data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. Craig Matthews
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C24 H18 F18 N10 O22 Pb4 S6'
_chemical_formula_weight          2161.60
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 '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'
 'N'  'N'   0.0061   0.0033
 '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'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pb'  'Pb'  -3.3944  10.1111
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Triclinic
_symmetry_space_group_name_H-M    P-1
_symmetry_space_group_name_hall   '-P 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    10.8538(5)
_cell_length_b                    11.3876(7)
_cell_length_c                    12.5537(8)
_cell_angle_alpha                 115.212(2)
_cell_angle_beta                  112.293(3)
_cell_angle_gamma                 94.433(3)
_cell_volume                      1244.87(12)
_cell_formula_units_Z             1
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     5404
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             Orange
_exptl_crystal_size_max           0.12
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.883
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              994
_exptl_absorpt_coefficient_mu     13.890
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.2865
_exptl_absorpt_correction_T_max   0.7686
_exptl_absorpt_process_details    'SORTAV Blessing (1997)'
 
_exptl_special_details
;
 PLEASE NOTE cell_measurement_ fields are not relevant to area detector data,
 the entire data set is used to refine the cell, which is indexed from all
 observed reflections in a 10 degree phi range.
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             22501
_diffrn_reflns_av_R_equivalents   0.0770
_diffrn_reflns_av_sigmaI/netI     0.0701
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          3.18
_diffrn_reflns_theta_max          27.39
_reflns_number_total              5600
_reflns_number_gt                 3988
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection
' DENZO (Otwinowski and Minor, 1997)'
_computing_cell_refinement        
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction         
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'PLATON (Spek, 1990)'
_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 > 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)+(0.0757P)²+6.8520P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          5600
_refine_ls_number_parameters      410
_refine_ls_number_restraints      126
_refine_ls_R_factor_all           0.0864
_refine_ls_R_factor_gt            0.0536
_refine_ls_wR_factor_ref          0.1430
_refine_ls_wR_factor_gt           0.1301
_refine_ls_goodness_of_fit_ref    1.053
_refine_ls_restrained_S_all       1.050
_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
Pb1 Pb 0.75463(4) 0.51301(4) 1.24893(4) 0.03516(16) Uani 1 1 d . . .
Pb2 Pb 1.11984(4) 0.82960(4) 1.43173(4) 0.02991(15) Uani 1 1 d . . .
C1 C 0.7365(11) 0.2155(11) 1.0053(11) 0.029(3) Uani 1 1 d . . .
H1 H 0.6510 0.1883 1.0044 0.035 Uiso 1 1 calc R A .
C2 C 0.7710(11) 0.1237(11) 0.9183(11) 0.029(3) Uani 1 1 d . A .
H2 H 0.7138 0.0328 0.8604 0.035 Uiso 1 1 calc R . .
C3 C 0.8922(12) 0.1669(12) 0.9167(11) 0.037(3) Uani 1 1 d . . .
H3 H 0.9188 0.1059 0.8552 0.045 Uiso 1 1 calc R A .
C4 C 0.9753(12) 0.2991(12) 1.0046(11) 0.033(3) Uani 1 1 d . A .
H4 H 1.0593 0.3293 1.0045 0.039 Uiso 1 1 calc R . .
C5 C 0.9348(10) 0.3857(11) 1.0917(10) 0.025(2) Uani 1 1 d . . .
C6 C 1.0209(10) 0.5265(11) 1.1934(9) 0.024(2) Uani 1 1 d . A .
C7 C 1.3325(11) 0.7369(11) 1.2977(10) 0.025(2) Uani 1 1 d . . .
C8 C 1.4205(9) 0.8749(10) 1.4025(9) 0.019(2) Uani 1 1 d . . .
C9 C 1.4566(11) 1.0643(12) 1.5869(11) 0.033(3) Uani 1 1 d . . .
H9 H 1.4270 1.1139 1.6507 0.039 Uiso 1 1 calc R A .
N1 N 0.8178(9) 0.3443(9) 1.0937(8) 0.0247(19) Uani 1 1 d . A .
N2 N 1.1354(9) 0.5671(9) 1.1908(8) 0.025(2) Uani 1 1 d . . .
N3 N 1.2104(8) 0.6989(8) 1.2907(8) 0.0194(18) Uani 1 1 d . A .
N4 N 1.3742(9) 0.6582(9) 1.2108(8) 0.028(2) Uani 1 1 d . A .
H4A H 1.3192 0.5775 1.1457 0.033 Uiso 1 1 calc R . .
H4B H 1.4565 0.6874 1.2190 0.033 Uiso 1 1 calc R . .
N5 N 1.3800(8) 0.9421(9) 1.4931(8) 0.0249(19) Uani 1 1 d . A .
O1 O 0.9794(7) 0.6000(7) 1.2790(7) 0.0250(16) Uani 1 1 d . A .
O1W O 0.9296(17) 0.4543(16) 1.4097(17) 0.089(5) Uani 0.81(2) 1 d P A 1
O2W O 0.806(7) 0.323(7) 1.331(8) 0.089(5) Uani 0.19(2) 1 d P A 2
C11 C 0.2831(8) 0.1701(9) 0.9214(8) 0.061(4) Uani 1 1 d D A .
O11 O 0.4975(7) 0.3753(9) 1.0438(7) 0.058(3) Uani 1 1 d D A .
O12 O 0.2726(7) 0.4059(8) 0.9466(8) 0.046(2) Uani 1 1 d D A .
O13 O 0.3662(9) 0.2745(9) 0.8067(6) 0.054(3) Uani 1 1 d D A .
F11 F 0.2675(10) 0.1998(10) 1.0285(9) 0.085(3) Uani 1 1 d D . .
F12 F 0.3596(8) 0.0847(8) 0.9098(10) 0.087(3) Uani 1 1 d D . .
F13 F 0.1585(7) 0.1103(9) 0.8170(9) 0.083(3) Uani 1 1 d D . .
S11 S 0.3644(3) 0.3229(3) 0.9316(3) 0.0307(6) Uani 1 1 d D . .
C14 C 0.8954(9) 0.7807(8) 1.6971(8) 0.039(3) Uani 1 1 d D A .
O14 O 0.6916(6) 0.7423(8) 1.4818(8) 0.040(2) Uani 1 1 d D A .
O15 O 0.9163(7) 0.7447(8) 1.4888(7) 0.040(2) Uani 1 1 d D A .
O16 O 0.8750(9) 0.9529(7) 1.6152(8) 0.044(2) Uani 1 1 d D A .
F14 F 0.8391(9) 0.8415(8) 1.7741(7) 0.062(2) Uani 1 1 d D . .
F15 F 1.0327(7) 0.8317(8) 1.7695(7) 0.059(2) Uani 1 1 d D . .
F16 F 0.8628(9) 0.6493(7) 1.6587(8) 0.062(2) Uani 1 1 d D . .
S14 S 0.8367(3) 0.8083(3) 1.5556(3) 0.0289(6) Uani 1 1 d D . .
C17A C 1.4577(12) 0.6556(12) 1.6111(12) 0.042(4) Uani 0.543(4) 1 d PD A 3
O17A O 1.3595(17) 0.7328(15) 1.7783(13) 0.045(4) Uani 0.543(4) 1 d PD A 3
O18A O 1.4566(14) 0.9035(10) 1.7415(14) 0.049(4) Uani 0.543(4) 1 d PD A 3
O19A O 1.2390(12) 0.7311(16) 1.5731(12) 0.042(5) Uani 0.543(4) 1 d PD A 3
F17A F 1.5846(11) 0.6788(16) 1.6998(14) 0.070(4) Uani 0.543(4) 1 d PD A 3
F18A F 1.3898(15) 0.5276(10) 1.5618(16) 0.067(4) Uani 0.543(4) 1 d PD A 3
F19A F 1.4630(17) 0.6703(16) 1.5132(13) 0.065(4) Uani 0.543(4) 1 d PD A 3
S17A S 1.3707(6) 0.7703(5) 1.6863(5) 0.0326(10) Uani 0.543(4) 1 d PD A 3
C17B C 1.4322(13) 0.6649(14) 1.6070(14) 0.042(4) Uani 0.457(4) 1 d PD A 4
O17B O 1.1992(14) 0.5899(12) 1.6010(16) 0.045(4) Uani 0.457(4) 1 d PD . 4
O18B O 1.3755(19) 0.7828(19) 1.8017(10) 0.049(4) Uani 0.457(4) 1 d PD A 4
O19B O 1.2543(19) 0.7996(18) 1.6034(19) 0.042(5) Uani 0.457(4) 1 d PD A 4
F17B F 1.5338(14) 0.7716(16) 1.6524(18) 0.070(4) Uani 0.457(4) 1 d PD A 4
F18B F 1.4867(18) 0.5853(17) 1.6528(19) 0.067(4) Uani 0.457(4) 1 d PD A 4
F19B F 1.3763(18) 0.5974(19) 1.4755(13) 0.065(4) Uani 0.457(4) 1 d PD A 4
S17B S 1.3012(7) 0.7158(7) 1.6597(6) 0.0326(10) Uani 0.457(4) 1 d PD A 4
 
 
_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
Pb1 O1 2.385(7) . ?
Pb1 N1 2.447(8) . ?
Pb1 O17B 2.535(17) 2_768 ?
Pb1 O1W 2.562(16) . ?
Pb1 O11 2.704(6) . ?
Pb1 O15 2.759(7) . ?
Pb2 O19B 2.282(13) . ?
Pb2 N3 2.370(8) . ?
Pb2 O1 2.394(7) . ?
Pb2 O19A 2.502(14) . ?
Pb2 N5 2.676(8) . ?
C1 C2 1.350(15) . ?
C1 N1 1.354(13) . ?
C1 H1 0.9500 . ?
C2 C3 1.380(16) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(16) . ?
C3 H3 0.9500 . ?
C4 C5 1.369(15) . ?
C4 H4 0.9500 . ?
C5 N1 1.333(13) . ?
C5 C6 1.481(14) . ?
C6 N2 1.309(14) . ?
C6 O1 1.311(12) . ?
C7 N3 1.320(13) . ?
C7 N4 1.342(13) . ?
C7 C8 1.472(14) . ?
C8 N5 1.327(12) . ?
C8 C9 1.385(15) 2_878 ?
C9 N5 1.303(14) . ?
C9 C8 1.385(15) 2_878 ?
C9 H9 0.9500 . ?
N2 N3 1.387(11) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
C11 F11 1.321(8) . ?
C11 F12 1.324(8) . ?
C11 F13 1.328(8) . ?
C11 S11 1.819(9) . ?
O11 S11 1.426(6) . ?
O12 S11 1.435(6) . ?
O13 S11 1.432(6) . ?
C14 F14 1.316(9) . ?
C14 F15 1.331(9) . ?
C14 F16 1.331(9) . ?
C14 S14 1.819(9) . ?
O14 S14 1.422(6) . ?
O15 S14 1.450(6) . ?
O16 S14 1.433(7) . ?
C17A F17A 1.317(10) . ?
C17A F18A 1.330(10) . ?
C17A F19A 1.331(10) . ?
C17A S17A 1.819(10) . ?
O17A S17A 1.432(9) . ?
O18A S17A 1.431(8) . ?
O19A S17A 1.443(8) . ?
C17B F17B 1.320(10) . ?
C17B F18B 1.331(10) . ?
C17B F19B 1.331(10) . ?
C17B S17B 1.819(10) . ?
O17B S17B 1.435(9) . ?
O17B Pb1 2.535(17) 2_768 ?
O18B S17B 1.437(9) . ?
O19B S17B 1.430(8) . ?
 
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
O1 Pb1 N1 68.0(3) . . ?
O1 Pb1 O17B 104.0(3) . 2_768 ?
N1 Pb1 O17B 94.5(4) . 2_768 ?
O1 Pb1 O1W 72.6(4) . . ?
N1 Pb1 O1W 81.3(4) . . ?
O17B Pb1 O1W 31.5(5) 2_768 . ?
O1 Pb1 O11 136.9(3) . . ?
N1 Pb1 O11 81.5(3) . . ?
O17B Pb1 O11 108.2(3) 2_768 . ?
O1W Pb1 O11 133.4(4) . . ?
O1 Pb1 O15 66.1(2) . . ?
N1 Pb1 O15 131.2(2) . . ?
O17B Pb1 O15 81.1(3) 2_768 . ?
O1W Pb1 O15 69.9(4) . . ?
O11 Pb1 O15 146.2(2) . . ?
O19B Pb2 N3 94.2(5) . . ?
O19B Pb2 O1 98.2(5) . . ?
N3 Pb2 O1 65.9(2) . . ?
O19B Pb2 O19A 15.4(5) . . ?
N3 Pb2 O19A 85.0(4) . . ?
O1 Pb2 O19A 83.2(4) . . ?
O19B Pb2 N5 76.0(5) . . ?
N3 Pb2 N5 63.8(3) . . ?
O1 Pb2 N5 128.7(2) . . ?
O19A Pb2 N5 83.0(4) . . ?
C2 C1 N1 123.2(10) . . ?
C2 C1 H1 118.4 . . ?
N1 C1 H1 118.4 . . ?
C1 C2 C3 117.5(10) . . ?
C1 C2 H2 121.2 . . ?
C3 C2 H2 121.2 . . ?
C2 C3 C4 119.9(11) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 119.2(10) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N1 C5 C4 121.0(10) . . ?
N1 C5 C6 116.3(9) . . ?
C4 C5 C6 122.6(9) . . ?
N2 C6 O1 125.0(9) . . ?
N2 C6 C5 116.1(9) . . ?
O1 C6 C5 118.8(9) . . ?
N3 C7 N4 122.8(10) . . ?
N3 C7 C8 116.7(8) . . ?
N4 C7 C8 120.4(9) . . ?
N5 C8 C9 119.0(9) . 2_878 ?
N5 C8 C7 117.2(9) . . ?
C9 C8 C7 123.7(9) 2_878 . ?
N5 C9 C8 122.8(10) . 2_878 ?
N5 C9 H9 118.6 . . ?
C8 C9 H9 118.6 2_878 . ?
C5 N1 C1 119.0(9) . . ?
C5 N1 Pb1 117.3(7) . . ?
C1 N1 Pb1 123.6(7) . . ?
C6 N2 N3 112.2(8) . . ?
C7 N3 N2 112.9(8) . . ?
C7 N3 Pb2 126.6(6) . . ?
N2 N3 Pb2 120.5(6) . . ?
C7 N4 H4A 120.0 . . ?
C7 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C9 N5 C8 118.1(9) . . ?
C9 N5 Pb2 126.0(7) . . ?
C8 N5 Pb2 114.5(6) . . ?
C6 O1 Pb1 118.8(6) . . ?
C6 O1 Pb2 116.1(6) . . ?
Pb1 O1 Pb2 124.1(3) . . ?
F11 C11 F12 108.5(7) . . ?
F11 C11 F13 108.3(7) . . ?
F12 C11 F13 109.1(7) . . ?
F11 C11 S11 110.6(6) . . ?
F12 C11 S11 110.7(6) . . ?
F13 C11 S11 109.5(6) . . ?
S11 O11 Pb1 169.6(6) . . ?
O11 S11 O13 115.3(5) . . ?
O11 S11 O12 114.7(5) . . ?
O13 S11 O12 112.9(5) . . ?
O11 S11 C11 104.3(5) . . ?
O13 S11 C11 103.5(5) . . ?
O12 S11 C11 104.4(4) . . ?
F14 C14 F15 107.4(8) . . ?
F14 C14 F16 108.6(8) . . ?
F15 C14 F16 108.2(8) . . ?
F14 C14 S14 110.7(6) . . ?
F15 C14 S14 110.5(6) . . ?
F16 C14 S14 111.3(6) . . ?
S14 O15 Pb1 112.9(4) . . ?
O14 S14 O16 115.6(5) . . ?
O14 S14 O15 113.7(5) . . ?
O16 S14 O15 113.9(5) . . ?
O14 S14 C14 105.3(5) . . ?
O16 S14 C14 103.3(4) . . ?
O15 S14 C14 103.1(4) . . ?
F17A C17A F18A 107.4(11) . . ?
F17A C17A F19A 109.5(11) . . ?
F18A C17A F19A 108.4(11) . . ?
F17A C17A S17A 110.6(9) . . ?
F18A C17A S17A 110.6(8) . . ?
F19A C17A S17A 110.2(9) . . ?
S17A O19A Pb2 136.8(10) . . ?
O18A S17A O17A 116.5(8) . . ?
O18A S17A O19A 114.8(9) . . ?
O17A S17A O19A 113.0(9) . . ?
O18A S17A C17A 105.4(7) . . ?
O17A S17A C17A 103.6(7) . . ?
O19A S17A C17A 101.2(7) . . ?
F17B C17B F18B 108.1(12) . . ?
F17B C17B F19B 108.6(12) . . ?
F18B C17B F19B 108.6(11) . . ?
F17B C17B S17B 110.9(9) . . ?
F18B C17B S17B 110.2(9) . . ?
F19B C17B S17B 110.5(9) . . ?
S17B O17B Pb1 112.7(9) . 2_768 ?
S17B O19B Pb2 152.1(13) . . ?
O19B S17B O17B 113.9(9) . . ?
O19B S17B O18B 116.1(10) . . ?
O17B S17B O18B 114.1(9) . . ?
O19B S17B C17B 103.1(8) . . ?
O17B S17B C17B 103.6(7) . . ?
O18B S17B C17B 103.9(8) . . ?
 
_diffrn_measured_fraction_theta_max    0.992
_diffrn_reflns_theta_full              27.39
_diffrn_measured_fraction_theta_full   0.992
_refine_diff_density_max    3.586
_refine_diff_density_min   -2.632
_refine_diff_density_rms    0.288
