data_2011jaa0007_p21nii

_audit_update_record
;
2012-06-07 # Formatted by publCIF
;
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'F3 K Mn O3 P '
_chemical_formula_weight          230.01
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 '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'
 'K'  'K'   0.2009   0.2494
 '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    P21/n
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    5.4027(2)
_cell_length_b                    12.4794(6)
_cell_length_c                    7.3305(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  107.145(3)
_cell_angle_gamma                 90.00
_cell_volume                      472.28(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     4805
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        plate
_exptl_crystal_colour             brown
_exptl_crystal_size_max           0.02
_exptl_crystal_size_mid           0.02
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.235
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              327
_exptl_absorpt_coefficient_mu     4.008
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9425
_exptl_absorpt_correction_T_max   0.9707
_exptl_absorpt_process_details    ?
 
_exptl_special_details
?
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode' 
_diffrn_radiation_monochromator   '10cm confocal mirrors'
_diffrn_measurement_device_type   'Bruker-Nonius APEX II CCD camera on κ-goniostat' 
_diffrn_measurement_method        'φ & ω scans'
_diffrn_detector_area_resol_mean  '4096x4096pixels / 62x62mm'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             6113
_diffrn_reflns_av_R_equivalents   0.0685
_diffrn_reflns_av_sigmaI/netI     0.0511
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -7
_diffrn_reflns_limit_l_max        9
_diffrn_reflns_theta_min          3.26
_diffrn_reflns_theta_max          27.58
_reflns_number_total              1080
_reflns_number_gt                 865
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_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 > 2σ(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)+(0.0000P)²+17.1752P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          1080
_refine_ls_number_parameters      85
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0723
_refine_ls_R_factor_gt            0.0516
_refine_ls_wR_factor_ref          0.1151
_refine_ls_wR_factor_gt           0.1012
_refine_ls_goodness_of_fit_ref    0.837
_refine_ls_restrained_S_all       0.837
_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
O12 O 0.2244(8) 0.6147(4) 0.0541(6) 0.0106(9) Uani 1 1 d . . .
O10 O 0.1472(8) 0.5268(4) 0.3458(6) 0.0102(9) Uani 1 1 d . . .
O11 O 0.7706(8) 0.6034(4) 0.0838(6) 0.0105(9) Uani 1 1 d . . .
F1 F 0.4218(7) 0.5566(3) -0.2456(5) 0.0103(8) Uani 1 1 d . . .
F2 F 0.5944(7) 0.6361(3) -0.5384(5) 0.0137(8) Uani 1 1 d . . .
F3 F 0.0829(8) 0.7201(3) 0.2919(6) 0.0166(9) Uani 1 1 d . . .
K1 K 0.0430(3) 0.70063(12) -0.3118(2) 0.0156(3) Uani 1 1 d . . .
Mn2 Mn 0.5000 0.5000 0.0000 0.0074(3) Uani 1 2 d S . .
Mn3 Mn 0.5000 0.5000 -0.5000 0.0077(3) Uani 1 2 d S . .
P2 P 0.0585(3) 0.60840(13) 0.1859(2) 0.0080(3) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
O12 P2 1.501(5) . ?
O12 Mn2 2.185(4) . ?
O12 K1 2.785(5) . ?
O12 K1 2.871(5) 4_676 ?
O10 P2 1.520(5) . ?
O10 Mn3 1.937(4) 1_556 ?
O10 K1 3.004(5) 3_565 ?
O11 P2 1.515(4) 1_655 ?
O11 Mn2 1.911(4) . ?
O11 K1 2.938(5) 4_676 ?
F1 Mn2 1.863(4) . ?
F1 Mn3 2.149(4) . ?
F1 K1 2.659(4) . ?
F2 Mn3 1.819(4) . ?
F2 K1 2.628(4) 1_655 ?
F2 K1 2.814(4) 4_675 ?
F3 P2 1.582(4) . ?
F3 K1 2.959(4) 4_576 ?
F3 K1 2.975(4) 4_676 ?
F3 K1 2.986(4) 1_556 ?
K1 F2 2.628(4) 1_455 ?
K1 F2 2.814(4) 4_576 ?
K1 O12 2.871(5) 4_575 ?
K1 O11 2.938(5) 4_575 ?
K1 F3 2.959(4) 4_675 ?
K1 F3 2.975(4) 4_575 ?
K1 F3 2.986(4) 1_554 ?
K1 O10 3.004(5) 3_565 ?
K1 P2 3.536(2) 4_575 ?
K1 P2 3.670(2) 4_675 ?
Mn2 F1 1.863(4) 3_665 ?
Mn2 O11 1.911(4) 3_665 ?
Mn2 O12 2.185(4) 3_665 ?
Mn2 K1 3.7766(14) 3_665 ?
Mn2 K1 3.9656(15) 2_544 ?
Mn2 K1 3.9656(15) 4_676 ?
Mn3 F2 1.819(4) 3_664 ?
Mn3 O10 1.937(4) 1_554 ?
Mn3 O10 1.937(4) 3_665 ?
Mn3 F1 2.149(4) 3_664 ?
Mn3 K1 3.7936(15) 3_564 ?
Mn3 K1 3.7936(15) 1_655 ?
Mn3 K1 4.0345(16) 3_664 ?
P2 O11 1.515(4) 1_455 ?
P2 K1 3.536(2) 4_676 ?
P2 K1 3.670(2) 4_576 ?
 
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
P2 O12 Mn2 130.6(3) . . ?
P2 O12 K1 122.2(2) . . ?
Mn2 O12 K1 98.19(16) . . ?
P2 O12 K1 103.5(2) . 4_676 ?
Mn2 O12 K1 102.48(16) . 4_676 ?
K1 O12 K1 91.49(13) . 4_676 ?
P2 O10 Mn3 126.7(3) . 1_556 ?
P2 O10 K1 123.1(2) . 3_565 ?
Mn3 O10 K1 97.98(17) 1_556 3_565 ?
P2 O11 Mn2 139.7(3) 1_655 . ?
P2 O11 K1 106.6(2) 1_655 4_676 ?
Mn2 O11 K1 107.85(18) . 4_676 ?
Mn2 F1 Mn3 131.89(19) . . ?
Mn2 F1 K1 112.06(16) . . ?
Mn3 F1 K1 113.67(15) . . ?
Mn3 F2 K1 115.89(17) . 1_655 ?
Mn3 F2 K1 144.38(19) . 4_675 ?
K1 F2 K1 96.18(12) 1_655 4_675 ?
P2 F3 K1 103.61(18) . 4_576 ?
P2 F3 K1 97.03(18) . 4_676 ?
K1 F3 K1 131.14(15) 4_576 4_676 ?
P2 F3 K1 112.7(2) . 1_556 ?
K1 F3 K1 85.91(11) 4_576 1_556 ?
K1 F3 K1 125.53(14) 4_676 1_556 ?
F2 K1 F1 115.15(13) 1_455 . ?
F2 K1 O12 119.21(14) 1_455 . ?
F1 K1 O12 62.01(12) . . ?
F2 K1 F2 123.44(15) 1_455 4_576 ?
F1 K1 F2 116.77(12) . 4_576 ?
O12 K1 F2 70.11(13) . 4_576 ?
F2 K1 O12 71.42(13) 1_455 4_575 ?
F1 K1 O12 163.08(13) . 4_575 ?
O12 K1 O12 130.09(16) . 4_575 ?
F2 K1 O12 65.55(12) 4_576 4_575 ?
F2 K1 O11 117.98(13) 1_455 4_575 ?
F1 K1 O11 104.56(12) . 4_575 ?
O12 K1 O11 121.05(14) . 4_575 ?
F2 K1 O11 67.78(12) 4_576 4_575 ?
O12 K1 O11 59.84(12) 4_575 4_575 ?
F2 K1 F3 156.95(13) 1_455 4_675 ?
F1 K1 F3 62.08(12) . 4_675 ?
O12 K1 F3 80.85(12) . 4_675 ?
F2 K1 F3 72.07(12) 4_576 4_675 ?
O12 K1 F3 105.41(12) 4_575 4_675 ?
O11 K1 F3 48.09(11) 4_575 4_675 ?
F2 K1 F3 65.10(12) 1_455 4_575 ?
F1 K1 F3 146.55(12) . 4_575 ?
O12 K1 F3 88.00(12) . 4_575 ?
F2 K1 F3 59.45(11) 4_576 4_575 ?
O12 K1 F3 50.11(12) 4_575 4_575 ?
O11 K1 F3 103.61(12) 4_575 4_575 ?
F3 K1 F3 131.14(15) 4_675 4_575 ?
F2 K1 F3 74.19(12) 1_455 1_554 ?
F1 K1 F3 87.71(12) . 1_554 ?
O12 K1 F3 149.62(13) . 1_554 ?
F2 K1 F3 127.87(12) 4_576 1_554 ?
O12 K1 F3 79.02(12) 4_575 1_554 ?
O11 K1 F3 61.51(12) 4_575 1_554 ?
F3 K1 F3 82.78(11) 4_675 1_554 ?
F3 K1 F3 121.80(13) 4_575 1_554 ?
F2 K1 O10 55.18(12) 1_455 3_565 ?
F1 K1 O10 66.57(12) . 3_565 ?
O12 K1 O10 74.39(13) . 3_565 ?
F2 K1 O10 134.65(13) 4_576 3_565 ?
O12 K1 O10 125.04(13) 4_575 3_565 ?
O11 K1 O10 157.52(14) 4_575 3_565 ?
F3 K1 O10 128.63(12) 4_675 3_565 ?
F3 K1 O10 92.54(12) 4_575 3_565 ?
F3 K1 O10 96.73(12) 1_554 3_565 ?
F2 K1 P2 70.13(10) 1_455 4_575 ?
F1 K1 P2 170.18(10) . 4_575 ?
O12 K1 P2 108.29(11) . 4_575 ?
F2 K1 P2 55.46(8) 4_576 4_575 ?
O12 K1 P2 24.37(9) 4_575 4_575 ?
O11 K1 P2 78.69(9) 4_575 4_575 ?
F3 K1 P2 116.62(9) 4_675 4_575 ?
F3 K1 P2 26.37(8) 4_575 4_575 ?
F3 K1 P2 101.89(9) 1_554 4_575 ?
O10 K1 P2 113.69(10) 3_565 4_575 ?
F2 K1 P2 139.09(10) 1_455 4_675 ?
F1 K1 P2 84.00(9) . 4_675 ?
O12 K1 P2 101.68(10) . 4_675 ?
F2 K1 P2 67.50(9) 4_576 4_675 ?
O12 K1 P2 81.75(10) 4_575 4_675 ?
O11 K1 P2 23.32(9) 4_575 4_675 ?
F3 K1 P2 24.78(8) 4_675 4_675 ?
F3 K1 P2 118.54(9) 4_575 4_675 ?
F3 K1 P2 70.73(9) 1_554 4_675 ?
O10 K1 P2 148.74(10) 3_565 4_675 ?
P2 K1 P2 97.12(5) 4_575 4_675 ?
F1 Mn2 F1 180.0(2) . 3_665 ?
F1 Mn2 O11 89.37(18) . . ?
F1 Mn2 O11 90.63(18) 3_665 . ?
F1 Mn2 O11 90.63(18) . 3_665 ?
F1 Mn2 O11 89.37(18) 3_665 3_665 ?
O11 Mn2 O11 180.0 . 3_665 ?
F1 Mn2 O12 92.59(16) . 3_665 ?
F1 Mn2 O12 87.41(16) 3_665 3_665 ?
O11 Mn2 O12 90.18(18) . 3_665 ?
O11 Mn2 O12 89.82(18) 3_665 3_665 ?
F1 Mn2 O12 87.41(16) . . ?
F1 Mn2 O12 92.59(16) 3_665 . ?
O11 Mn2 O12 89.82(18) . . ?
O11 Mn2 O12 90.18(18) 3_665 . ?
O12 Mn2 O12 180.000(1) 3_665 . ?
F1 Mn2 K1 40.74(11) . . ?
F1 Mn2 K1 139.26(11) 3_665 . ?
O11 Mn2 K1 92.79(14) . . ?
O11 Mn2 K1 87.21(14) 3_665 . ?
O12 Mn2 K1 133.12(12) 3_665 . ?
O12 Mn2 K1 46.88(12) . . ?
F1 Mn2 K1 139.26(11) . 3_665 ?
F1 Mn2 K1 40.74(11) 3_665 3_665 ?
O11 Mn2 K1 87.21(14) . 3_665 ?
O11 Mn2 K1 92.79(14) 3_665 3_665 ?
O12 Mn2 K1 46.88(12) 3_665 3_665 ?
O12 Mn2 K1 133.12(12) . 3_665 ?
K1 Mn2 K1 180.00(3) . 3_665 ?
F1 Mn2 K1 92.71(11) . 2_544 ?
F1 Mn2 K1 87.29(11) 3_665 2_544 ?
O11 Mn2 K1 135.15(14) . 2_544 ?
O11 Mn2 K1 44.85(14) 3_665 2_544 ?
O12 Mn2 K1 44.98(12) 3_665 2_544 ?
O12 Mn2 K1 135.02(12) . 2_544 ?
K1 Mn2 K1 116.952(13) . 2_544 ?
K1 Mn2 K1 63.048(13) 3_665 2_544 ?
F1 Mn2 K1 87.29(11) . 4_676 ?
F1 Mn2 K1 92.71(11) 3_665 4_676 ?
O11 Mn2 K1 44.85(14) . 4_676 ?
O11 Mn2 K1 135.15(14) 3_665 4_676 ?
O12 Mn2 K1 135.02(12) 3_665 4_676 ?
O12 Mn2 K1 44.98(12) . 4_676 ?
K1 Mn2 K1 63.048(13) . 4_676 ?
K1 Mn2 K1 116.952(13) 3_665 4_676 ?
K1 Mn2 K1 180.00(4) 2_544 4_676 ?
F2 Mn3 F2 180.0 . 3_664 ?
F2 Mn3 O10 91.20(18) . 1_554 ?
F2 Mn3 O10 88.80(18) 3_664 1_554 ?
F2 Mn3 O10 88.80(18) . 3_665 ?
F2 Mn3 O10 91.20(18) 3_664 3_665 ?
O10 Mn3 O10 180.0(3) 1_554 3_665 ?
F2 Mn3 F1 92.10(16) . 3_664 ?
F2 Mn3 F1 87.90(16) 3_664 3_664 ?
O10 Mn3 F1 87.81(17) 1_554 3_664 ?
O10 Mn3 F1 92.19(17) 3_665 3_664 ?
F2 Mn3 F1 87.90(16) . . ?
F2 Mn3 F1 92.10(16) 3_664 . ?
O10 Mn3 F1 92.19(17) 1_554 . ?
O10 Mn3 F1 87.81(17) 3_665 . ?
F1 Mn3 F1 180.00(18) 3_664 . ?
F2 Mn3 K1 141.45(12) . 3_564 ?
F2 Mn3 K1 38.55(12) 3_664 3_564 ?
O10 Mn3 K1 51.64(14) 1_554 3_564 ?
O10 Mn3 K1 128.36(14) 3_665 3_564 ?
F1 Mn3 K1 78.26(10) 3_664 3_564 ?
F1 Mn3 K1 101.74(10) . 3_564 ?
F2 Mn3 K1 38.55(12) . 1_655 ?
F2 Mn3 K1 141.45(12) 3_664 1_655 ?
O10 Mn3 K1 128.36(14) 1_554 1_655 ?
O10 Mn3 K1 51.64(14) 3_665 1_655 ?
F1 Mn3 K1 101.74(10) 3_664 1_655 ?
F1 Mn3 K1 78.26(10) . 1_655 ?
K1 Mn3 K1 180.00(5) 3_564 1_655 ?
F2 Mn3 K1 107.38(12) . 3_664 ?
F2 Mn3 K1 72.62(12) 3_664 3_664 ?
O10 Mn3 K1 120.25(14) 1_554 3_664 ?
O10 Mn3 K1 59.75(14) 3_665 3_664 ?
F1 Mn3 K1 37.13(10) 3_664 3_664 ?
F1 Mn3 K1 142.87(10) . 3_664 ?
K1 Mn3 K1 87.23(3) 3_564 3_664 ?
K1 Mn3 K1 92.77(3) 1_655 3_664 ?
F2 Mn3 K1 72.62(12) . . ?
F2 Mn3 K1 107.38(12) 3_664 . ?
O10 Mn3 K1 59.75(14) 1_554 . ?
O10 Mn3 K1 120.25(14) 3_665 . ?
F1 Mn3 K1 142.87(10) 3_664 . ?
F1 Mn3 K1 37.13(10) . . ?
K1 Mn3 K1 92.77(3) 3_564 . ?
K1 Mn3 K1 87.23(3) 1_655 . ?
K1 Mn3 K1 180.0 3_664 . ?
O12 P2 O11 113.9(3) . 1_455 ?
O12 P2 O10 114.8(3) . . ?
O11 P2 O10 113.4(3) 1_455 . ?
O12 P2 F3 106.9(2) . . ?
O11 P2 F3 101.7(2) 1_455 . ?
O10 P2 F3 104.5(2) . . ?
O12 P2 K1 52.13(18) . 4_676 ?
O11 P2 K1 132.88(19) 1_455 4_676 ?
O10 P2 K1 112.53(18) . 4_676 ?
F3 P2 K1 56.60(15) . 4_676 ?
O12 P2 K1 124.53(19) . 4_576 ?
O11 P2 K1 50.13(18) 1_455 4_576 ?
O10 P2 K1 119.92(19) . 4_576 ?
F3 P2 K1 51.61(15) . 4_576 ?
K1 P2 K1 97.12(5) 4_676 4_576 ?
O12 P2 K1 38.30(18) . . ?
O11 P2 K1 79.03(18) 1_455 . ?
O10 P2 K1 148.83(19) . . ?
F3 P2 K1 100.35(16) . . ?
K1 P2 K1 66.90(4) 4_676 . ?
K1 P2 K1 90.33(4) 4_576 . ?
 
_diffrn_measured_fraction_theta_max    0.992
_diffrn_reflns_theta_full              27.58
_diffrn_measured_fraction_theta_full   0.992
_refine_diff_density_max    0.822
_refine_diff_density_min   -0.691
_refine_diff_density_rms    0.198

