data_2010jaa0012_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 H4 Mn N O3 P'
_chemical_formula_weight          208.95
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'N'  'N'   0.0061   0.0033
 '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'
 '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'
 '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                    5.3999(2)
_cell_length_b                    13.1644(6)
_cell_length_c                    7.4117(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  107.501(3)
_cell_angle_gamma                 90.00
_cell_volume                      502.48(4)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     8098
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        plate
_exptl_crystal_colour             brown
_exptl_crystal_size_max           0.05
_exptl_crystal_size_mid           0.03
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.762
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              324
_exptl_absorpt_coefficient_mu     2.949
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8976
_exptl_absorpt_correction_T_max   0.9729
_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             6305
_diffrn_reflns_av_R_equivalents   0.0561
_diffrn_reflns_av_sigmaI/netI     0.0356
_diffrn_reflns_limit_h_min        -6
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        9
_diffrn_reflns_theta_min          3.09
_diffrn_reflns_theta_max          27.52
_reflns_number_total              1147
_reflns_number_gt                 1038
_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)+(0.0225P)²+1.7630P] 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          1147
_refine_ls_number_parameters      101
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0342
_refine_ls_R_factor_gt            0.0292
_refine_ls_wR_factor_ref          0.0714
_refine_ls_wR_factor_gt           0.0677
_refine_ls_goodness_of_fit_ref    0.964
_refine_ls_restrained_S_all       0.964
_refine_ls_shift/su_max           0.001
_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
F1 F 0.0950(3) 0.62898(12) 0.9601(2) 0.0129(3) Uani 1 1 d . . .
O1 O 0.2847(3) 0.39487(14) 0.4472(3) 0.0107(4) Uani 1 1 d . . .
N1 N 0.4493(5) 0.2973(2) 0.8130(3) 0.0129(5) Uani 1 1 d . . .
O2 O 0.6481(3) 0.52866(14) 0.8504(2) 0.0112(4) Uani 1 1 d . . .
H1 H 0.436(8) 0.237(4) 0.816(6) 0.035(12) Uiso 1 1 d . . .
H2 H 0.600(8) 0.325(3) 0.890(6) 0.031(10) Uiso 1 1 d . . .
H3 H 0.442(8) 0.308(3) 0.691(7) 0.044(12) Uiso 1 1 d . . .
H4 H 0.330(9) 0.333(4) 0.838(6) 0.050(13) Uiso 1 1 d . . .
Mn1 Mn 0.0000 0.5000 0.5000 0.00739(15) Uani 1 2 d S . .
P1 P 0.55664(12) 0.60340(5) 0.68804(9) 0.00849(17) Uani 1 1 d . . .
Mn2 Mn 0.0000 0.5000 1.0000 0.00810(16) Uani 1 2 d S . .
F2 F 0.5889(3) 0.71133(12) 0.7826(2) 0.0133(3) Uani 1 1 d . . .
F3 F 0.0669(3) 0.44657(11) 0.7416(2) 0.0114(3) Uani 1 1 d . . .
O3 O 0.2656(3) 0.59982(13) 0.5926(2) 0.0104(4) Uani 1 1 d . . .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
F1 0.0131(8) 0.0127(7) 0.0113(7) 0.0019(6) 0.0013(6) -0.0014(6)
O1 0.0097(9) 0.0128(9) 0.0113(8) 0.0015(7) 0.0055(7) 0.0018(7)
N1 0.0123(12) 0.0120(12) 0.0132(12) -0.0004(9) 0.0022(9) -0.0008(9)
O2 0.0089(9) 0.0150(9) 0.0097(9) 0.0024(7) 0.0025(7) 0.0002(7)
Mn1 0.0068(3) 0.0091(3) 0.0061(3) 0.00054(18) 0.0017(2) -0.00004(19)
P1 0.0076(3) 0.0103(3) 0.0076(3) -0.0006(2) 0.0023(2) 0.0004(2)
Mn2 0.0075(3) 0.0096(3) 0.0066(3) 0.00087(18) 0.0012(2) -0.00011(19)
F2 0.0133(8) 0.0112(7) 0.0154(8) -0.0031(6) 0.0041(6) -0.0005(6)
F3 0.0123(7) 0.0132(7) 0.0084(7) 0.0021(6) 0.0029(6) 0.0025(6)
O3 0.0079(9) 0.0112(9) 0.0117(9) 0.0003(7) 0.0024(7) 0.0008(7)
 
_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
F1 Mn2 1.8235(15) . ?
O1 P1 1.5019(18) 3_666 ?
O1 Mn1 2.1896(18) . ?
O2 P1 1.5174(19) . ?
O2 Mn2 1.9277(18) 1_655 ?
Mn1 F3 1.8554(14) . ?
Mn1 F3 1.8554(14) 3_566 ?
Mn1 O3 1.9138(18) 3_566 ?
Mn1 O3 1.9138(18) . ?
Mn1 O1 2.1896(18) 3_566 ?
P1 O1 1.5019(18) 3_666 ?
P1 O3 1.5178(19) . ?
P1 F2 1.5706(16) . ?
Mn2 F1 1.8235(15) 3_567 ?
Mn2 O2 1.9277(18) 3_667 ?
Mn2 O2 1.9277(18) 1_455 ?
Mn2 F3 2.1701(14) . ?
Mn2 F3 2.1701(14) 3_567 ?
 
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 O1 Mn1 132.98(11) 3_666 . ?
P1 O2 Mn2 127.77(11) . 1_655 ?
F3 Mn1 F3 180.0 . 3_566 ?
F3 Mn1 O3 89.61(7) . 3_566 ?
F3 Mn1 O3 90.39(7) 3_566 3_566 ?
F3 Mn1 O3 90.39(7) . . ?
F3 Mn1 O3 89.61(7) 3_566 . ?
O3 Mn1 O3 180.00(8) 3_566 . ?
F3 Mn1 O1 89.40(7) . . ?
F3 Mn1 O1 90.60(7) 3_566 . ?
O3 Mn1 O1 89.59(7) 3_566 . ?
O3 Mn1 O1 90.41(7) . . ?
F3 Mn1 O1 90.60(7) . 3_566 ?
F3 Mn1 O1 89.40(7) 3_566 3_566 ?
O3 Mn1 O1 90.41(7) 3_566 3_566 ?
O3 Mn1 O1 89.59(7) . 3_566 ?
O1 Mn1 O1 180.00(9) . 3_566 ?
O1 P1 O2 115.11(11) 3_666 . ?
O1 P1 O3 114.06(11) 3_666 . ?
O2 P1 O3 113.20(10) . . ?
O1 P1 F2 105.97(10) 3_666 . ?
O2 P1 F2 105.48(10) . . ?
O3 P1 F2 101.33(9) . . ?
F1 Mn2 F1 180.0 3_567 . ?
F1 Mn2 O2 90.08(7) 3_567 3_667 ?
F1 Mn2 O2 89.92(7) . 3_667 ?
F1 Mn2 O2 89.92(7) 3_567 1_455 ?
F1 Mn2 O2 90.08(7) . 1_455 ?
O2 Mn2 O2 180.0 3_667 1_455 ?
F1 Mn2 F3 88.34(6) 3_567 . ?
F1 Mn2 F3 91.66(6) . . ?
O2 Mn2 F3 92.71(7) 3_667 . ?
O2 Mn2 F3 87.29(7) 1_455 . ?
F1 Mn2 F3 91.66(6) 3_567 3_567 ?
F1 Mn2 F3 88.34(6) . 3_567 ?
O2 Mn2 F3 87.29(7) 3_667 3_567 ?
O2 Mn2 F3 92.71(7) 1_455 3_567 ?
F3 Mn2 F3 180.000(1) . 3_567 ?
Mn1 F3 Mn2 133.88(8) . . ?
P1 O3 Mn1 138.39(11) . . ?
 
_diffrn_measured_fraction_theta_max    0.993
_diffrn_reflns_theta_full              27.52
_diffrn_measured_fraction_theta_full   0.993
_refine_diff_density_max    0.413
_refine_diff_density_min   -0.501
_refine_diff_density_rms    0.108

