data_2012wql277_p21c

_audit_update_record
;
2012-07-12 # Formatted by publCIF
;
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'F4 Li3 Mn O6 P2'
_chemical_formula_weight          309.70
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Li'  'Li'  -0.0003   0.0001
 '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/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                    6.333(5)
_cell_length_b                    7.395(5)
_cell_length_c                    7.575(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.947(11)
_cell_angle_gamma                 90.00
_cell_volume                      354.7(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     1447
_cell_measurement_theta_min       2.7
_cell_measurement_theta_max       31.5
 
_exptl_crystal_description        plate
_exptl_crystal_colour             brown
_exptl_crystal_size_max           0.02
_exptl_crystal_size_mid           0.01
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.900
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              226
_exptl_absorpt_coefficient_mu     2.395
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9726
_exptl_absorpt_correction_T_max   0.9862
_exptl_absorpt_process_details    ?
 
_exptl_special_details
?
 
_diffrn_special_details
;
 ?
;
_diffrn_ambient_temperature             100
_diffrn_source_power                    2.5
_diffrn_source_voltage                  45.0
_diffrn_source_current                  55.0
_diffrn_radiation_wavelength            0.71075
_diffrn_radiation_type                  'Molybdenum'
_diffrn_source                          'Rotating Anode'
_diffrn_radiation_monochromator         'Confocal'
_diffrn_measurement_specimen_support    'Mitegen'
_diffrn_detector                        'CCD'
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean        28.5714
_diffrn_measurement_method              'profile data from ω-scans'
_diffrn_reflns_number                   0
_diffrn_reflns_av_R_equivalents         0.052
_diffrn_reflns_av_unetI/netI            0.056
_diffrn_reflns_theta_min                2.7
_diffrn_reflns_theta_max                31.5
_diffrn_reflns_limit_h_min              -9
_diffrn_reflns_limit_h_max              8
_diffrn_reflns_limit_k_min              -10
_diffrn_reflns_limit_k_max              10
_diffrn_reflns_limit_l_min              -10
_diffrn_reflns_limit_l_max              11
_diffrn_measurement_details
;
scan:
	Number of images: 128
	           Slice: -110.0000 - 18.0000
	     Image width: 1.0000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -70.0000
	             Phi: 180.0000
	             XTD: 45.0017
	          2theta: -20.1070
scan:
	Number of images: 117
	           Slice: -110.0000 - 7.0000
	     Image width: 1.0000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -70.0000
	             Phi: 45.0000
	             XTD: 45.0017
	          2theta: -20.1070
scan:
	Number of images: 94
	           Slice: -84.0000 - 10.0000
	     Image width: 1.0000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -70.0000
	             Phi: 270.0000
	             XTD: 45.0017
	          2theta: -20.1070
scan:
	Number of images: 34
	           Slice: -110.0000 - -76.0000
	     Image width: 1.0000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 270.0000
	             XTD: 45.0017
	          2theta: -20.1070
scan:
	Number of images: 30
	           Slice: -100.0000 - -70.0000
	     Image width: 1.0000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 315.0000
	             XTD: 45.0017
	          2theta: -20.1070

;
_diffrn_orient_matrix_UB_11             -0.045944
_diffrn_orient_matrix_UB_12             -0.149413
_diffrn_orient_matrix_UB_13             -0.022509
_diffrn_orient_matrix_UB_21             0.085253
_diffrn_orient_matrix_UB_22             -0.010481
_diffrn_orient_matrix_UB_23             -0.104440
_diffrn_orient_matrix_UB_31             0.094371
_diffrn_orient_matrix_UB_32             -0.043590
_diffrn_orient_matrix_UB_33             0.081408
_diffrn_orient_matrix_type              'd*Trek'


_reflns_number_total              1082
_reflns_number_gt                 887
_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)+(0.0655P)²+3.0155P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    '.'
_refine_ls_hydrogen_treatment     '.'
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          1082
_refine_ls_number_parameters      76
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0633
_refine_ls_R_factor_gt            0.0456
_refine_ls_wR_factor_ref          0.1174
_refine_ls_wR_factor_gt           0.1028
_refine_ls_goodness_of_fit_ref    0.816
_refine_ls_restrained_S_all       0.816
_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
F5 F 0.2301(3) 0.1110(3) 0.6115(3) 0.0084(4) Uani 1 1 d . . .
Li1 Li 0.2595(11) 0.2638(11) 0.3245(11) 0.0199(15) Uani 1 1 d . . .
Li2 Li 0.5000 0.0000 0.5000 0.0127(18) Uani 1 2 d S . .
Mn1 Mn 0.0000 0.0000 0.5000 0.0064(2) Uani 1 2 d S . .
P1 P 0.25097(14) 0.65974(13) 0.63886(12) 0.0068(2) Uani 1 1 d . . .
F1 F 0.2384(4) 0.5269(3) 0.4780(3) 0.0129(5) Uani 1 1 d . . .
O3 O 0.2357(4) -0.0405(4) 0.2996(3) 0.0094(5) Uani 1 1 d . . .
O4 O -0.0506(4) 0.2253(4) 0.3836(3) 0.0086(5) Uani 1 1 d . . .
O2 O 0.5503(4) 0.2369(4) 0.3794(3) 0.0097(5) 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
F5 Mn1 1.862(2) . ?
F5 Li1 1.867(8) 4_566 ?
F5 Li2 2.087(2) . ?
F5 Li1 2.460(8) . ?
Li1 F5 1.867(8) 4_565 ?
Li1 O2 1.891(8) . ?
Li1 O4 2.042(8) . ?
Li1 O3 2.263(9) . ?
Li1 F1 2.272(9) . ?
Li1 Li2 2.797(7) . ?
Li1 Mn1 2.889(8) . ?
Li1 Li2 3.396(8) 2_655 ?
Li2 O2 2.004(3) 3_656 ?
Li2 O2 2.004(3) . ?
Li2 F5 2.087(2) 3_656 ?
Li2 O3 2.261(3) 3_656 ?
Li2 O3 2.261(3) . ?
Li2 Li1 2.797(7) 3_656 ?
Li2 Mn1 3.166(2) . ?
Li2 Mn1 3.166(2) 1_655 ?
Li2 Li1 3.396(8) 4_566 ?
Li2 Li1 3.396(8) 2_645 ?
Mn1 F5 1.862(2) 3_556 ?
Mn1 O4 1.909(3) 3_556 ?
Mn1 O4 1.909(3) . ?
Mn1 O3 2.168(3) 3_556 ?
Mn1 O3 2.168(3) . ?
Mn1 Li1 2.889(8) 3_556 ?
Mn1 Li2 3.166(2) 1_455 ?
P1 O2 1.481(3) 3_666 ?
P1 O3 1.507(3) 4_566 ?
P1 O4 1.535(3) 3_566 ?
P1 F1 1.566(3) . ?
O3 P1 1.507(3) 4_565 ?
O4 P1 1.535(3) 3_566 ?
O2 P1 1.481(3) 3_666 ?
 
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
Mn1 F5 Li1 132.6(3) . 4_566 ?
Mn1 F5 Li2 106.45(11) . . ?
Li1 F5 Li2 118.3(2) 4_566 . ?
Mn1 F5 Li1 82.6(2) . . ?
Li1 F5 Li1 121.86(14) 4_566 . ?
Li2 F5 Li1 75.43(19) . . ?
F5 Li1 O2 109.0(4) 4_565 . ?
F5 Li1 O4 100.1(3) 4_565 . ?
O2 Li1 O4 150.9(5) . . ?
F5 Li1 O3 114.6(4) 4_565 . ?
O2 Li1 O3 88.7(3) . . ?
O4 Li1 O3 79.4(3) . . ?
F5 Li1 F1 90.7(3) 4_565 . ?
O2 Li1 F1 92.5(3) . . ?
O4 Li1 F1 86.7(3) . . ?
O3 Li1 F1 152.9(4) . . ?
F5 Li1 F5 169.6(4) 4_565 . ?
O2 Li1 F5 81.1(3) . . ?
O4 Li1 F5 69.8(2) . . ?
O3 Li1 F5 67.1(2) . . ?
F1 Li1 F5 86.3(3) . . ?
F5 Li1 Li2 143.4(4) 4_565 . ?
O2 Li1 Li2 45.72(18) . . ?
O4 Li1 Li2 108.5(3) . . ?
O3 Li1 Li2 51.77(17) . . ?
F1 Li1 Li2 113.0(3) . . ?
F5 Li1 Li2 46.23(14) . . ?
F5 Li1 Mn1 133.1(3) 4_565 . ?
O2 Li1 Mn1 112.8(3) . . ?
O4 Li1 Mn1 41.25(16) . . ?
O3 Li1 Mn1 47.88(16) . . ?
F1 Li1 Mn1 107.7(3) . . ?
F5 Li1 Mn1 39.74(12) . . ?
Li2 Li1 Mn1 67.65(18) . . ?
F5 Li1 Li2 32.76(16) 4_565 2_655 ?
O2 Li1 Li2 76.5(2) . 2_655 ?
O4 Li1 Li2 132.5(3) . 2_655 ?
O3 Li1 Li2 118.8(3) . 2_655 ?
F1 Li1 Li2 87.8(2) . 2_655 ?
F5 Li1 Li2 156.5(3) . 2_655 ?
Li2 Li1 Li2 117.1(2) . 2_655 ?
Mn1 Li1 Li2 161.0(3) . 2_655 ?
O2 Li2 O2 180.0 3_656 . ?
O2 Li2 F5 91.26(10) 3_656 . ?
O2 Li2 F5 88.74(10) . . ?
O2 Li2 F5 88.74(10) 3_656 3_656 ?
O2 Li2 F5 91.26(10) . 3_656 ?
F5 Li2 F5 180.00(11) . 3_656 ?
O2 Li2 O3 86.06(10) 3_656 3_656 ?
O2 Li2 O3 93.94(10) . 3_656 ?
F5 Li2 O3 106.16(10) . 3_656 ?
F5 Li2 O3 73.84(10) 3_656 3_656 ?
O2 Li2 O3 93.94(10) 3_656 . ?
O2 Li2 O3 86.06(10) . . ?
F5 Li2 O3 73.84(10) . . ?
F5 Li2 O3 106.16(10) 3_656 . ?
O3 Li2 O3 180.0 3_656 . ?
O2 Li2 Li1 137.48(17) 3_656 . ?
O2 Li2 Li1 42.52(17) . . ?
F5 Li2 Li1 58.34(18) . . ?
F5 Li2 Li1 121.66(18) 3_656 . ?
O3 Li2 Li1 128.15(19) 3_656 . ?
O3 Li2 Li1 51.85(18) . . ?
O2 Li2 Li1 42.52(17) 3_656 3_656 ?
O2 Li2 Li1 137.48(17) . 3_656 ?
F5 Li2 Li1 121.66(18) . 3_656 ?
F5 Li2 Li1 58.34(18) 3_656 3_656 ?
O3 Li2 Li1 51.85(18) 3_656 3_656 ?
O3 Li2 Li1 128.15(19) . 3_656 ?
Li1 Li2 Li1 180.000(1) . 3_656 ?
O2 Li2 Mn1 80.42(7) 3_656 . ?
O2 Li2 Mn1 99.58(7) . . ?
F5 Li2 Mn1 34.34(6) . . ?
F5 Li2 Mn1 145.66(6) 3_656 . ?
O3 Li2 Mn1 136.81(7) 3_656 . ?
O3 Li2 Mn1 43.19(7) . . ?
Li1 Li2 Mn1 57.55(15) . . ?
Li1 Li2 Mn1 122.45(15) 3_656 . ?
O2 Li2 Mn1 99.58(7) 3_656 1_655 ?
O2 Li2 Mn1 80.42(7) . 1_655 ?
F5 Li2 Mn1 145.66(6) . 1_655 ?
F5 Li2 Mn1 34.34(6) 3_656 1_655 ?
O3 Li2 Mn1 43.19(7) 3_656 1_655 ?
O3 Li2 Mn1 136.81(7) . 1_655 ?
Li1 Li2 Mn1 122.45(15) . 1_655 ?
Li1 Li2 Mn1 57.55(15) 3_656 1_655 ?
Mn1 Li2 Mn1 180.0 . 1_655 ?
O2 Li2 Li1 92.48(17) 3_656 4_566 ?
O2 Li2 Li1 87.52(17) . 4_566 ?
F5 Li2 Li1 28.95(13) . 4_566 ?
F5 Li2 Li1 151.05(13) 3_656 4_566 ?
O3 Li2 Li1 77.38(14) 3_656 4_566 ?
O3 Li2 Li1 102.62(14) . 4_566 ?
Li1 Li2 Li1 74.82(12) . 4_566 ?
Li1 Li2 Li1 105.18(12) 3_656 4_566 ?
Mn1 Li2 Li1 62.59(12) . 4_566 ?
Mn1 Li2 Li1 117.41(12) 1_655 4_566 ?
O2 Li2 Li1 87.52(17) 3_656 2_645 ?
O2 Li2 Li1 92.48(17) . 2_645 ?
F5 Li2 Li1 151.05(13) . 2_645 ?
F5 Li2 Li1 28.95(13) 3_656 2_645 ?
O3 Li2 Li1 102.62(14) 3_656 2_645 ?
O3 Li2 Li1 77.38(14) . 2_645 ?
Li1 Li2 Li1 105.18(12) . 2_645 ?
Li1 Li2 Li1 74.82(12) 3_656 2_645 ?
Mn1 Li2 Li1 117.41(12) . 2_645 ?
Mn1 Li2 Li1 62.59(12) 1_655 2_645 ?
Li1 Li2 Li1 180.0 4_566 2_645 ?
F5 Mn1 F5 180.0 . 3_556 ?
F5 Mn1 O4 92.93(11) . 3_556 ?
F5 Mn1 O4 87.07(11) 3_556 3_556 ?
F5 Mn1 O4 87.07(11) . . ?
F5 Mn1 O4 92.93(11) 3_556 . ?
O4 Mn1 O4 180.0 3_556 . ?
F5 Mn1 O3 99.45(11) . 3_556 ?
F5 Mn1 O3 80.55(11) 3_556 3_556 ?
O4 Mn1 O3 84.81(11) 3_556 3_556 ?
O4 Mn1 O3 95.19(11) . 3_556 ?
F5 Mn1 O3 80.55(11) . . ?
F5 Mn1 O3 99.45(10) 3_556 . ?
O4 Mn1 O3 95.19(11) 3_556 . ?
O4 Mn1 O3 84.81(11) . . ?
O3 Mn1 O3 180.0 3_556 . ?
F5 Mn1 Li1 122.39(17) . 3_556 ?
F5 Mn1 Li1 57.61(17) 3_556 3_556 ?
O4 Mn1 Li1 44.83(17) 3_556 3_556 ?
O4 Mn1 Li1 135.17(17) . 3_556 ?
O3 Mn1 Li1 50.76(19) 3_556 3_556 ?
O3 Mn1 Li1 129.24(19) . 3_556 ?
F5 Mn1 Li1 57.61(17) . . ?
F5 Mn1 Li1 122.39(17) 3_556 . ?
O4 Mn1 Li1 135.17(17) 3_556 . ?
O4 Mn1 Li1 44.83(17) . . ?
O3 Mn1 Li1 129.24(19) 3_556 . ?
O3 Mn1 Li1 50.76(19) . . ?
Li1 Mn1 Li1 180.0(2) 3_556 . ?
F5 Mn1 Li2 39.21(7) . . ?
F5 Mn1 Li2 140.79(7) 3_556 . ?
O4 Mn1 Li2 80.79(8) 3_556 . ?
O4 Mn1 Li2 99.21(8) . . ?
O3 Mn1 Li2 134.45(7) 3_556 . ?
O3 Mn1 Li2 45.55(7) . . ?
Li1 Mn1 Li2 125.21(14) 3_556 . ?
Li1 Mn1 Li2 54.79(14) . . ?
F5 Mn1 Li2 140.79(7) . 1_455 ?
F5 Mn1 Li2 39.21(7) 3_556 1_455 ?
O4 Mn1 Li2 99.21(8) 3_556 1_455 ?
O4 Mn1 Li2 80.79(8) . 1_455 ?
O3 Mn1 Li2 45.55(7) 3_556 1_455 ?
O3 Mn1 Li2 134.45(7) . 1_455 ?
Li1 Mn1 Li2 54.79(14) 3_556 1_455 ?
Li1 Mn1 Li2 125.21(14) . 1_455 ?
Li2 Mn1 Li2 180.0 . 1_455 ?
O2 P1 O3 116.31(15) 3_666 4_566 ?
O2 P1 O4 113.97(16) 3_666 3_566 ?
O3 P1 O4 110.47(15) 4_566 3_566 ?
O2 P1 F1 106.45(15) 3_666 . ?
O3 P1 F1 104.98(16) 4_566 . ?
O4 P1 F1 103.28(14) 3_566 . ?
P1 F1 Li1 158.9(2) . . ?
P1 O3 Mn1 134.47(16) 4_565 . ?
P1 O3 Li2 124.29(15) 4_565 . ?
Mn1 O3 Li2 91.26(11) . . ?
P1 O3 Li1 130.1(3) 4_565 . ?
Mn1 O3 Li1 81.4(2) . . ?
Li2 O3 Li1 76.4(2) . . ?
P1 O4 Mn1 131.81(16) 3_566 . ?
P1 O4 Li1 134.0(3) 3_566 . ?
Mn1 O4 Li1 93.9(2) . . ?
P1 O2 Li1 138.7(3) 3_666 . ?
P1 O2 Li2 129.47(16) 3_666 . ?
Li1 O2 Li2 91.8(3) . . ?
 
_diffrn_measured_fraction_theta_max    0.916
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   1.000
_refine_diff_density_max    0.694
_refine_diff_density_min   -0.939
_refine_diff_density_rms    0.185

