101.80(5)
P3 O12 M2 . . 153.67(7)
P1 O1 M1 . 2_565 137.39(7)
P1 O1 M4 . 2_565 121.67(6)
M1 O1 M4 2_565 2_565 97.21(4)
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
M1 O11 . 2.0833(11) yes
M1 O3 1_566 2.0890(11) yes
M1 O1 2_565 2.0911(11) yes
M1 O11 2_566 2.1208(11) yes
M1 O7 2_576 2.1288(12) yes
M1 O5 2_676 2.1322(12) yes
M2 O12 . 2.1390(11) yes
M2 O12 2 2.1390(11) yes
M2 O4 2 2.1710(11) yes
M2 O4 . 2.1710(11) yes
M2 O8 1_545 2.2430(12) yes
M2 O8 2_565 2.2430(12) yes
M3 O9 2_565 2.0748(11) yes
M3 O6 1_545 2.0882(12) yes
M3 O9 1_655 2.1032(11) yes
M3 O10 . 2.1149(11) yes
M3 O4 . 2.1320(11) yes
M3 O2 2_665 2.2199(11) yes
M3 M3 2_665 3.0824(5) ?
M4 O10 . 2.0604(11) yes
M4 O8 . 2.0926(12) yes
M4 O2 2_665 2.0976(11) yes
M4 O5 2_676 2.1081(12) yes
M4 O1 2_565 2.2034(12) yes
P1 O1 . 1.5274(12) y
P1 O2 . 1.5310(11) y
P1 O4 . 1.5486(11) y
P1 O3 . 1.5777(11) yes
P2 O8 . 1.5257(12) y
P2 O6 . 1.5285(12) y
P2 O5 . 1.5300(12) y
P2 O7 . 1.5799(12) yes
P3 O9 . 1.5298(11) y
P3 O11 . 1.5400(11) y
P3 O10 . 1.5445(11) y
P3 O12 . 1.5512(11) y
O2 M4 2_665 2.0976(11) ?
O2 M3 2_665 2.2199(11) ?
O6 M3 1_565 2.0882(12) ?
O7 M1 2_576 2.1288(12) ?
O7 H2P . 0.85(3) ?
O5 M4 2_676 2.1081(12) ?
O5 M1 2_676 2.1322(12) ?
O3 M1 1_544 2.0890(11) ?
O3 H1P . 0.85(3) ?
O8 M2 1_565 2.2430(12) ?
O9 M3 2_565 2.0748(11) ?
O9 M3 1_455 2.1032(11) ?
O11 M1 2_566 2.1208(11) ?
O1 M1 2_565 2.0911(11) ?
O1 M4 2_565 2.2034(12) ?
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
O3 H1P O12 2_555 0.85(3) 1.63(3) 2.4663(18) 169(3) yes
O7 H2P O6 2_686 0.85(2) 1.77(2) 2.6143(18) 172(3) yes
