data_ICSD-421646
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'H10 Mn5 O20 P4'
_chemical_formula_weight          728.66
 
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'
 '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'
 'Mn'  'Mn'   0.3368   0.7283
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    'c 2/c'
_symmetry_space_group_name_hall   '-c 2yc'
 
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'
 
_cell_length_a                    17.612(4)
_cell_length_b                    9.1348(14)
_cell_length_c                    9.4806(15)
_cell_angle_alpha                 90.00
_cell_angle_beta                  96.491(3)
_cell_angle_gamma                 90.00
_cell_volume                      1515.5(4)
_cell_formula_units_Z             4
_cell_measurement_temperature     298(2)
_cell_measurement_reflns_used     1341
_cell_measurement_theta_min       2.52
_cell_measurement_theta_max       25.03
 
_exptl_crystal_description        'needle-like'
_exptl_crystal_colour             transparent
_exptl_crystal_size_max           0.40
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.194
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1420
_exptl_absorpt_coefficient_mu     4.592
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.345
_exptl_absorpt_correction_T_max   0.399
_exptl_absorpt_process_details    
;
CrysAlis (Oxford Diffraction, 2006)
; 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       298(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Oxford diffraction Gemini R Ultra'
_diffrn_measurement_method        'ω scan' 
_diffrn_detector_area_resol_mean  10.0
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             3670
_diffrn_reflns_av_R_equivalents   0.0344
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_limit_h_min        -20
_diffrn_reflns_limit_h_max        20
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -10
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          2.52
_diffrn_reflns_theta_max          25.03
_reflns_number_total              1341
_reflns_number_gt                 1279
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'CrysAlis (Oxford Diffraction,2006)'
_computing_cell_refinement        'CrysAlis'
_computing_data_reduction         'CrysAlis'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material   'SHELXL-97'
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0609P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          1334
_refine_ls_number_parameters      147
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0262
_refine_ls_R_factor_gt            0.0233
_refine_ls_wR_factor_ref          0.0734
_refine_ls_wR_factor_gt           0.0726
_refine_ls_goodness_of_fit_ref    1.009
_refine_ls_restrained_S_all       1.009
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Mn1 Mn 0.181831(19) 0.08905(4) 0.31518(4) 0.00915(16) Uani 1 1 d . . .
Mn2 Mn 0.17446(2) 0.47209(4) 0.36510(4) 0.00891(16) Uani 1 1 d . . .
Mn3 Mn 0.0000 0.60264(5) 0.2500 0.00862(18) Uani 1 2 d S . .
P1 P 0.08267(3) 0.32092(7) 0.08975(6) 0.00681(18) Uani 1 1 d . . .
P2 P 0.16070(3) 0.23961(6) 0.62822(6) 0.00600(18) Uani 1 1 d . . .
O1 O 0.01198(11) 0.21589(19) 0.0809(2) 0.0136(4) Uani 1 1 d . . .
H1 H -0.014(2) 0.227(3) 0.013(4) 0.020 Uiso 1 1 d . . .
O2 O 0.15435(9) 0.22929(19) 0.13261(18) 0.0113(4) Uani 1 1 d . . .
O3 O 0.07709(9) 0.4330(2) 0.20626(19) 0.0120(4) Uani 1 1 d . . .
O4 O 0.08409(9) 0.39165(18) -0.05537(19) 0.0111(4) Uani 1 1 d . . .
O5 O 0.16374(9) 0.26413(18) 0.46778(19) 0.0092(4) Uani 1 1 d . . .
O6 O 0.20170(9) 0.36645(18) 0.71087(18) 0.0099(4) Uani 1 1 d . . .
O7 O 0.20151(9) 0.09629(17) 0.67322(18) 0.0101(4) Uani 1 1 d . . .
O8 O 0.07587(9) 0.23415(18) 0.65791(19) 0.0098(4) Uani 1 1 d . . .
O1W O 0.07720(11) -0.0114(2) 0.3486(2) 0.0194(5) Uani 1 1 d . . .
H1A H 0.0700(19) -0.078(4) 0.284(4) 0.029 Uiso 1 1 d . . .
H1B H 0.0380(19) 0.040(4) 0.359(4) 0.029 Uiso 1 1 d . . .
O2W O 0.25929(11) 0.57961(19) 0.5299(2) 0.0118(4) Uani 1 1 d . . .
H2A H 0.288(2) 0.626(4) 0.484(4) 0.018 Uiso 1 1 d . . .
H2B H 0.2469(18) 0.631(4) 0.579(4) 0.018 Uiso 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Mn1 O1W 2.1145(19) . ?
Mn1 O6 2.1327(16) 7_556 ?
Mn1 O2 2.1637(17) . ?
Mn1 O5 2.2037(17) . ?
Mn1 O7 2.2144(17) 6 ?
Mn1 O2W 2.2941(18) 7_556 ?
Mn2 O5 2.1526(17) . ?
Mn2 O6 2.1684(17) 6_565 ?
Mn2 O3 2.1799(17) . ?
Mn2 O4 2.2186(17) 6_566 ?
Mn2 O2W 2.2604(19) . ?
Mn2 O7 2.3394(17) 7_556 ?
Mn3 O3 2.1315(18) 2 ?
Mn3 O3 2.1315(18) . ?
Mn3 O4 2.2323(18) 6_566 ?
Mn3 O4 2.2323(18) 5_565 ?
Mn3 O8 2.2437(17) 6_565 ?
Mn3 O8 2.2437(17) 5_566 ?
P1 O3 1.5177(19) . ?
P1 O4 1.5228(18) . ?
P1 O2 1.5308(17) . ?
P1 O1 1.5666(19) . ?
P2 O7 1.5309(16) . ?
P2 O6 1.5330(17) . ?
P2 O5 1.5444(18) . ?
P2 O8 1.5520(17) . ?
O1 H1 0.75(4) . ?
O4 Mn2 2.2186(17) 6_565 ?
O4 Mn3 2.2323(18) 5_565 ?
O6 Mn1 2.1327(16) 7_556 ?
O6 Mn2 2.1684(17) 6_566 ?
O7 Mn1 2.2144(17) 6_556 ?
O7 Mn2 2.3394(17) 7_556 ?
O8 Mn3 2.2437(17) 5_566 ?
O1W H1A 0.86(4) . ?
O1W H1B 0.85(4) . ?
O2W Mn1 2.2941(18) 7_556 ?
O2W H2A 0.82(4) . ?
O2W H2B 0.71(4) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1W Mn1 O6 165.02(8) . 7_556 ?
O1W Mn1 O2 104.90(8) . . ?
O6 Mn1 O2 85.73(7) 7_556 . ?
O1W Mn1 O5 91.34(7) . . ?
O6 Mn1 O5 98.63(6) 7_556 . ?
O2 Mn1 O5 93.42(7) . . ?
O1W Mn1 O7 87.61(7) . 6 ?
O6 Mn1 O7 81.76(6) 7_556 6 ?
O2 Mn1 O7 90.15(7) . 6 ?
O5 Mn1 O7 176.42(7) . 6 ?
O1W Mn1 O2W 87.19(8) . 7_556 ?
O6 Mn1 O2W 80.28(7) 7_556 7_556 ?
O2 Mn1 O2W 162.54(7) . 7_556 ?
O5 Mn1 O2W 98.94(7) . 7_556 ?
O7 Mn1 O2W 77.60(7) 6 7_556 ?
O5 Mn2 O6 160.49(7) . 6_565 ?
O5 Mn2 O3 93.76(7) . . ?
O6 Mn2 O3 82.08(7) 6_565 . ?
O5 Mn2 O4 103.79(7) . 6_566 ?
O6 Mn2 O4 93.98(6) 6_565 6_566 ?
O3 Mn2 O4 77.76(7) . 6_566 ?
O5 Mn2 O2W 98.97(7) . . ?
O6 Mn2 O2W 89.49(7) 6_565 . ?
O3 Mn2 O2W 162.82(7) . . ?
O4 Mn2 O2W 87.99(7) 6_566 . ?
O5 Mn2 O7 88.04(6) . 7_556 ?
O6 Mn2 O7 78.19(6) 6_565 7_556 ?
O3 Mn2 O7 121.63(6) . 7_556 ?
O4 Mn2 O7 157.05(6) 6_566 7_556 ?
O2W Mn2 O7 70.58(7) . 7_556 ?
O3 Mn3 O3 86.75(10) 2 . ?
O3 Mn3 O4 103.52(6) 2 6_566 ?
O3 Mn3 O4 78.47(6) . 6_566 ?
O3 Mn3 O4 78.47(6) 2 5_565 ?
O3 Mn3 O4 103.52(6) . 5_565 ?
O4 Mn3 O4 177.33(9) 6_566 5_565 ?
O3 Mn3 O8 168.29(6) 2 6_565 ?
O3 Mn3 O8 89.24(7) . 6_565 ?
O4 Mn3 O8 86.41(6) 6_566 6_565 ?
O4 Mn3 O8 91.81(6) 5_565 6_565 ?
O3 Mn3 O8 89.24(7) 2 5_566 ?
O3 Mn3 O8 168.29(6) . 5_566 ?
O4 Mn3 O8 91.81(6) 6_566 5_566 ?
O4 Mn3 O8 86.41(6) 5_565 5_566 ?
O8 Mn3 O8 96.72(9) 6_565 5_566 ?
O3 P1 O4 112.35(10) . . ?
O3 P1 O2 107.17(10) . . ?
O4 P1 O2 112.00(10) . . ?
O3 P1 O1 109.63(10) . . ?
O4 P1 O1 107.78(10) . . ?
O2 P1 O1 107.82(10) . . ?
O7 P2 O6 108.95(10) . . ?
O7 P2 O5 109.33(9) . . ?
O6 P2 O5 109.09(9) . . ?
O7 P2 O8 110.69(9) . . ?
O6 P2 O8 109.82(9) . . ?
O5 P2 O8 108.94(10) . . ?
P1 O1 H1 112(3) . . ?
P1 O2 Mn1 129.73(10) . . ?
P1 O3 Mn3 136.66(10) . . ?
P1 O3 Mn2 120.17(9) . . ?
Mn3 O3 Mn2 102.43(8) . . ?
P1 O4 Mn2 129.11(10) . 6_565 ?
P1 O4 Mn3 132.81(10) . 5_565 ?
Mn2 O4 Mn3 98.07(7) 6_565 5_565 ?
P2 O5 Mn2 126.01(10) . . ?
P2 O5 Mn1 124.41(10) . . ?
Mn2 O5 Mn1 108.48(8) . . ?
P2 O6 Mn1 119.24(9) . 7_556 ?
P2 O6 Mn2 137.00(9) . 6_566 ?
Mn1 O6 Mn2 103.74(7) 7_556 6_566 ?
P2 O7 Mn1 136.25(10) . 6_556 ?
P2 O7 Mn2 127.04(9) . 7_556 ?
Mn1 O7 Mn2 95.93(6) 6_556 7_556 ?
P2 O8 Mn3 132.61(10) . 5_566 ?
Mn1 O1W H1A 105(2) . . ?
Mn1 O1W H1B 121(2) . . ?
H1A O1W H1B 114(3) . . ?
Mn2 O2W Mn1 111.49(8) . 7_556 ?
Mn2 O2W H2A 105(2) . . ?
Mn1 O2W H2A 116(2) 7_556 . ?
Mn2 O2W H2B 121(2) . . ?
Mn1 O2W H2B 100(3) 7_556 . ?
H2A O2W H2B 105(3) . . ?
 
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_angle_DHA
 _geom_hbond_site_symmetry_A
O2W H2B O2  0.71(4) 2.18(3) 2.796(3) 146(3) 6_566
O2W H2A O2  0.82(4) 1.84(4) 2.662(3) 175(3) 4
O1W H1B O1  0.85(4) 1.95(4) 2.732(3) 153(3) 2
O1W H1A O8  0.86(4) 1.87(4) 2.720(3) 168(3) 6
O1 H1 O8  0.75(4) 1.85(4) 2.599(3) 173(4) 2
 
_diffrn_measured_fraction_theta_max    0.994
_diffrn_reflns_theta_full              25.03
_diffrn_measured_fraction_theta_full   0.994
_refine_diff_density_max    0.654
_refine_diff_density_min   -1.142
_refine_diff_density_rms    0.231
