data_2010jaa0013_p21c

_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
 'F2 H3 Mn O8 P2 Rb2'
_chemical_formula_weight          456.84
 
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'
 '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'
 'Rb'  'Rb'  -0.9393   2.9676
 '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'
 'H'  'H'   0.0000   0.0000
 '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/c
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    7.3481(2)
_cell_length_b                    7.8143(3)
_cell_length_c                    8.5789(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  114.364(2)
_cell_angle_gamma                 90.00
_cell_volume                      448.73(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3113
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        brown
_exptl_crystal_colour             'irregular plates'
_exptl_crystal_size_max           0.05
_exptl_crystal_size_mid           0.03
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.381
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              327
_exptl_absorpt_coefficient_mu     12.660
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6226
_exptl_absorpt_correction_T_max   0.8803
_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             4697
_diffrn_reflns_av_R_equivalents   0.0259
_diffrn_reflns_av_sigmaI/netI     0.0258
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          3.04
_diffrn_reflns_theta_max          27.49
_reflns_number_total              1020
_reflns_number_gt                 998
_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+0.9902P] 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          1020
_refine_ls_number_parameters      78
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0183
_refine_ls_R_factor_gt            0.0176
_refine_ls_wR_factor_ref          0.0401
_refine_ls_wR_factor_gt           0.0397
_refine_ls_goodness_of_fit_ref    1.074
_refine_ls_restrained_S_all       1.074
_refine_ls_shift/su_max           0.006
_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
O3 O -0.4218(2) 0.2720(2) -0.0172(2) 0.0096(3) Uani 1 1 d . . .
O4 O -0.1619(3) 0.4844(2) 0.0043(2) 0.0118(4) Uani 1 1 d . . .
H1 H -0.269(6) 0.219(5) -0.276(5) 0.030(10) Uiso 1 1 d . . .
H2 H -0.077(8) 0.489(8) -0.005(8) 0.006(16) Uiso 0.50 1 d P . .
Rb1 Rb 0.13195(3) 0.16329(3) 0.19187(3) 0.00977(9) Uani 1 1 d . . .
Mn1 Mn 0.5000 0.0000 0.0000 0.00621(12) Uani 1 2 d S . .
P1 P -0.32238(9) 0.36388(7) -0.11724(7) 0.00669(13) Uani 1 1 d . . .
F1 F 0.23269(19) 0.05317(17) -0.08368(16) 0.0097(3) Uani 1 1 d . . .
O1 O 0.5217(2) 0.0447(2) 0.22792(19) 0.0093(3) Uani 1 1 d . . .
O2 O -0.2071(3) 0.2322(2) -0.1844(2) 0.0095(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
O3 P1 1.5176(17) . ?
O3 Mn1 2.2228(16) 1_455 ?
O3 Rb1 3.2380(16) 4_465 ?
O4 P1 1.5330(18) . ?
O4 Rb1 2.8850(17) 2 ?
O4 Rb1 3.2680(18) . ?
O4 Rb1 3.2813(18) 3_565 ?
Rb1 F1 2.8264(13) 4_566 ?
Rb1 F1 2.8846(13) . ?
Rb1 O4 2.8850(17) 2_545 ?
Rb1 O1 2.9031(17) . ?
Rb1 F1 2.9749(13) 3 ?
Rb1 O2 3.1449(16) 3 ?
Rb1 O2 3.1908(17) 4_566 ?
Rb1 O2 3.2064(17) . ?
Rb1 O3 3.2380(16) 4_666 ?
Rb1 O4 3.2813(18) 3_565 ?
Rb1 P1 3.6511(6) . ?
Mn1 F1 1.8392(13) . ?
Mn1 F1 1.8392(13) 3_655 ?
Mn1 O1 1.9269(15) 3_655 ?
Mn1 O1 1.9269(15) . ?
Mn1 O3 2.2228(16) 1_655 ?
Mn1 O3 2.2228(16) 3 ?
Mn1 Rb1 3.9147(2) 3_655 ?
Mn1 Rb1 3.9148(2) 2_645 ?
Mn1 Rb1 3.9148(2) 4_565 ?
P1 O1 1.5269(16) 4_465 ?
P1 O2 1.5846(17) . ?
P1 Rb1 3.6588(6) 4_465 ?
P1 Rb1 4.0664(6) 2 ?
F1 Rb1 2.8264(13) 4_565 ?
F1 Rb1 2.9749(13) 3 ?
O1 P1 1.5269(16) 4_666 ?
O2 Rb1 3.1449(16) 3 ?
O2 Rb1 3.1908(17) 4_565 ?
 
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
P1 O3 Mn1 133.45(10) . 1_455 ?
P1 O3 Rb1 93.49(7) . 4_465 ?
Mn1 O3 Rb1 89.60(5) 1_455 4_465 ?
P1 O4 Rb1 131.51(10) . 2 ?
P1 O4 Rb1 91.72(8) . . ?
Rb1 O4 Rb1 97.97(5) 2 . ?
P1 O4 Rb1 111.22(8) . 3_565 ?
Rb1 O4 Rb1 93.47(5) 2 3_565 ?
Rb1 O4 Rb1 136.58(6) . 3_565 ?
F1 Rb1 F1 135.12(4) 4_566 . ?
F1 Rb1 O4 82.16(4) 4_566 2_545 ?
F1 Rb1 O4 130.25(4) . 2_545 ?
F1 Rb1 O1 102.01(4) 4_566 . ?
F1 Rb1 O1 54.31(4) . . ?
O4 Rb1 O1 92.57(5) 2_545 . ?
F1 Rb1 F1 127.40(2) 4_566 3 ?
F1 Rb1 F1 94.43(4) . 3 ?
O4 Rb1 F1 74.31(4) 2_545 3 ?
O1 Rb1 F1 125.01(4) . 3 ?
F1 Rb1 O2 141.76(4) 4_566 3 ?
F1 Rb1 O2 65.39(4) . 3 ?
O4 Rb1 O2 66.02(5) 2_545 3 ?
O1 Rb1 O2 60.96(4) . 3 ?
F1 Rb1 O2 65.03(4) 3 3 ?
F1 Rb1 O2 66.03(4) 4_566 4_566 ?
F1 Rb1 O2 148.05(4) . 4_566 ?
O4 Rb1 O2 66.58(5) 2_545 4_566 ?
O1 Rb1 O2 156.58(4) . 4_566 ?
F1 Rb1 O2 61.51(4) 3 4_566 ?
O2 Rb1 O2 115.21(4) 3 4_566 ?
F1 Rb1 O2 115.50(4) 4_566 . ?
F1 Rb1 O2 65.20(4) . . ?
O4 Rb1 O2 136.79(5) 2_545 . ?
O1 Rb1 O2 118.92(4) . . ?
F1 Rb1 O2 63.62(4) 3 . ?
O2 Rb1 O2 102.39(4) 3 . ?
O2 Rb1 O2 84.43(4) 4_566 . ?
F1 Rb1 O3 56.99(4) 4_566 4_666 ?
F1 Rb1 O3 99.07(4) . 4_666 ?
O4 Rb1 O3 72.76(5) 2_545 4_666 ?
O1 Rb1 O3 47.69(4) . 4_666 ?
F1 Rb1 O3 145.54(4) 3 4_666 ?
O2 Rb1 O3 92.21(4) 3 4_666 ?
O2 Rb1 O3 112.64(4) 4_566 4_666 ?
O2 Rb1 O3 150.34(4) . 4_666 ?
F1 Rb1 O4 70.59(4) 4_566 . ?
F1 Rb1 O4 99.57(4) . . ?
O4 Rb1 O4 127.27(3) 2_545 . ?
O1 Rb1 O4 136.05(5) . . ?
F1 Rb1 O4 87.47(4) 3 . ?
O2 Rb1 O4 146.14(4) 3 . ?
O2 Rb1 O4 61.28(4) 4_566 . ?
O2 Rb1 O4 45.11(4) . . ?
O3 Rb1 O4 120.86(4) 4_666 . ?
F1 Rb1 O4 68.75(4) 4_566 3_565 ?
F1 Rb1 O4 74.68(4) . 3_565 ?
O4 Rb1 O4 150.90(5) 2_545 3_565 ?
O1 Rb1 O4 92.90(5) . 3_565 ?
F1 Rb1 O4 124.01(4) 3 3_565 ?
O2 Rb1 O4 139.88(4) 3 3_565 ?
O2 Rb1 O4 100.53(5) 4_566 3_565 ?
O2 Rb1 O4 62.05(4) . 3_565 ?
O3 Rb1 O4 90.21(4) 4_666 3_565 ?
O4 Rb1 O4 43.42(6) . 3_565 ?
F1 Rb1 P1 93.57(3) 4_566 . ?
F1 Rb1 P1 89.98(3) . . ?
O4 Rb1 P1 124.77(4) 2_545 . ?
O1 Rb1 P1 141.33(3) . . ?
F1 Rb1 P1 65.26(3) 3 . ?
O2 Rb1 P1 121.51(3) 3 . ?
O2 Rb1 P1 61.73(3) 4_566 . ?
O2 Rb1 P1 25.68(3) . . ?
O3 Rb1 P1 145.55(3) 4_666 . ?
O4 Rb1 P1 24.82(3) . . ?
O4 Rb1 P1 60.13(3) 3_565 . ?
F1 Mn1 F1 180.00(9) . 3_655 ?
F1 Mn1 O1 90.96(6) . 3_655 ?
F1 Mn1 O1 89.04(6) 3_655 3_655 ?
F1 Mn1 O1 89.04(6) . . ?
F1 Mn1 O1 90.96(6) 3_655 . ?
O1 Mn1 O1 180.00(13) 3_655 . ?
F1 Mn1 O3 91.24(6) . 1_655 ?
F1 Mn1 O3 88.76(6) 3_655 1_655 ?
O1 Mn1 O3 91.23(6) 3_655 1_655 ?
O1 Mn1 O3 88.77(6) . 1_655 ?
F1 Mn1 O3 88.76(6) . 3 ?
F1 Mn1 O3 91.24(6) 3_655 3 ?
O1 Mn1 O3 88.77(6) 3_655 3 ?
O1 Mn1 O3 91.23(6) . 3 ?
O3 Mn1 O3 180.00(2) 1_655 3 ?
F1 Mn1 Rb1 136.16(4) . 3_655 ?
F1 Mn1 Rb1 43.84(4) 3_655 3_655 ?
O1 Mn1 Rb1 45.31(5) 3_655 3_655 ?
O1 Mn1 Rb1 134.69(5) . 3_655 ?
O3 Mn1 Rb1 92.38(4) 1_655 3_655 ?
O3 Mn1 Rb1 87.62(4) 3 3_655 ?
F1 Mn1 Rb1 43.84(4) . . ?
F1 Mn1 Rb1 136.16(4) 3_655 . ?
O1 Mn1 Rb1 134.69(5) 3_655 . ?
O1 Mn1 Rb1 45.31(5) . . ?
O3 Mn1 Rb1 87.62(4) 1_655 . ?
O3 Mn1 Rb1 92.38(4) 3 . ?
Rb1 Mn1 Rb1 180.0 3_655 . ?
F1 Mn1 Rb1 138.11(4) . 2_645 ?
F1 Mn1 Rb1 41.89(4) 3_655 2_645 ?
O1 Mn1 Rb1 107.96(5) 3_655 2_645 ?
O1 Mn1 Rb1 72.04(5) . 2_645 ?
O3 Mn1 Rb1 124.20(4) 1_655 2_645 ?
O3 Mn1 Rb1 55.80(4) 3 2_645 ?
Rb1 Mn1 Rb1 70.135(4) 3_655 2_645 ?
Rb1 Mn1 Rb1 109.865(4) . 2_645 ?
F1 Mn1 Rb1 41.89(4) . 4_565 ?
F1 Mn1 Rb1 138.11(4) 3_655 4_565 ?
O1 Mn1 Rb1 72.04(5) 3_655 4_565 ?
O1 Mn1 Rb1 107.96(5) . 4_565 ?
O3 Mn1 Rb1 55.80(4) 1_655 4_565 ?
O3 Mn1 Rb1 124.20(4) 3 4_565 ?
Rb1 Mn1 Rb1 109.865(4) 3_655 4_565 ?
Rb1 Mn1 Rb1 70.135(4) . 4_565 ?
Rb1 Mn1 Rb1 180.000(5) 2_645 4_565 ?
O3 P1 O1 110.49(9) . 4_465 ?
O3 P1 O4 108.69(10) . . ?
O1 P1 O4 113.25(10) 4_465 . ?
O3 P1 O2 110.67(9) . . ?
O1 P1 O2 108.02(9) 4_465 . ?
O4 P1 O2 105.63(10) . . ?
O3 P1 Rb1 84.00(7) . . ?
O1 P1 Rb1 164.96(7) 4_465 . ?
O4 P1 Rb1 63.47(7) . . ?
O2 P1 Rb1 61.28(6) . . ?
O3 P1 Rb1 62.05(6) . 4_465 ?
O1 P1 Rb1 49.27(6) 4_465 4_465 ?
O4 P1 Rb1 137.19(8) . 4_465 ?
O2 P1 Rb1 116.82(7) . 4_465 ?
Rb1 P1 Rb1 143.614(17) . 4_465 ?
O3 P1 Rb1 80.34(6) . 2 ?
O1 P1 Rb1 111.61(7) 4_465 2 ?
O4 P1 Rb1 32.09(7) . 2 ?
O2 P1 Rb1 131.47(7) . 2 ?
Rb1 P1 Rb1 73.870(11) . 2 ?
Rb1 P1 Rb1 110.054(15) 4_465 2 ?
Mn1 F1 Rb1 112.36(6) . 4_565 ?
Mn1 F1 Rb1 109.96(5) . . ?
Rb1 F1 Rb1 103.93(4) 4_565 . ?
Mn1 F1 Rb1 132.28(6) . 3 ?
Rb1 F1 Rb1 106.51(4) 4_565 3 ?
Rb1 F1 Rb1 85.57(4) . 3 ?
P1 O1 Mn1 133.31(10) 4_666 . ?
P1 O1 Rb1 107.24(8) 4_666 . ?
Mn1 O1 Rb1 106.53(6) . . ?
P1 O2 Rb1 140.37(9) . 3 ?
P1 O2 Rb1 124.24(8) . 4_565 ?
Rb1 O2 Rb1 94.41(4) 3 4_565 ?
P1 O2 Rb1 93.04(7) . . ?
Rb1 O2 Rb1 77.61(4) 3 . ?
Rb1 O2 Rb1 89.36(4) 4_565 . ?
 
_diffrn_measured_fraction_theta_max    0.994
_diffrn_reflns_theta_full              27.49
_diffrn_measured_fraction_theta_full   0.994
_refine_diff_density_max    0.413
_refine_diff_density_min   -0.516
_refine_diff_density_rms    0.117

