# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2013JEBRWRG08
_database_code_depnum_ccdc_archive 'CCDC 1060048'
_audit_update_record             
;
2015-04-16 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H16 N2 O6 P2 Pb'
_chemical_formula_sum            'C6 H16 N2 O6 P2 Pb'
_chemical_formula_weight         481.34

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'
P P 0.1023 0.0942 '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           Tetragonal
_symmetry_space_group_name_H-M   P41212
_SYMMETRY_SPACE_GROUP_NAME_HALL  P4abw2nw
_SYMMETRY_INT_TABLES_NUMBER      92

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   8.2128(18)
_cell_length_b                   8.2128(18)
_cell_length_c                   20.989(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1415.7(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2906
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Chunk
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    12.159
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.5291
_exptl_absorpt_correction_T_max  0.5816
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6585
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1628
_reflns_number_gt                1405
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_structure_solution    'Superflip (Palatinus et al., 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
The highest residual electron density peak (ca. 3.0 e_angs_3) is 
located 0.916 angstroms from Pb1. Attempts to improve the absorption 
correction failed to improve the refinement.
;

_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)+(0.0267P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(11)
_refine_ls_number_reflns         1628
_refine_ls_number_parameters     80
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0255
_refine_ls_wR_factor_ref         0.0562
_refine_ls_wR_factor_gt          0.0554
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_restrained_S_all      0.951
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.002

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 0.27740(2) 0.27740(2) 0.0000 0.01712(10) Uani 1 2 d S . .
P1 P 0.33634(18) 0.60190(17) -0.03222(8) 0.0159(3) Uani 1 1 d . . .
O1 O 0.4370(5) 0.2723(5) -0.1081(2) 0.0279(10) Uani 1 1 d . . .
O3 O 0.5208(5) 0.0734(6) -0.1672(2) 0.0272(11) Uani 1 1 d . . .
O2 O 0.4378(6) 0.0275(5) -0.0711(2) 0.0343(12) Uani 1 1 d . . .
C1 C 0.1899(6) 0.7514(5) -0.0052(3) 0.0196(12) Uani 1 1 d . . .
H1A H 0.0813 0.7221 -0.0207 0.029 Uiso 1 1 calc R . .
H1B H 0.2199 0.8590 -0.0217 0.029 Uiso 1 1 calc R . .
H1C H 0.1892 0.7542 0.0415 0.029 Uiso 1 1 calc R . .
C2 C 0.3600(8) 0.6441(7) -0.1159(3) 0.0224(13) Uani 1 1 d . . .
H2A H 0.3919 0.7581 -0.1217 0.034 Uiso 1 1 calc R . .
H2B H 0.2565 0.6242 -0.1379 0.034 Uiso 1 1 calc R . .
H2C H 0.4442 0.5729 -0.1338 0.034 Uiso 1 1 calc R . .
N1 N 0.4645(6) 0.1232(6) -0.1166(2) 0.0207(12) Uani 1 1 d . . .
C3 C 0.5290(6) 0.6618(6) 0.0041(3) 0.0194(12) Uani 1 1 d . . .
H3A H 0.5672 0.7644 -0.0156 0.023 Uiso 1 1 calc R . .
H3B H 0.5118 0.6824 0.0501 0.023 Uiso 1 1 calc R . .


_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
Pb1 O1 2.621(4) 7 ?
Pb1 O1 2.621(4) . ?
Pb1 P1 2.7918(15) 7 ?
Pb1 P1 2.7918(15) . ?
P1 C2 1.802(5) . ?
P1 C1 1.810(5) . ?
P1 C3 1.824(5) . ?
O1 N1 1.257(7) . ?
O3 N1 1.229(6) . ?
O2 N1 1.256(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C3 1.551(10) 7 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?

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 O1 139.98(19) 7 . ?
O1 Pb1 P1 73.67(10) 7 7 ?
O1 Pb1 P1 74.65(10) . 7 ?
O1 Pb1 P1 74.65(10) 7 . ?
O1 Pb1 P1 73.67(10) . . ?
P1 Pb1 P1 74.19(6) 7 . ?
C2 P1 C1 104.3(3) . . ?
C2 P1 C3 105.2(3) . . ?
C1 P1 C3 105.2(2) . . ?
C2 P1 Pb1 116.01(19) . . ?
C1 P1 Pb1 117.16(17) . . ?
C3 P1 Pb1 107.85(19) . . ?
N1 O1 Pb1 103.1(4) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O3 N1 O2 120.9(5) . . ?
O3 N1 O1 120.9(6) . . ?
O2 N1 O1 118.2(5) . . ?
C3 C3 P1 112.0(3) 7 . ?
C3 C3 H3A 109.2 7 . ?
P1 C3 H3A 109.2 . . ?
C3 C3 H3B 109.2 7 . ?
P1 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Pb1 P1 C2 -178.3(3) 7 . . . ?
O1 Pb1 P1 C2 26.5(3) . . . . ?
P1 Pb1 P1 C2 104.7(2) 7 . . . ?
O1 Pb1 P1 C1 -54.3(2) 7 . . . ?
O1 Pb1 P1 C1 150.5(2) . . . . ?
P1 Pb1 P1 C1 -131.3(2) 7 . . . ?
O1 Pb1 P1 C3 64.1(2) 7 . . . ?
O1 Pb1 P1 C3 -91.2(2) . . . . ?
P1 Pb1 P1 C3 -12.9(2) 7 . . . ?
O1 Pb1 O1 N1 134.3(4) 7 . . . ?
P1 Pb1 O1 N1 95.6(4) 7 . . . ?
P1 Pb1 O1 N1 173.2(4) . . . . ?
Pb1 O1 N1 O3 171.0(4) . . . . ?
Pb1 O1 N1 O2 -11.3(6) . . . . ?
C2 P1 C3 C3 -80.5(6) . . . 7 ?
C1 P1 C3 C3 169.6(5) . . . 7 ?
Pb1 P1 C3 C3 43.9(6) . . . 7 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         3.006
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.167
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2014jbr04
_database_code_depnum_ccdc_archive 'CCDC 1060049'
_audit_update_record             
;
2015-04-16 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H16 N2 O6 P2 Pb'
_chemical_formula_sum            'C10 H16 N2 O6 P2 Pb'
_chemical_formula_weight         529.38

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'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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                   10.182(4)
_cell_length_b                   10.863(3)
_cell_length_c                   14.771(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.614(5)
_cell_angle_gamma                90.00
_cell_volume                     1633.0(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3882
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       chunk
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1000
_exptl_absorpt_coefficient_mu    10.552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6205
_exptl_absorpt_correction_T_max  0.8167
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7115
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         27.55
_reflns_number_total             3709
_reflns_number_gt                2948
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
PLAT971_ALERT_2_A Check Calcd Residual Density 0.87A From Pb1 3.78 eA-3
PLAT972_ALERT_2_A Check Calcd Residual Density 0.72A From Pb1 -4.29 eA-3
PLAT972_ALERT_2_A Check Calcd Residual Density 0.80A From Pb1 -3.75 eA-3

PLAT971_ALERT_2_B Check Calcd Residual Density 0.94A From Pb1 3.33 eA-3
PLAT971_ALERT_2_B Check Calcd Residual Density 0.92A From Pb1 2.93 eA-3
PLAT972_ALERT_2_B Check Calcd Residual Density 0.88A From Pb1 -2.90 eA-3
 
The residual electron density peaks indicated above are close to the Pb atom and 
are assumed to be the result of inadequacies in the absorption correction.
;

_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)+(0.0476P)²+0.0000P] 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         3709
_refine_ls_number_parameters     188
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0425
_refine_ls_wR_factor_ref         0.1040
_refine_ls_wR_factor_gt          0.1012
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_restrained_S_all      0.962
_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
C1 C 0.4304(7) 0.2765(7) 0.9639(5) 0.0185(14) Uani 1 1 d . . .
C2 C 0.5499(7) 0.3094(8) 0.9272(5) 0.0267(17) Uani 1 1 d . . .
H2 H 0.5505 0.3466 0.8690 0.032 Uiso 1 1 calc R . .
C3 C 0.6668(8) 0.2893(8) 0.9732(6) 0.0322(19) Uani 1 1 d . . .
H3 H 0.7471 0.3118 0.9464 0.039 Uiso 1 1 calc R . .
C4 C 0.6684(8) 0.2357(7) 1.0594(6) 0.0269(17) Uani 1 1 d . . .
H4 H 0.7494 0.2217 1.0912 0.032 Uiso 1 1 calc R . .
C5 C 0.5519(7) 0.2037(8) 1.0975(6) 0.0252(16) Uani 1 1 d . . .
H5 H 0.5533 0.1672 1.1560 0.030 Uiso 1 1 calc R . .
C6 C 0.4316(7) 0.2232(7) 1.0524(5) 0.0179(14) Uani 1 1 d . . .
C7 C 0.2824(8) 0.2650(7) 1.2104(5) 0.0263(17) Uani 1 1 d . . .
H7A H 0.2028 0.2473 1.2438 0.039 Uiso 1 1 calc R . .
H7B H 0.2874 0.3536 1.1981 0.039 Uiso 1 1 calc R . .
H7C H 0.3598 0.2395 1.2466 0.039 Uiso 1 1 calc R . .
C8 C 0.3003(7) 0.0211(7) 1.1358(5) 0.0247(16) Uani 1 1 d . . .
H8A H 0.3793 0.0131 1.1748 0.037 Uiso 1 1 calc R . .
H8B H 0.3103 -0.0286 1.0811 0.037 Uiso 1 1 calc R . .
H8C H 0.2237 -0.0077 1.1686 0.037 Uiso 1 1 calc R . .
C9 C 0.2863(8) 0.4493(7) 0.8512(5) 0.0270(17) Uani 1 1 d . . .
H9A H 0.3669 0.4585 0.8171 0.040 Uiso 1 1 calc R . .
H9B H 0.2863 0.5092 0.9008 0.040 Uiso 1 1 calc R . .
H9C H 0.2098 0.4636 0.8108 0.040 Uiso 1 1 calc R . .
C10 C 0.3044(8) 0.1951(8) 0.8014(5) 0.0262(17) Uani 1 1 d . . .
H10A H 0.2291 0.2012 0.7589 0.039 Uiso 1 1 calc R . .
H10B H 0.3138 0.1099 0.8224 0.039 Uiso 1 1 calc R . .
H10C H 0.3845 0.2203 0.7711 0.039 Uiso 1 1 calc R . .
N1 N 0.0541(6) 0.0048(6) 0.8741(4) 0.0209(10) Uani 1 1 d . . .
N2 N 0.0596(6) 0.4792(6) 1.1122(4) 0.0209(10) Uani 1 1 d . . .
O1 O 0.0096(5) 0.0989(5) 0.8342(4) 0.0283(13) Uani 1 1 d . . .
O2 O 0.1225(5) 0.0186(5) 0.9469(3) 0.0259(12) Uani 1 1 d . . .
O3 O 0.0310(5) -0.1001(5) 0.8439(4) 0.0266(12) Uani 1 1 d . . .
O4 O 0.1304(5) 0.4592(5) 1.0441(3) 0.0235(12) Uani 1 1 d . . .
O5 O 0.0029(5) 0.3902(5) 1.1474(4) 0.0287(13) Uani 1 1 d . . .
O6 O 0.0482(5) 0.5859(5) 1.1413(4) 0.0268(12) Uani 1 1 d . . .
P1 P 0.27856(17) 0.29470(18) 0.89733(12) 0.0178(4) Uani 1 1 d . . .
P2 P 0.27723(17) 0.18143(18) 1.10447(12) 0.0169(4) Uani 1 1 d . . .
Pb1 Pb 0.05469(2) 0.23997(2) 0.996261(17) 0.01746(10) 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
C1 C2 1.393(10) . ?
C1 C6 1.430(12) . ?
C1 P1 1.820(7) . ?
C2 C3 1.371(11) . ?
C2 H2 0.9500 . ?
C3 C4 1.400(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.372(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(10) . ?
C5 H5 0.9500 . ?
C6 P2 1.826(7) . ?
C7 P2 1.809(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 P2 1.816(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 P1 1.814(8) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 P1 1.808(7) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
N1 O3 1.243(8) . ?
N1 O1 1.258(8) . ?
N1 O2 1.273(7) . ?
N2 O6 1.243(8) . ?
N2 O5 1.247(8) . ?
N2 O4 1.273(8) . ?
O2 Pb1 2.611(6) . ?
O4 Pb1 2.595(5) . ?
P1 Pb1 2.806(2) . ?
P2 Pb1 2.8088(19) . ?

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
C2 C1 C6 118.4(7) . . ?
C2 C1 P1 120.0(6) . . ?
C6 C1 P1 121.6(6) . . ?
C3 C2 C1 121.5(8) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C2 C3 C4 120.3(8) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 119.4(7) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 121.6(8) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C1 118.9(7) . . ?
C5 C6 P2 121.1(6) . . ?
C1 C6 P2 120.0(5) . . ?
P2 C7 H7A 109.5 . . ?
P2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
P2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P2 C8 H8A 109.5 . . ?
P2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
P2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
P1 C9 H9A 109.5 . . ?
P1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P1 C10 H10A 109.5 . . ?
P1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O3 N1 O1 120.9(6) . . ?
O3 N1 O2 120.3(6) . . ?
O1 N1 O2 118.8(6) . . ?
O6 N2 O5 121.9(6) . . ?
O6 N2 O4 119.6(6) . . ?
O5 N2 O4 118.5(6) . . ?
N1 O2 Pb1 101.6(4) . . ?
N2 O4 Pb1 101.6(4) . . ?
C10 P1 C9 104.5(4) . . ?
C10 P1 C1 102.6(4) . . ?
C9 P1 C1 105.0(4) . . ?
C10 P1 Pb1 114.8(3) . . ?
C9 P1 Pb1 115.9(3) . . ?
C1 P1 Pb1 112.7(3) . . ?
C7 P2 C8 105.1(4) . . ?
C7 P2 C6 103.6(4) . . ?
C8 P2 C6 103.8(4) . . ?
C7 P2 Pb1 112.4(3) . . ?
C8 P2 Pb1 117.3(3) . . ?
C6 P2 Pb1 113.2(2) . . ?
O4 Pb1 O2 147.37(16) . . ?
O4 Pb1 P1 73.01(12) . . ?
O2 Pb1 P1 79.90(12) . . ?
O4 Pb1 P2 79.87(12) . . ?
O2 Pb1 P2 74.63(12) . . ?
P1 Pb1 P2 71.95(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.4(12) . . . . ?
P1 C1 C2 C3 -175.6(7) . . . . ?
C1 C2 C3 C4 -0.6(13) . . . . ?
C2 C3 C4 C5 -0.1(13) . . . . ?
C3 C4 C5 C6 -0.1(12) . . . . ?
C4 C5 C6 C1 0.9(12) . . . . ?
C4 C5 C6 P2 -179.4(6) . . . . ?
C2 C1 C6 C5 -1.5(11) . . . . ?
P1 C1 C6 C5 175.5(6) . . . . ?
C2 C1 C6 P2 178.7(6) . . . . ?
P1 C1 C6 P2 -4.2(9) . . . . ?
O3 N1 O2 Pb1 -159.7(5) . . . . ?
O1 N1 O2 Pb1 19.6(6) . . . . ?
O6 N2 O4 Pb1 -164.4(5) . . . . ?
O5 N2 O4 Pb1 15.2(7) . . . . ?
C2 C1 P1 C10 61.1(7) . . . . ?
C6 C1 P1 C10 -115.9(7) . . . . ?
C2 C1 P1 C9 -47.9(7) . . . . ?
C6 C1 P1 C9 135.1(6) . . . . ?
C2 C1 P1 Pb1 -174.9(5) . . . . ?
C6 C1 P1 Pb1 8.2(7) . . . . ?
C5 C6 P2 C7 56.3(7) . . . . ?
C1 C6 P2 C7 -123.9(6) . . . . ?
C5 C6 P2 C8 -53.3(7) . . . . ?
C1 C6 P2 C8 126.5(6) . . . . ?
C5 C6 P2 Pb1 178.4(6) . . . . ?
C1 C6 P2 Pb1 -1.9(7) . . . . ?
N2 O4 Pb1 O2 -134.3(4) . . . . ?
N2 O4 Pb1 P1 -169.4(4) . . . . ?
N2 O4 Pb1 P2 -95.4(4) . . . . ?
N1 O2 Pb1 O4 -127.2(4) . . . . ?
N1 O2 Pb1 P1 -93.2(4) . . . . ?
N1 O2 Pb1 P2 -167.1(4) . . . . ?
C10 P1 Pb1 O4 -164.5(3) . . . . ?
C9 P1 Pb1 O4 -42.4(3) . . . . ?
C1 P1 Pb1 O4 78.5(3) . . . . ?
C10 P1 Pb1 O2 33.9(3) . . . . ?
C9 P1 Pb1 O2 156.0(3) . . . . ?
C1 P1 Pb1 O2 -83.1(3) . . . . ?
C10 P1 Pb1 P2 110.9(3) . . . . ?
C9 P1 Pb1 P2 -127.0(3) . . . . ?
C1 P1 Pb1 P2 -6.1(3) . . . . ?
C7 P2 Pb1 O4 46.2(3) . . . . ?
C8 P2 Pb1 O4 168.2(3) . . . . ?
C6 P2 Pb1 O4 -70.8(3) . . . . ?
C7 P2 Pb1 O2 -154.4(3) . . . . ?
C8 P2 Pb1 O2 -32.4(3) . . . . ?
C6 P2 Pb1 O2 88.6(3) . . . . ?
C7 P2 Pb1 P1 121.4(3) . . . . ?
C8 P2 Pb1 P1 -116.5(3) . . . . ?
C6 P2 Pb1 P1 4.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         3.961
_refine_diff_density_min         -4.710
_refine_diff_density_rms         0.282
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2014JEBR35a
_database_code_depnum_ccdc_archive 'CCDC 1060050'
_audit_update_record             
;
2015-04-16 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H18 F6 O P2 Pb Si, H2 O'
_chemical_formula_sum            'C10 H20 F6 O2 P2 Pb Si'
_chemical_formula_weight         583.48

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
Pb Pb -3.3944 10.1111 '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'

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        P-1
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.6164(17)
_cell_length_b                   10.637(3)
_cell_length_c                   12.354(3)
_cell_angle_alpha                93.580(6)
_cell_angle_beta                 93.952(3)
_cell_angle_gamma                100.854(6)
_cell_volume                     849.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2296
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      27.5

_exptl_crystal_description       chunk
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             552
_exptl_absorpt_coefficient_mu    10.250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5339
_exptl_absorpt_correction_T_max  0.7485
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Sealed Tube'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Fiber
_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7661
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         27.45
_reflns_number_total             3848
_reflns_number_gt                3557
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)
;
_computing_structure_solution    'Superflip (Palatinus et al., 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
The residual electron density peaks close to the Pb atom 
are assumed to be the result of inadequacies in the absorption correction.
;

_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)+(0.0323P)²+0.0000P] 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         3848
_refine_ls_number_parameters     219
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_ref         0.0646
_refine_ls_wR_factor_gt          0.0643
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.002
_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 0.76277(2) 0.927632(15) 0.388215(13) 0.01542(6) Uani 1 1 d . . .
P1 P 0.58523(17) 0.66630(11) 0.33184(10) 0.0166(2) Uani 1 1 d . . .
P2 P 0.77851(17) 0.86793(11) 0.16557(9) 0.0160(2) Uani 1 1 d . . .
Si1 Si 1.38715(19) 1.12535(12) 0.31642(10) 0.0167(3) Uani 1 1 d . . .
C10 C 0.7628(8) 0.9990(5) 0.0814(4) 0.0246(10) Uani 1 1 d . . .
H10A H 0.7638 0.9692 0.0048 0.037 Uiso 1 1 calc R . .
H10B H 0.8815 1.0689 0.1015 0.037 Uiso 1 1 calc R . .
H10C H 0.6348 1.0301 0.0922 0.037 Uiso 1 1 calc R . .
C8 C 0.5644(7) 0.7380(5) 0.1168(4) 0.0182(9) Uani 1 1 d . . .
C3 C 0.4853(7) 0.6479(4) 0.1897(4) 0.0179(9) Uani 1 1 d . . .
C7 C 0.4849(7) 0.7233(5) 0.0083(4) 0.0235(10) Uani 1 1 d . . .
H7 H 0.5366 0.7846 -0.0407 0.028 Uiso 1 1 calc R . .
C4 C 0.3324(7) 0.5423(5) 0.1502(4) 0.0230(10) Uani 1 1 d . . .
H4 H 0.2799 0.4799 0.1981 0.028 Uiso 1 1 calc R . .
C5 C 0.2569(7) 0.5281(5) 0.0419(5) 0.0274(12) Uani 1 1 d . . .
H5 H 0.1543 0.4555 0.0158 0.033 Uiso 1 1 calc R . .
C6 C 0.3297(7) 0.6184(5) -0.0284(4) 0.0289(12) Uani 1 1 d . . .
H6 H 0.2740 0.6093 -0.1021 0.035 Uiso 1 1 calc R . .
C1 C 0.7603(7) 0.5535(4) 0.3384(4) 0.0207(10) Uani 1 1 d . . .
H1A H 0.6846 0.4671 0.3134 0.031 Uiso 1 1 calc R . .
H1B H 0.8180 0.5537 0.4137 0.031 Uiso 1 1 calc R . .
H1C H 0.8725 0.5789 0.2917 0.031 Uiso 1 1 calc R . .
C9 C 1.0060(7) 0.8086(5) 0.1272(4) 0.0207(10) Uani 1 1 d . . .
H9A H 0.9966 0.7903 0.0481 0.031 Uiso 1 1 calc R . .
H9B H 1.0142 0.7297 0.1629 0.031 Uiso 1 1 calc R . .
H9C H 1.1299 0.8736 0.1499 0.031 Uiso 1 1 calc R . .
C2 C 0.3726(7) 0.5944(4) 0.4064(4) 0.0210(10) Uani 1 1 d . . .
H2A H 0.2535 0.6346 0.3901 0.031 Uiso 1 1 calc R . .
H2B H 0.4138 0.6074 0.4847 0.031 Uiso 1 1 calc R . .
H2C H 0.3352 0.5022 0.3850 0.031 Uiso 1 1 calc R . .
F4 F 1.4963(4) 1.1368(3) 0.4461(2) 0.0225(6) Uani 1 1 d . . .
F3 F 1.1519(4) 1.0792(3) 0.3639(2) 0.0232(6) Uani 1 1 d . . .
F5 F 1.4101(4) 0.9642(3) 0.3094(2) 0.0219(6) Uani 1 1 d . . .
F6 F 1.3612(5) 1.2781(3) 0.3300(3) 0.0289(7) Uani 1 1 d . . .
F2 F 1.2818(5) 1.1054(3) 0.1897(2) 0.0287(7) Uani 1 1 d . . .
F1 F 1.6259(4) 1.1638(3) 0.2741(2) 0.0278(7) Uani 1 1 d . . .
O1 O 1.0615(5) 0.8151(4) 0.4000(3) 0.0239(8) Uani 1 1 d . . .
O2 O 1.0439(6) 0.7017(4) 0.5897(3) 0.0264(8) Uani 1 1 d D . .
H17 H 1.179(9) 0.854(6) 0.383(5) 0.023(15) Uiso 1 1 d . . .
H18 H 1.083(9) 0.782(6) 0.460(5) 0.031(17) Uiso 1 1 d . . .
H19 H 1.138(8) 0.743(6) 0.635(4) 0.04(2) Uiso 1 1 d D . .
H20 H 0.940(8) 0.713(8) 0.621(6) 0.07(3) Uiso 1 1 d 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
Pb1 O1 2.496(3) . ?
Pb1 F5 2.573(3) 1_455 ?
Pb1 P2 2.7976(13) . ?
Pb1 P1 2.8299(14) . ?
P1 C2 1.810(5) . ?
P1 C3 1.819(5) . ?
P1 C1 1.820(5) . ?
P2 C10 1.805(5) . ?
P2 C9 1.819(5) . ?
P2 C8 1.822(5) . ?
Si1 F2 1.654(3) . ?
Si1 F6 1.665(3) . ?
Si1 F1 1.683(3) . ?
Si1 F3 1.697(3) . ?
Si1 F4 1.699(3) . ?
Si1 F5 1.746(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C8 C7 1.394(7) . ?
C8 C3 1.409(7) . ?
C3 C4 1.400(6) . ?
C7 C6 1.395(7) . ?
C7 H7 0.9500 . ?
C4 C5 1.385(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.377(8) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
F5 Pb1 2.573(3) 1_655 ?
O1 H17 0.86(6) . ?
O1 H18 0.85(7) . ?
O2 H19 0.84(2) . ?
O2 H20 0.83(2) . ?

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 F5 154.76(11) . 1_455 ?
O1 Pb1 P2 81.77(10) . . ?
F5 Pb1 P2 78.03(7) 1_455 . ?
O1 Pb1 P1 75.63(9) . . ?
F5 Pb1 P1 83.23(7) 1_455 . ?
P2 Pb1 P1 69.67(4) . . ?
C2 P1 C3 105.6(2) . . ?
C2 P1 C1 103.7(2) . . ?
C3 P1 C1 103.4(2) . . ?
C2 P1 Pb1 117.51(16) . . ?
C3 P1 Pb1 108.89(15) . . ?
C1 P1 Pb1 116.33(16) . . ?
C10 P2 C9 104.9(2) . . ?
C10 P2 C8 106.8(2) . . ?
C9 P2 C8 104.0(2) . . ?
C10 P2 Pb1 114.71(17) . . ?
C9 P2 Pb1 115.81(16) . . ?
C8 P2 Pb1 109.71(15) . . ?
F2 Si1 F6 92.72(16) . . ?
F2 Si1 F1 91.50(16) . . ?
F6 Si1 F1 92.86(16) . . ?
F2 Si1 F3 90.74(16) . . ?
F6 Si1 F3 90.01(15) . . ?
F1 Si1 F3 176.27(16) . . ?
F2 Si1 F4 176.73(16) . . ?
F6 Si1 F4 90.55(15) . . ?
F1 Si1 F4 88.51(15) . . ?
F3 Si1 F4 89.09(15) . . ?
F2 Si1 F5 89.65(15) . . ?
F6 Si1 F5 176.84(16) . . ?
F1 Si1 F5 89.16(15) . . ?
F3 Si1 F5 87.87(14) . . ?
F4 Si1 F5 87.08(14) . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C8 C3 119.9(4) . . ?
C7 C8 P2 121.2(4) . . ?
C3 C8 P2 118.9(4) . . ?
C4 C3 C8 118.9(5) . . ?
C4 C3 P1 120.5(4) . . ?
C8 C3 P1 120.5(3) . . ?
C8 C7 C6 120.0(5) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C5 C4 C3 120.5(5) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C6 C5 C4 120.5(5) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 120.1(5) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 F5 Pb1 113.72(13) . 1_655 ?
Pb1 O1 H17 119(4) . . ?
Pb1 O1 H18 116(4) . . ?
H17 O1 H18 107(5) . . ?
H19 O2 H20 100(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Pb1 P1 C2 126.7(2) . . . . ?
F5 Pb1 P1 C2 -67.2(2) 1_455 . . . ?
P2 Pb1 P1 C2 -146.95(19) . . . . ?
O1 Pb1 P1 C3 -113.39(18) . . . . ?
F5 Pb1 P1 C3 52.72(16) 1_455 . . . ?
P2 Pb1 P1 C3 -26.98(15) . . . . ?
O1 Pb1 P1 C1 2.9(2) . . . . ?
F5 Pb1 P1 C1 169.0(2) 1_455 . . . ?
P2 Pb1 P1 C1 89.29(19) . . . . ?
O1 Pb1 P2 C10 -133.4(2) . . . . ?
F5 Pb1 P2 C10 61.8(2) 1_455 . . . ?
P1 Pb1 P2 C10 148.9(2) . . . . ?
O1 Pb1 P2 C9 -10.9(2) . . . . ?
F5 Pb1 P2 C9 -175.67(19) 1_455 . . . ?
P1 Pb1 P2 C9 -88.53(18) . . . . ?
O1 Pb1 P2 C8 106.37(18) . . . . ?
F5 Pb1 P2 C8 -58.42(17) 1_455 . . . ?
P1 Pb1 P2 C8 28.72(15) . . . . ?
C10 P2 C8 C7 29.0(4) . . . . ?
C9 P2 C8 C7 -81.6(4) . . . . ?
Pb1 P2 C8 C7 153.9(3) . . . . ?
C10 P2 C8 C3 -154.0(4) . . . . ?
C9 P2 C8 C3 95.4(4) . . . . ?
Pb1 P2 C8 C3 -29.1(4) . . . . ?
C7 C8 C3 C4 2.2(6) . . . . ?
P2 C8 C3 C4 -174.9(3) . . . . ?
C7 C8 C3 P1 -179.4(3) . . . . ?
P2 C8 C3 P1 3.5(5) . . . . ?
C2 P1 C3 C4 -31.3(4) . . . . ?
C1 P1 C3 C4 77.4(4) . . . . ?
Pb1 P1 C3 C4 -158.3(3) . . . . ?
C2 P1 C3 C8 150.4(4) . . . . ?
C1 P1 C3 C8 -101.0(4) . . . . ?
Pb1 P1 C3 C8 23.3(4) . . . . ?
C3 C8 C7 C6 -1.0(7) . . . . ?
P2 C8 C7 C6 176.0(3) . . . . ?
C8 C3 C4 C5 -1.3(7) . . . . ?
P1 C3 C4 C5 -179.7(3) . . . . ?
C3 C4 C5 C6 -0.7(7) . . . . ?
C4 C5 C6 C7 2.0(7) . . . . ?
C8 C7 C6 C5 -1.1(7) . . . . ?
F2 Si1 F5 Pb1 135.17(16) . . . 1_655 ?
F6 Si1 F5 Pb1 -86(3) . . . 1_655 ?
F1 Si1 F5 Pb1 43.66(16) . . . 1_655 ?
F3 Si1 F5 Pb1 -134.08(16) . . . 1_655 ?
F4 Si1 F5 Pb1 -44.88(15) . . . 1_655 ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         2.286
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.187
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2015jebr02
_database_code_depnum_ccdc_archive 'CCDC 1060051'
_audit_update_record             
;
2015-04-16 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H23 F6 N O P2 Pb Si, 2(C3 H7 N O)'
_chemical_formula_sum            'C19 H37 F6 N3 O3 P2 Pb Si'
_chemical_formula_weight         766.74

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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        P-1
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.404(2)
_cell_length_b                   10.352(3)
_cell_length_c                   15.994(5)
_cell_angle_alpha                87.522(7)
_cell_angle_beta                 89.782(6)
_cell_angle_gamma                86.063(7)
_cell_volume                     1386.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3796
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.5

_exptl_crystal_description       chunk
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             752
_exptl_absorpt_coefficient_mu    6.307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7433
_exptl_absorpt_correction_T_max  0.8333
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Sealed Tube'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Fiber
_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13101
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0920
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6322
_reflns_number_gt                5323
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)
;
_computing_structure_solution    'Superflip (Palatinus et al., 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
The residual electron density peaks close to the Pb atom 
are assumed to be the result of inadequacies in the absorption correction.
;

_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)+(0.0250P)²+0.0000P] 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         6322
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0425
_refine_ls_wR_factor_ref         0.0880
_refine_ls_wR_factor_gt          0.0869
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_restrained_S_all      0.887
_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 0.96375(2) 0.87278(2) 0.382686(14) 0.02649(7) Uani 1 1 d . . .
P1 P 1.03046(17) 0.86646(15) 0.21330(10) 0.0282(3) Uani 1 1 d . . .
P2 P 1.26645(16) 0.95423(14) 0.35845(10) 0.0245(3) Uani 1 1 d . . .
Si1 Si 0.80510(18) 1.19678(16) 0.37057(11) 0.0261(3) Uani 1 1 d . . .
F1 F 0.9500(4) 1.1063(3) 0.3177(2) 0.0295(8) Uani 1 1 d . . .
F2 F 0.8946(4) 1.1367(3) 0.4621(2) 0.0332(8) Uani 1 1 d . . .
F3 F 0.6971(4) 1.0652(3) 0.3737(2) 0.0327(8) Uani 1 1 d . . .
F4 F 0.9223(4) 1.3203(3) 0.3688(2) 0.0342(8) Uani 1 1 d . . .
F5 F 0.7215(4) 1.2477(3) 0.2793(2) 0.0379(9) Uani 1 1 d . . .
F6 F 0.6654(4) 1.2789(3) 0.4244(2) 0.0375(9) Uani 1 1 d . . .
O1 O 1.1192(4) 0.6633(4) 0.3738(3) 0.0303(9) Uani 1 1 d . . .
N1 N 1.2539(6) 0.4934(5) 0.4417(3) 0.0310(12) Uani 1 1 d . . .
C1 C 1.2025(6) 0.9598(6) 0.1855(4) 0.0273(13) Uani 1 1 d . . .
C2 C 1.2358(7) 0.9878(6) 0.1018(4) 0.0299(13) Uani 1 1 d . . .
H2 H 1.1693 0.9592 0.0594 0.036 Uiso 1 1 calc R . .
C3 C 1.3650(7) 1.0571(6) 0.0802(4) 0.0331(14) Uani 1 1 d . . .
H3 H 1.3860 1.0783 0.0230 0.040 Uiso 1 1 calc R . .
C4 C 1.4640(7) 1.0957(6) 0.1417(4) 0.0325(14) Uani 1 1 d . . .
H4 H 1.5534 1.1432 0.1265 0.039 Uiso 1 1 calc R . .
C5 C 1.4349(6) 1.0665(6) 0.2243(4) 0.0277(13) Uani 1 1 d . . .
H5 H 1.5043 1.0934 0.2659 0.033 Uiso 1 1 calc R . .
C6 C 1.3023(6) 0.9965(5) 0.2481(4) 0.0254(12) Uani 1 1 d . . .
C7 C 1.0842(8) 0.7070(6) 0.1756(4) 0.0394(16) Uani 1 1 d . . .
H7A H 1.1173 0.7149 0.1169 0.059 Uiso 1 1 calc R . .
H7B H 0.9920 0.6541 0.1802 0.059 Uiso 1 1 calc R . .
H7C H 1.1723 0.6657 0.2092 0.059 Uiso 1 1 calc R . .
C8 C 0.8723(7) 0.9351(7) 0.1452(5) 0.0492(19) Uani 1 1 d . . .
H8A H 0.8560 1.0283 0.1533 0.074 Uiso 1 1 calc R . .
H8B H 0.7736 0.8934 0.1586 0.074 Uiso 1 1 calc R . .
H8C H 0.9017 0.9207 0.0868 0.074 Uiso 1 1 calc R . .
C9 C 1.4299(6) 0.8381(5) 0.3877(4) 0.0295(13) Uani 1 1 d . . .
H9A H 1.5313 0.8780 0.3786 0.044 Uiso 1 1 calc R . .
H9B H 1.4268 0.7622 0.3534 0.044 Uiso 1 1 calc R . .
H9C H 1.4199 0.8114 0.4469 0.044 Uiso 1 1 calc R . .
C10 C 1.3012(7) 1.0965(6) 0.4157(4) 0.0299(13) Uani 1 1 d . . .
H10A H 1.4042 1.1285 0.3991 0.045 Uiso 1 1 calc R . .
H10B H 1.3022 1.0740 0.4759 0.045 Uiso 1 1 calc R . .
H10C H 1.2161 1.1640 0.4032 0.045 Uiso 1 1 calc R . .
C21 C 1.1555(7) 0.5982(6) 0.4389(4) 0.0307(14) Uani 1 1 d . . .
H21 H 1.1093 0.6258 0.4900 0.037 Uiso 1 1 calc R . .
C22 C 1.2872(8) 0.4199(6) 0.5200(4) 0.0414(16) Uani 1 1 d . . .
H22A H 1.2387 0.4673 0.5665 0.062 Uiso 1 1 calc R . .
H22B H 1.4028 0.4078 0.5284 0.062 Uiso 1 1 calc R . .
H22C H 1.2425 0.3351 0.5179 0.062 Uiso 1 1 calc R . .
C23 C 1.3282(7) 0.4483(6) 0.3658(4) 0.0368(15) Uani 1 1 d . . .
H23A H 1.4359 0.4102 0.3784 0.055 Uiso 1 1 calc R . .
H23B H 1.3346 0.5214 0.3252 0.055 Uiso 1 1 calc R . .
H23C H 1.2646 0.3828 0.3423 0.055 Uiso 1 1 calc R . .
O2 O 0.7363(6) 0.6978(5) 0.2754(3) 0.0498(13) Uani 1 1 d . . .
N2 N 0.5855(6) 0.5897(6) 0.1859(4) 0.0426(14) Uani 1 1 d . . .
C24 C 0.6846(8) 0.5973(8) 0.2503(5) 0.0458(18) Uani 1 1 d . . .
H27 H 0.7186 0.5185 0.2796 0.055 Uiso 1 1 calc R . .
C26 C 0.5374(10) 0.4672(7) 0.1577(5) 0.057(2) Uani 1 1 d . . .
H28A H 0.5754 0.3973 0.1975 0.085 Uiso 1 1 calc R . .
H28B H 0.5836 0.4514 0.1024 0.085 Uiso 1 1 calc R . .
H28C H 0.4208 0.4700 0.1542 0.085 Uiso 1 1 calc R . .
C25 C 0.5316(8) 0.7066(6) 0.1367(5) 0.0459(18) Uani 1 1 d . . .
H29A H 0.6108 0.7247 0.0934 0.069 Uiso 1 1 calc R . .
H29B H 0.5187 0.7799 0.1735 0.069 Uiso 1 1 calc R . .
H29C H 0.4293 0.6936 0.1103 0.069 Uiso 1 1 calc R . .
O3 O 0.8321(8) 0.2707(8) 0.0275(4) 0.090(2) Uani 1 1 d . . .
N3 N 1.0377(7) 0.3314(5) 0.1056(4) 0.0404(13) Uani 1 1 d . . .
C27 C 0.8963(10) 0.2840(8) 0.0939(5) 0.059(2) Uani 1 1 d . . .
H24 H 0.8401 0.2579 0.1427 0.071 Uiso 1 1 calc R . .
C29 C 1.1037(8) 0.3418(6) 0.1880(4) 0.0406(16) Uani 1 1 d . . .
H31A H 1.2053 0.2896 0.1926 0.061 Uiso 1 1 calc R . .
H31B H 1.0291 0.3103 0.2302 0.061 Uiso 1 1 calc R . .
H31C H 1.1215 0.4327 0.1972 0.061 Uiso 1 1 calc R . .
C28 C 1.1368(8) 0.3703(7) 0.0357(4) 0.0497(19) Uani 1 1 d . . .
H32A H 1.1457 0.4642 0.0351 0.074 Uiso 1 1 calc R . .
H32B H 1.0884 0.3471 -0.0168 0.074 Uiso 1 1 calc R . .
H32C H 1.2432 0.3258 0.0415 0.074 Uiso 1 1 calc R . .


_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
Pb1 O1 2.463(4) . ?
Pb1 F1 2.585(3) . ?
Pb1 P2 2.7553(16) . ?
Pb1 P1 2.7671(19) . ?
P1 C8 1.808(6) . ?
P1 C7 1.809(6) . ?
P1 C1 1.836(6) . ?
P2 C10 1.808(6) . ?
P2 C9 1.811(5) . ?
P2 C6 1.829(6) . ?
Si1 F6 1.662(3) . ?
Si1 F4 1.666(4) . ?
Si1 F5 1.671(4) . ?
Si1 F3 1.687(4) . ?
Si1 F2 1.721(4) . ?
Si1 F1 1.725(3) . ?
O1 C21 1.242(7) . ?
N1 C21 1.317(7) . ?
N1 C23 1.444(7) . ?
N1 C22 1.455(8) . ?
C1 C2 1.389(8) . ?
C1 C6 1.391(8) . ?
C2 C3 1.376(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.382(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.367(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.412(8) . ?
C5 H5 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
O2 C24 1.237(9) . ?
N2 C24 1.336(9) . ?
N2 C26 1.447(9) . ?
N2 C25 1.461(8) . ?
C24 H27 0.9500 . ?
C26 H28A 0.9800 . ?
C26 H28B 0.9800 . ?
C26 H28C 0.9800 . ?
C25 H29A 0.9800 . ?
C25 H29B 0.9800 . ?
C25 H29C 0.9800 . ?
O3 C27 1.210(9) . ?
N3 C27 1.333(9) . ?
N3 C29 1.443(8) . ?
N3 C28 1.452(8) . ?
C27 H24 0.9500 . ?
C29 H31A 0.9800 . ?
C29 H31B 0.9800 . ?
C29 H31C 0.9800 . ?
C28 H32A 0.9800 . ?
C28 H32B 0.9800 . ?
C28 H32C 0.9800 . ?

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 F1 140.82(12) . . ?
O1 Pb1 P2 79.17(10) . . ?
F1 Pb1 P2 69.68(7) . . ?
O1 Pb1 P1 78.07(10) . . ?
F1 Pb1 P1 70.37(8) . . ?
P2 Pb1 P1 72.30(5) . . ?
C8 P1 C7 105.6(4) . . ?
C8 P1 C1 104.5(3) . . ?
C7 P1 C1 104.0(3) . . ?
C8 P1 Pb1 115.1(3) . . ?
C7 P1 Pb1 115.0(2) . . ?
C1 P1 Pb1 111.4(2) . . ?
C10 P2 C9 104.8(3) . . ?
C10 P2 C6 106.5(3) . . ?
C9 P2 C6 104.5(3) . . ?
C10 P2 Pb1 112.68(19) . . ?
C9 P2 Pb1 116.3(2) . . ?
C6 P2 Pb1 111.24(19) . . ?
F6 Si1 F4 91.84(19) . . ?
F6 Si1 F5 92.01(19) . . ?
F4 Si1 F5 91.85(19) . . ?
F6 Si1 F3 90.91(19) . . ?
F4 Si1 F3 176.27(18) . . ?
F5 Si1 F3 90.57(19) . . ?
F6 Si1 F2 90.60(19) . . ?
F4 Si1 F2 89.70(19) . . ?
F5 Si1 F2 176.9(2) . . ?
F3 Si1 F2 87.74(18) . . ?
F6 Si1 F1 177.6(2) . . ?
F4 Si1 F1 89.60(17) . . ?
F5 Si1 F1 89.83(18) . . ?
F3 Si1 F1 87.57(17) . . ?
F2 Si1 F1 87.52(17) . . ?
Si1 F1 Pb1 107.86(16) . . ?
C21 O1 Pb1 119.8(4) . . ?
C21 N1 C23 119.9(5) . . ?
C21 N1 C22 121.2(6) . . ?
C23 N1 C22 118.9(5) . . ?
C2 C1 C6 120.6(5) . . ?
C2 C1 P1 119.6(5) . . ?
C6 C1 P1 119.7(5) . . ?
C3 C2 C1 120.1(6) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 119.9(6) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.7(6) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 120.4(6) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C1 C6 C5 118.2(5) . . ?
C1 C6 P2 121.5(4) . . ?
C5 C6 P2 120.3(4) . . ?
P1 C7 H7A 109.5 . . ?
P1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
P1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P1 C8 H8A 109.5 . . ?
P1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
P1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O1 C21 N1 124.3(6) . . ?
O1 C21 H21 117.9 . . ?
N1 C21 H21 117.9 . . ?
N1 C22 H22A 109.5 . . ?
N1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N1 C23 H23A 109.5 . . ?
N1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C24 N2 C26 122.4(6) . . ?
C24 N2 C25 120.1(6) . . ?
C26 N2 C25 117.3(6) . . ?
O2 C24 N2 125.9(7) . . ?
O2 C24 H27 117.0 . . ?
N2 C24 H27 117.0 . . ?
N2 C26 H28A 109.5 . . ?
N2 C26 H28B 109.5 . . ?
H28A C26 H28B 109.5 . . ?
N2 C26 H28C 109.5 . . ?
H28A C26 H28C 109.5 . . ?
H28B C26 H28C 109.5 . . ?
N2 C25 H29A 109.5 . . ?
N2 C25 H29B 109.5 . . ?
H29A C25 H29B 109.5 . . ?
N2 C25 H29C 109.5 . . ?
H29A C25 H29C 109.5 . . ?
H29B C25 H29C 109.5 . . ?
C27 N3 C29 122.1(6) . . ?
C27 N3 C28 121.6(6) . . ?
C29 N3 C28 116.3(6) . . ?
O3 C27 N3 126.8(7) . . ?
O3 C27 H24 116.6 . . ?
N3 C27 H24 116.6 . . ?
N3 C29 H31A 109.5 . . ?
N3 C29 H31B 109.5 . . ?
H31A C29 H31B 109.5 . . ?
N3 C29 H31C 109.5 . . ?
H31A C29 H31C 109.5 . . ?
H31B C29 H31C 109.5 . . ?
N3 C28 H32A 109.5 . . ?
N3 C28 H32B 109.5 . . ?
H32A C28 H32B 109.5 . . ?
N3 C28 H32C 109.5 . . ?
H32A C28 H32C 109.5 . . ?
H32B C28 H32C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Pb1 P1 C8 143.2(3) . . . . ?
F1 Pb1 P1 C8 -60.4(3) . . . . ?
P2 Pb1 P1 C8 -134.5(3) . . . . ?
O1 Pb1 P1 C7 20.0(3) . . . . ?
F1 Pb1 P1 C7 176.4(3) . . . . ?
P2 Pb1 P1 C7 102.3(2) . . . . ?
O1 Pb1 P1 C1 -98.1(2) . . . . ?
F1 Pb1 P1 C1 58.3(2) . . . . ?
P2 Pb1 P1 C1 -15.80(18) . . . . ?
O1 Pb1 P2 C10 -144.0(2) . . . . ?
F1 Pb1 P2 C10 60.1(2) . . . . ?
P1 Pb1 P2 C10 135.2(2) . . . . ?
O1 Pb1 P2 C9 -23.0(2) . . . . ?
F1 Pb1 P2 C9 -178.8(2) . . . . ?
P1 Pb1 P2 C9 -103.8(2) . . . . ?
O1 Pb1 P2 C6 96.5(2) . . . . ?
F1 Pb1 P2 C6 -59.4(2) . . . . ?
P1 Pb1 P2 C6 15.67(19) . . . . ?
F6 Si1 F1 Pb1 12(5) . . . . ?
F4 Si1 F1 Pb1 139.25(17) . . . . ?
F5 Si1 F1 Pb1 -128.89(18) . . . . ?
F3 Si1 F1 Pb1 -38.31(17) . . . . ?
F2 Si1 F1 Pb1 49.53(18) . . . . ?
O1 Pb1 F1 Si1 -174.93(17) . . . . ?
P2 Pb1 F1 Si1 -135.44(18) . . . . ?
P1 Pb1 F1 Si1 146.80(18) . . . . ?
F1 Pb1 O1 C21 138.4(4) . . . . ?
P2 Pb1 O1 C21 101.0(4) . . . . ?
P1 Pb1 O1 C21 175.0(4) . . . . ?
C8 P1 C1 C2 -43.2(5) . . . . ?
C7 P1 C1 C2 67.3(5) . . . . ?
Pb1 P1 C1 C2 -168.1(4) . . . . ?
C8 P1 C1 C6 139.7(5) . . . . ?
C7 P1 C1 C6 -109.8(5) . . . . ?
Pb1 P1 C1 C6 14.8(5) . . . . ?
C6 C1 C2 C3 -2.6(8) . . . . ?
P1 C1 C2 C3 -179.6(4) . . . . ?
C1 C2 C3 C4 1.7(8) . . . . ?
C2 C3 C4 C5 -0.3(9) . . . . ?
C3 C4 C5 C6 -0.3(8) . . . . ?
C2 C1 C6 C5 2.0(8) . . . . ?
P1 C1 C6 C5 179.0(4) . . . . ?
C2 C1 C6 P2 -177.1(4) . . . . ?
P1 C1 C6 P2 -0.1(6) . . . . ?
C4 C5 C6 C1 -0.6(8) . . . . ?
C4 C5 C6 P2 178.5(4) . . . . ?
C10 P2 C6 C1 -137.9(5) . . . . ?
C9 P2 C6 C1 111.5(5) . . . . ?
Pb1 P2 C6 C1 -14.7(5) . . . . ?
C10 P2 C6 C5 43.1(5) . . . . ?
C9 P2 C6 C5 -67.6(5) . . . . ?
Pb1 P2 C6 C5 166.2(4) . . . . ?
Pb1 O1 C21 N1 -171.4(4) . . . . ?
C23 N1 C21 O1 0.5(9) . . . . ?
C22 N1 C21 O1 -178.2(6) . . . . ?
C26 N2 C24 O2 176.5(7) . . . . ?
C25 N2 C24 O2 1.6(10) . . . . ?
C29 N3 C27 O3 -179.4(9) . . . . ?
C28 N3 C27 O3 -2.1(14) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.223
_refine_diff_density_min         -1.931
_refine_diff_density_rms         0.174
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2015jebr01
_database_code_depnum_ccdc_archive 'CCDC 1060052'
_audit_update_record             
;
2015-04-16 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H48 N2 O10 P4 Pb'
_chemical_formula_sum            'C20 H48 N2 O10 P4 Pb'
_chemical_formula_weight         807.67

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'
Pb Pb -3.3944 10.1111 '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'

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/c'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'

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                   15.1483(5)
_cell_length_b                   13.8900(4)
_cell_length_c                   16.2854(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.383(3)
_cell_angle_gamma                90.00
_cell_volume                     3168.44(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4046
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      27.5

_exptl_crystal_description       chunk
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    5.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7679
_exptl_absorpt_correction_T_max  0.8506
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Sealed Tube'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Fiber
_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26042
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         27.48
_reflns_number_total             7234
_reflns_number_gt                5641
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)
;
_computing_structure_solution    'Superflip (Palatinus et al., 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
?
;

_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)+(0.0341P)²+3.3379P] 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         7234
_refine_ls_number_parameters     342
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0730
_refine_ls_wR_factor_gt          0.0674
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_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 0.252071(9) 0.345578(9) 0.499334(8) 0.01268(5) Uani 1 1 d . . .
P1 P -0.00524(7) 0.34133(6) 0.48308(6) 0.01527(19) Uani 1 1 d . . .
P4 P 0.50794(7) 0.34247(6) 0.51944(6) 0.01531(19) Uani 1 1 d . . .
P2 P 0.23933(7) 0.13753(7) 0.35559(6) 0.01392(19) Uani 1 1 d . . .
O1 O 0.09850(18) 0.31423(18) 0.51637(16) 0.0197(6) Uani 1 1 d . . .
O4 O 0.40520(18) 0.31617(18) 0.46812(16) 0.0183(5) Uani 1 1 d . . .
O2 O 0.19946(17) 0.20401(18) 0.40578(15) 0.0170(5) Uani 1 1 d . . .
O6 O 0.1289(2) 0.4264(2) 0.34040(18) 0.0346(7) Uani 1 1 d . . .
O9 O 0.3798(2) 0.4647(2) 0.6401(2) 0.0365(8) Uani 1 1 d . . .
N1 N 0.1568(3) 0.5115(3) 0.3544(2) 0.0265(8) Uani 1 1 d . . .
C8 C 0.3385(3) 0.0684(3) 0.4298(2) 0.0198(8) Uani 1 1 d . . .
H8A H 0.3878 0.1136 0.4674 0.024 Uiso 1 1 calc R . .
H8B H 0.3161 0.0303 0.4695 0.024 Uiso 1 1 calc R . .
N2 N 0.3166(3) 0.5150(2) 0.6497(2) 0.0247(8) Uani 1 1 d . . .
C3 C -0.0639(3) 0.3384(3) 0.3648(3) 0.0255(9) Uani 1 1 d . . .
H3A H -0.1323 0.3537 0.3488 0.031 Uiso 1 1 calc R . .
H3B H -0.0363 0.3893 0.3392 0.031 Uiso 1 1 calc R . .
C16 C 0.5533(3) 0.2815(3) 0.6261(3) 0.0243(9) Uani 1 1 d . . .
H16A H 0.5164 0.3042 0.6611 0.029 Uiso 1 1 calc R . .
H16B H 0.5406 0.2118 0.6154 0.029 Uiso 1 1 calc R . .
C6 C 0.1495(3) 0.0548(3) 0.2880(2) 0.0229(9) Uani 1 1 d . . .
H6A H 0.0948 0.0920 0.2468 0.027 Uiso 1 1 calc R . .
H6B H 0.1762 0.0161 0.2519 0.027 Uiso 1 1 calc R . .
C18 C 0.5829(3) 0.3132(3) 0.4599(3) 0.0248(9) Uani 1 1 d . . .
H18A H 0.5648 0.3549 0.4067 0.030 Uiso 1 1 calc R . .
H18B H 0.6499 0.3286 0.4981 0.030 Uiso 1 1 calc R . .
C1 C -0.0652(3) 0.2587(3) 0.5308(3) 0.0286(9) Uani 1 1 d . . .
H1A H -0.0478 0.1922 0.5210 0.034 Uiso 1 1 calc R . .
H1B H -0.0404 0.2695 0.5958 0.034 Uiso 1 1 calc R . .
C7 C 0.1135(3) -0.0130(3) 0.3420(3) 0.0343(11) Uani 1 1 d . . .
H7A H 0.1655 -0.0555 0.3778 0.051 Uiso 1 1 calc R . .
H7B H 0.0607 -0.0518 0.3017 0.051 Uiso 1 1 calc R . .
H7C H 0.0912 0.0247 0.3812 0.051 Uiso 1 1 calc R . .
C19 C 0.5781(3) 0.2086(3) 0.4305(3) 0.0361(11) Uani 1 1 d . . .
H19A H 0.6039 0.1670 0.4829 0.054 Uiso 1 1 calc R . .
H19B H 0.6156 0.2005 0.3935 0.054 Uiso 1 1 calc R . .
H19C H 0.5115 0.1910 0.3962 0.054 Uiso 1 1 calc R . .
C2 C -0.1730(3) 0.2656(4) 0.4955(3) 0.0445(13) Uani 1 1 d . . .
H2A H -0.1917 0.3312 0.5039 0.067 Uiso 1 1 calc R . .
H2B H -0.1978 0.2202 0.5276 0.067 Uiso 1 1 calc R . .
H2C H -0.1993 0.2498 0.4321 0.067 Uiso 1 1 calc R . .
C4 C -0.0562(3) 0.2435(3) 0.3236(3) 0.0381(11) Uani 1 1 d . . .
H4A H 0.0111 0.2248 0.3433 0.057 Uiso 1 1 calc R . .
H4B H -0.0833 0.2495 0.2588 0.057 Uiso 1 1 calc R . .
H4C H -0.0913 0.1942 0.3419 0.057 Uiso 1 1 calc R . .
O5 O 0.1013(2) 0.5789(2) 0.3169(2) 0.0422(8) Uani 1 1 d . . .
O8 O 0.2333(2) 0.4818(2) 0.62459(19) 0.0380(8) Uani 1 1 d . . .
C9 C 0.3848(3) -0.0001(3) 0.3847(3) 0.0259(9) Uani 1 1 d . . .
H9A H 0.3372 -0.0464 0.3481 0.039 Uiso 1 1 calc R . .
H9B H 0.4373 -0.0347 0.4299 0.039 Uiso 1 1 calc R . .
H9C H 0.4098 0.0369 0.3469 0.039 Uiso 1 1 calc R . .
O10 O 0.3356(3) 0.5958(2) 0.6850(2) 0.0493(10) Uani 1 1 d . . .
O7 O 0.2380(2) 0.5298(2) 0.4098(3) 0.0557(10) Uani 1 1 d . . .
C5 C -0.0233(3) 0.4607(3) 0.5176(2) 0.0197(8) Uani 1 1 d . . .
H5A H -0.0927 0.4735 0.4966 0.024 Uiso 1 1 calc R . .
H5B H 0.0031 0.4634 0.5833 0.024 Uiso 1 1 calc R . .
C20 C 0.5257(3) 0.4698(3) 0.5419(2) 0.0174(7) Uani 1 1 d . . .
H20A H 0.5013 0.4878 0.5883 0.021 Uiso 1 1 calc R . .
H20B H 0.5949 0.4844 0.5649 0.021 Uiso 1 1 calc R . .
C17 C 0.6579(3) 0.2945(3) 0.6815(3) 0.0385(11) Uani 1 1 d . . .
H17A H 0.6958 0.2699 0.6490 0.058 Uiso 1 1 calc R . .
H17B H 0.6742 0.2590 0.7374 0.058 Uiso 1 1 calc R . .
H17C H 0.6716 0.3631 0.6943 0.058 Uiso 1 1 calc R . .
P3 P 0.26537(7) 0.15968(7) 0.65861(6) 0.01426(19) Uani 1 1 d . . .
O3 O 0.31309(18) 0.22275(18) 0.61213(15) 0.0184(5) Uani 1 1 d . . .
C15 C 0.2116(3) 0.2286(3) 0.7208(2) 0.0169(7) Uani 1 1 d . . .
H15A H 0.1566 0.2654 0.6795 0.020 Uiso 1 1 calc R . .
H15B H 0.1878 0.1847 0.7556 0.020 Uiso 1 1 calc R . .
C11 C 0.1731(3) 0.0866(3) 0.5817(2) 0.0191(8) Uani 1 1 d . . .
H11A H 0.1246 0.1296 0.5399 0.023 Uiso 1 1 calc R . .
H11B H 0.2013 0.0481 0.5467 0.023 Uiso 1 1 calc R . .
C13 C 0.3513(3) 0.0805(3) 0.7360(2) 0.0236(9) Uani 1 1 d . . .
H13A H 0.4012 0.1196 0.7809 0.028 Uiso 1 1 calc R . .
H13B H 0.3191 0.0416 0.7673 0.028 Uiso 1 1 calc R . .
C12 C 0.1228(3) 0.0181(3) 0.6232(3) 0.0354(11) Uani 1 1 d . . .
H12A H 0.1699 -0.0248 0.6652 0.053 Uiso 1 1 calc R . .
H12B H 0.0757 -0.0204 0.5764 0.053 Uiso 1 1 calc R . .
H12C H 0.0904 0.0554 0.6545 0.053 Uiso 1 1 calc R . .
C14 C 0.3984(3) 0.0132(3) 0.6913(3) 0.0363(11) Uani 1 1 d . . .
H14A H 0.3498 -0.0281 0.6489 0.054 Uiso 1 1 calc R . .
H14B H 0.4457 -0.0269 0.7363 0.054 Uiso 1 1 calc R . .
H14C H 0.4302 0.0512 0.6598 0.054 Uiso 1 1 calc R . .
C10 C 0.2849(3) 0.2014(3) 0.2839(2) 0.0156(7) Uani 1 1 d . . .
H10A H 0.3425 0.2380 0.3207 0.019 Uiso 1 1 calc R . .
H10B H 0.3042 0.1543 0.2482 0.019 Uiso 1 1 calc R . .


_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
Pb1 O3 2.418(2) . ?
Pb1 O2 2.429(2) . ?
Pb1 O1 2.484(2) . ?
Pb1 O4 2.589(2) . ?
P1 O1 1.502(3) . ?
P1 C3 1.788(4) . ?
P1 C5 1.805(4) . ?
P1 C1 1.813(4) . ?
P4 O4 1.504(3) . ?
P4 C18 1.799(4) . ?
P4 C20 1.806(4) . ?
P4 C16 1.815(4) . ?
P2 O2 1.504(2) . ?
P2 C6 1.801(4) . ?
P2 C10 1.801(3) . ?
P2 C8 1.805(4) . ?
O6 N1 1.247(4) . ?
O9 N2 1.243(4) . ?
N1 O7 1.244(5) . ?
N1 O5 1.251(4) . ?
C8 C9 1.526(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
N2 O10 1.243(4) . ?
N2 O8 1.256(4) . ?
C3 C4 1.505(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C16 C17 1.506(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C6 C7 1.523(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C18 C19 1.523(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C1 C2 1.514(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C5 C5 1.526(7) 3_566 ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C20 C20 1.536(7) 3_666 ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
P3 O3 1.510(3) . ?
P3 C11 1.794(4) . ?
P3 C15 1.799(3) . ?
P3 C13 1.801(4) . ?
C15 C10 1.537(5) 4_566 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C11 C12 1.528(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C13 C14 1.519(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C10 C15 1.537(5) 4_565 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?

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
O3 Pb1 O2 81.05(9) . . ?
O3 Pb1 O1 83.96(8) . . ?
O2 Pb1 O1 80.25(8) . . ?
O3 Pb1 O4 85.75(8) . . ?
O2 Pb1 O4 81.58(8) . . ?
O1 Pb1 O4 160.30(9) . . ?
O1 P1 C3 113.94(17) . . ?
O1 P1 C5 112.32(17) . . ?
C3 P1 C5 106.51(18) . . ?
O1 P1 C1 108.24(17) . . ?
C3 P1 C1 108.8(2) . . ?
C5 P1 C1 106.72(17) . . ?
O4 P4 C18 112.20(17) . . ?
O4 P4 C20 113.15(16) . . ?
C18 P4 C20 104.74(18) . . ?
O4 P4 C16 110.66(17) . . ?
C18 P4 C16 108.89(19) . . ?
C20 P4 C16 106.88(17) . . ?
O2 P2 C6 110.93(16) . . ?
O2 P2 C10 112.48(16) . . ?
C6 P2 C10 107.79(16) . . ?
O2 P2 C8 111.54(15) . . ?
C6 P2 C8 108.19(19) . . ?
C10 P2 C8 105.64(17) . . ?
P1 O1 Pb1 144.23(15) . . ?
P4 O4 Pb1 131.86(14) . . ?
P2 O2 Pb1 137.26(14) . . ?
O7 N1 O6 119.9(4) . . ?
O7 N1 O5 119.8(4) . . ?
O6 N1 O5 120.2(4) . . ?
C9 C8 P2 115.3(3) . . ?
C9 C8 H8A 108.4 . . ?
P2 C8 H8A 108.4 . . ?
C9 C8 H8B 108.4 . . ?
P2 C8 H8B 108.4 . . ?
H8A C8 H8B 107.5 . . ?
O10 N2 O9 120.7(4) . . ?
O10 N2 O8 120.6(4) . . ?
O9 N2 O8 118.7(3) . . ?
C4 C3 P1 114.1(3) . . ?
C4 C3 H3A 108.7 . . ?
P1 C3 H3A 108.7 . . ?
C4 C3 H3B 108.7 . . ?
P1 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C17 C16 P4 116.5(3) . . ?
C17 C16 H16A 108.2 . . ?
P4 C16 H16A 108.2 . . ?
C17 C16 H16B 108.2 . . ?
P4 C16 H16B 108.2 . . ?
H16A C16 H16B 107.3 . . ?
C7 C6 P2 113.3(3) . . ?
C7 C6 H6A 108.9 . . ?
P2 C6 H6A 108.9 . . ?
C7 C6 H6B 108.9 . . ?
P2 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
C19 C18 P4 114.8(3) . . ?
C19 C18 H18A 108.6 . . ?
P4 C18 H18A 108.6 . . ?
C19 C18 H18B 108.6 . . ?
P4 C18 H18B 108.6 . . ?
H18A C18 H18B 107.5 . . ?
C2 C1 P1 116.2(3) . . ?
C2 C1 H1A 108.2 . . ?
P1 C1 H1A 108.2 . . ?
C2 C1 H1B 108.2 . . ?
P1 C1 H1B 108.2 . . ?
H1A C1 H1B 107.4 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C5 P1 113.2(3) 3_566 . ?
C5 C5 H5A 108.9 3_566 . ?
P1 C5 H5A 108.9 . . ?
C5 C5 H5B 108.9 3_566 . ?
P1 C5 H5B 108.9 . . ?
H5A C5 H5B 107.8 . . ?
C20 C20 P4 111.6(3) 3_666 . ?
C20 C20 H20A 109.3 3_666 . ?
P4 C20 H20A 109.3 . . ?
C20 C20 H20B 109.3 3_666 . ?
P4 C20 H20B 109.3 . . ?
H20A C20 H20B 108.0 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O3 P3 C11 111.90(15) . . ?
O3 P3 C15 112.29(16) . . ?
C11 P3 C15 107.13(17) . . ?
O3 P3 C13 110.41(17) . . ?
C11 P3 C13 107.83(19) . . ?
C15 P3 C13 107.03(17) . . ?
P3 O3 Pb1 132.28(15) . . ?
C10 C15 P3 110.2(2) 4_566 . ?
C10 C15 H15A 109.6 4_566 . ?
P3 C15 H15A 109.6 . . ?
C10 C15 H15B 109.6 4_566 . ?
P3 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
C12 C11 P3 115.6(3) . . ?
C12 C11 H11A 108.4 . . ?
P3 C11 H11A 108.4 . . ?
C12 C11 H11B 108.4 . . ?
P3 C11 H11B 108.4 . . ?
H11A C11 H11B 107.5 . . ?
C14 C13 P3 112.7(3) . . ?
C14 C13 H13A 109.0 . . ?
P3 C13 H13A 109.0 . . ?
C14 C13 H13B 109.0 . . ?
P3 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 C10 P2 112.7(2) 4_565 . ?
C15 C10 H10A 109.0 4_565 . ?
P2 C10 H10A 109.0 . . ?
C15 C10 H10B 109.0 4_565 . ?
P2 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 P1 O1 Pb1 50.1(3) . . . . ?
C5 P1 O1 Pb1 -71.2(3) . . . . ?
C1 P1 O1 Pb1 171.3(3) . . . . ?
O3 Pb1 O1 P1 -178.5(3) . . . . ?
O2 Pb1 O1 P1 -96.5(3) . . . . ?
O4 Pb1 O1 P1 -119.5(3) . . . . ?
C18 P4 O4 Pb1 -174.43(19) . . . . ?
C20 P4 O4 Pb1 -56.2(2) . . . . ?
C16 P4 O4 Pb1 63.7(2) . . . . ?
O3 Pb1 O4 P4 -73.0(2) . . . . ?
O2 Pb1 O4 P4 -154.6(2) . . . . ?
O1 Pb1 O4 P4 -131.7(2) . . . . ?
C6 P2 O2 Pb1 -172.6(2) . . . . ?
C10 P2 O2 Pb1 -51.8(2) . . . . ?
C8 P2 O2 Pb1 66.7(2) . . . . ?
O3 Pb1 O2 P2 -88.1(2) . . . . ?
O1 Pb1 O2 P2 -173.4(2) . . . . ?
O4 Pb1 O2 P2 -1.1(2) . . . . ?
O2 P2 C8 C9 -179.0(3) . . . . ?
C6 P2 C8 C9 58.7(3) . . . . ?
C10 P2 C8 C9 -56.5(3) . . . . ?
O1 P1 C3 C4 55.4(4) . . . . ?
C5 P1 C3 C4 179.8(3) . . . . ?
C1 P1 C3 C4 -65.5(4) . . . . ?
O4 P4 C16 C17 175.0(3) . . . . ?
C18 P4 C16 C17 51.2(4) . . . . ?
C20 P4 C16 C17 -61.4(4) . . . . ?
O2 P2 C6 C7 -63.7(3) . . . . ?
C10 P2 C6 C7 172.8(3) . . . . ?
C8 P2 C6 C7 59.0(3) . . . . ?
O4 P4 C18 C19 -55.1(4) . . . . ?
C20 P4 C18 C19 -178.2(3) . . . . ?
C16 P4 C18 C19 67.8(4) . . . . ?
O1 P1 C1 C2 -171.9(3) . . . . ?
C3 P1 C1 C2 -47.6(4) . . . . ?
C5 P1 C1 C2 67.0(4) . . . . ?
O1 P1 C5 C5 61.6(4) . . . 3_566 ?
C3 P1 C5 C5 -63.8(4) . . . 3_566 ?
C1 P1 C5 C5 -180.0(4) . . . 3_566 ?
O4 P4 C20 C20 -47.9(4) . . . 3_666 ?
C18 P4 C20 C20 74.6(4) . . . 3_666 ?
C16 P4 C20 C20 -170.0(3) . . . 3_666 ?
C11 P3 O3 Pb1 59.1(2) . . . . ?
C15 P3 O3 Pb1 -61.4(2) . . . . ?
C13 P3 O3 Pb1 179.20(19) . . . . ?
O2 Pb1 O3 P3 -77.68(19) . . . . ?
O1 Pb1 O3 P3 3.36(19) . . . . ?
O4 Pb1 O3 P3 -159.8(2) . . . . ?
O3 P3 C15 C10 -52.8(3) . . . 4_566 ?
C11 P3 C15 C10 -176.0(2) . . . 4_566 ?
C13 P3 C15 C10 68.5(3) . . . 4_566 ?
O3 P3 C11 C12 178.2(3) . . . . ?
C15 P3 C11 C12 -58.3(3) . . . . ?
C13 P3 C11 C12 56.6(3) . . . . ?
O3 P3 C13 C14 -60.9(4) . . . . ?
C11 P3 C13 C14 61.6(4) . . . . ?
C15 P3 C13 C14 176.6(3) . . . . ?
O2 P2 C10 C15 -53.2(3) . . . 4_565 ?
C6 P2 C10 C15 69.4(3) . . . 4_565 ?
C8 P2 C10 C15 -175.1(3) . . . 4_565 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.703
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.130
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_13jebrwrg03
_database_code_depnum_ccdc_archive 'CCDC 1060053'
_audit_update_record             
;
2015-04-16 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C12 H32 O2 P4 Pb 2+, 2(B F4 1-), 0.5(C H3 N O2)'
_chemical_formula_sum            'C12.50 H33.50 B2 F8 N0.50 O3 P4 Pb'
_chemical_formula_weight         743.59

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'
B B 0.0013 0.0007 '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'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'F d d d'
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   16.938(6)
_cell_length_b                   24.212(9)
_cell_length_c                   25.686(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10534(7)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5317
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      31.3

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5760
_exptl_absorpt_coefficient_mu    6.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5530
_exptl_absorpt_correction_T_max  0.7299
_exptl_absorpt_process_details   
;Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11501
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.80
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3021
_reflns_number_gt                2685
_reflns_threshold_expression     >2σ(I)


_computing_data_collection       'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
The N1 of the fractionally occupied lattice nitromethane 
is located on a site with 222 symmetry giving a 
very disordered molecule. The hydrogen atoms have therefore
been omitted from the refinement but included in the formula.
;

_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)+(0.0317P)²+189.0746P] 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         3021
_refine_ls_number_parameters     212
_refine_ls_number_restraints     223
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0527
_refine_ls_wR_factor_ref         0.1075
_refine_ls_wR_factor_gt          0.1033
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_restrained_S_all      1.124
_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
Pb1 Pb 0.8750 0.3750 0.078880(14) 0.04998(14) Uani 1 2 d SU . .
P1 P 0.96539(12) 0.34891(10) 0.16625(8) 0.0587(5) Uani 1 1 d U . .
P2 P 0.94326(15) 0.52010(9) 0.07521(8) 0.0661(6) Uani 1 1 d DU . .
O1 O 0.9316(4) 0.4656(2) 0.0999(2) 0.0683(14) Uani 1 1 d U A .
C1 C 0.9038(6) 0.3516(6) 0.2233(3) 0.109(4) Uani 1 1 d U . .
H1A H 0.8743 0.3164 0.2261 0.130 Uiso 1 1 calc R . .
H1B H 0.9380 0.3548 0.2544 0.130 Uiso 1 1 calc R . .
C2 C 1.0132(6) 0.2821(4) 0.1695(4) 0.080(3) Uani 1 1 d U . .
H2A H 1.0462 0.2802 0.2008 0.120 Uiso 1 1 calc R . .
H2B H 1.0462 0.2768 0.1386 0.120 Uiso 1 1 calc R . .
H2C H 0.9730 0.2530 0.1710 0.120 Uiso 1 1 calc R . .
C3 C 1.0412(6) 0.3986(4) 0.1805(5) 0.095(3) Uani 1 1 d U . .
H3A H 1.0188 0.4359 0.1793 0.143 Uiso 1 1 calc R . .
H3B H 1.0835 0.3955 0.1546 0.143 Uiso 1 1 calc R . .
H3C H 1.0627 0.3915 0.2152 0.143 Uiso 1 1 calc R . .
C4 C 0.9623(5) 0.5160(3) 0.0064(3) 0.0557(18) Uani 1 1 d U . .
H4A H 0.9170 0.4978 -0.0109 0.067 Uiso 1 1 calc R . .
H4B H 0.9668 0.5538 -0.0079 0.067 Uiso 1 1 calc R . .
C5A C 0.8689(17) 0.5686(15) 0.088(2) 0.065(6) Uani 0.37(3) 1 d PDU A 1
H5A1 H 0.8840 0.6045 0.0739 0.098 Uiso 0.37(3) 1 calc PR A 1
H5A2 H 0.8618 0.5719 0.1261 0.098 Uiso 0.37(3) 1 calc PR A 1
H5A3 H 0.8193 0.5564 0.0724 0.098 Uiso 0.37(3) 1 calc PR A 1
C6A C 1.0086(13) 0.5702(9) 0.1015(8) 0.047(5) Uani 0.37(3) 1 d PDU A 1
H6A1 H 0.9966 0.5758 0.1384 0.070 Uiso 0.37(3) 1 calc PR A 1
H6A2 H 1.0021 0.6052 0.0827 0.070 Uiso 0.37(3) 1 calc PR A 1
H6A3 H 1.0631 0.5573 0.0978 0.070 Uiso 0.37(3) 1 calc PR A 1
F1A F 0.8986(16) 0.5622(17) 0.2219(13) 0.049(4) Uani 0.377(12) 1 d PDU B 1
F2A F 0.9641(16) 0.5722(12) 0.3002(7) 0.092(7) Uani 0.377(12) 1 d PDU B 1
F3A F 1.0045(11) 0.5126(7) 0.2431(10) 0.114(7) Uani 0.377(12) 1 d PDU B 1
F4A F 1.0185(9) 0.5994(7) 0.2247(4) 0.084(6) Uani 0.377(12) 1 d PDU B 1
B1A B 0.9687(11) 0.5625(6) 0.2479(8) 0.049(5) Uani 0.377(12) 1 d PDU B 1
C5B C 0.8549(11) 0.5616(8) 0.0803(11) 0.070(4) Uani 0.63(3) 1 d PDU A 2
H5B1 H 0.8105 0.5418 0.0646 0.104 Uiso 0.63(3) 1 calc PR A 2
H5B2 H 0.8629 0.5967 0.0620 0.104 Uiso 0.63(3) 1 calc PR A 2
H5B3 H 0.8436 0.5690 0.1171 0.104 Uiso 0.63(3) 1 calc PR A 2
C6B C 1.0368(10) 0.5433(10) 0.1031(6) 0.075(5) Uani 0.63(3) 1 d PDU A 2
H6B1 H 1.0315 0.5465 0.1409 0.113 Uiso 0.63(3) 1 calc PR A 2
H6B2 H 1.0508 0.5793 0.0884 0.113 Uiso 0.63(3) 1 calc PR A 2
H6B3 H 1.0783 0.5164 0.0948 0.113 Uiso 0.63(3) 1 calc PR A 2
F1B F 0.9120(11) 0.5550(12) 0.2189(10) 0.076(6) Uani 0.623(12) 1 d PDU B 2
F2B F 0.9600(10) 0.5937(4) 0.2915(5) 0.064(3) Uani 0.623(12) 1 d PDU B 2
F3B F 1.0408(4) 0.5466(4) 0.2368(3) 0.072(3) Uani 0.623(12) 1 d PDU B 2
F4B F 0.9493(6) 0.5016(3) 0.2812(4) 0.087(3) Uani 0.623(12) 1 d PDU B 2
B1B B 0.9668(7) 0.5502(4) 0.2574(5) 0.044(3) Uani 0.623(12) 1 d PDU B 2
N1 N 0.8750 0.3750 0.3750 0.117(7) Uiso 1 4 d SDU . .
O2 O 0.8411(11) 0.3311(7) 0.3803(11) 0.175(9) Uiso 0.50 1 d PDU . .
C7 C 0.7977(12) 0.3716(15) 0.3981(12) 0.065(8) Uiso 0.25 1 d PDU . .


_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
Pb1 O1 2.454(6) . ?
Pb1 O1 2.454(6) 2_655 ?
Pb1 P1 2.789(2) . ?
Pb1 P1 2.789(2) 2_655 ?
P1 C3 1.797(9) . ?
P1 C1 1.799(10) . ?
P1 C2 1.812(9) . ?
P2 O1 1.478(6) . ?
P2 C5A 1.754(18) . ?
P2 C6A 1.775(14) . ?
P2 C4 1.800(7) . ?
P2 C5B 1.807(14) . ?
P2 C6B 1.827(13) . ?
C1 C1 1.50(2) 2_655 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C4 1.528(16) 17_765 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5A H5A1 0.9800 . ?
C5A H5A2 0.9800 . ?
C5A H5A3 0.9800 . ?
C6A H6A1 0.9800 . ?
C6A H6A2 0.9800 . ?
C6A H6A3 0.9800 . ?
F1A B1A 1.363(10) . ?
F2A B1A 1.366(10) . ?
F3A B1A 1.357(10) . ?
F4A B1A 1.366(10) . ?
C5B H5B1 0.9800 . ?
C5B H5B2 0.9800 . ?
C5B H5B3 0.9800 . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
F1B B1B 1.360(9) . ?
F2B B1B 1.375(8) . ?
F3B B1B 1.363(8) . ?
F4B B1B 1.361(9) . ?
N1 O2 1.215(15) 3_655 ?
N1 O2 1.215(15) . ?
N1 O2 1.215(15) 4 ?
N1 O2 1.215(15) 2_655 ?
N1 C7 1.440(17) 4 ?
N1 C7 1.440(17) . ?
N1 C7 1.440(17) 3_655 ?
N1 C7 1.440(17) 2_655 ?
O2 O2 1.18(4) 3_655 ?
O2 C7 1.31(3) . ?
O2 C7 1.54(3) 4 ?
C7 C7 1.20(6) 4 ?
C7 O2 1.54(3) 4 ?

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 O1 154.5(3) . 2_655 ?
O1 Pb1 P1 79.09(14) . . ?
O1 Pb1 P1 80.48(14) 2_655 . ?
O1 Pb1 P1 80.48(14) . 2_655 ?
O1 Pb1 P1 79.09(14) 2_655 2_655 ?
P1 Pb1 P1 72.86(9) . 2_655 ?
C3 P1 C1 103.0(6) . . ?
C3 P1 C2 105.6(5) . . ?
C1 P1 C2 104.7(5) . . ?
C3 P1 Pb1 113.8(4) . . ?
C1 P1 Pb1 109.2(3) . . ?
C2 P1 Pb1 119.0(3) . . ?
O1 P2 C5A 114.7(18) . . ?
O1 P2 C6A 122.0(8) . . ?
C5A P2 C6A 85.3(16) . . ?
O1 P2 C4 113.4(3) . . ?
C5A P2 C4 110.8(18) . . ?
C6A P2 C4 107.4(8) . . ?
O1 P2 C5B 110.8(9) . . ?
C5A P2 C5B 11.3(16) . . ?
C6A P2 C5B 96.2(12) . . ?
C4 P2 C5B 104.5(10) . . ?
O1 P2 C6B 102.8(8) . . ?
C5A P2 C6B 110.0(16) . . ?
C6A P2 C6B 25.9(7) . . ?
C4 P2 C6B 104.2(6) . . ?
C5B P2 C6B 121.2(12) . . ?
P2 O1 Pb1 139.1(3) . . ?
C1 C1 P1 113.9(7) 2_655 . ?
C1 C1 H1A 108.8 2_655 . ?
P1 C1 H1A 108.8 . . ?
C1 C1 H1B 108.8 2_655 . ?
P1 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
P1 C3 H3A 109.5 . . ?
P1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
P1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C4 C4 P2 112.9(7) 17_765 . ?
C4 C4 H4A 109.0 17_765 . ?
P2 C4 H4A 109.0 . . ?
C4 C4 H4B 109.0 17_765 . ?
P2 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
P2 C5A H5A1 109.5 . . ?
P2 C5A H5A2 109.5 . . ?
P2 C5A H5A3 109.5 . . ?
P2 C6A H6A1 109.5 . . ?
P2 C6A H6A2 109.5 . . ?
P2 C6A H6A3 109.5 . . ?
F3A B1A F1A 110(2) . . ?
F3A B1A F4A 105.5(17) . . ?
F1A B1A F4A 109(2) . . ?
F3A B1A F2A 106(2) . . ?
F1A B1A F2A 116(2) . . ?
F4A B1A F2A 110.7(18) . . ?
P2 C5B H5B1 109.5 . . ?
P2 C5B H5B2 109.5 . . ?
H5B1 C5B H5B2 109.5 . . ?
P2 C5B H5B3 109.5 . . ?
H5B1 C5B H5B3 109.5 . . ?
H5B2 C5B H5B3 109.5 . . ?
P2 C6B H6B1 109.5 . . ?
P2 C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
P2 C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
F1B B1B F4B 104.5(15) . . ?
F1B B1B F3B 110.6(13) . . ?
F4B B1B F3B 108.6(10) . . ?
F1B B1B F2B 110.0(16) . . ?
F4B B1B F2B 110.9(9) . . ?
F3B B1B F2B 111.9(11) . . ?
O2 N1 O2 58(2) 3_655 . ?
O2 N1 O2 167(3) 3_655 4 ?
O2 N1 O2 124(2) . 4 ?
O2 N1 O2 124(2) 3_655 2_655 ?
O2 N1 O2 167(3) . 2_655 ?
O2 N1 O2 58(2) 4 2_655 ?
O2 N1 C7 115.7(19) 3_655 4 ?
O2 N1 C7 70.5(18) . 4 ?
O2 N1 C7 58.3(16) 4 4 ?
O2 N1 C7 115.3(19) 2_655 4 ?
O2 N1 C7 115.3(19) 3_655 . ?
O2 N1 C7 58.3(16) . . ?
O2 N1 C7 70.5(18) 4 . ?
O2 N1 C7 115.7(19) 2_655 . ?
C7 N1 C7 49(3) 4 . ?
O2 N1 C7 58.3(16) 3_655 3_655 ?
O2 N1 C7 115.3(19) . 3_655 ?
O2 N1 C7 115.7(19) 4 3_655 ?
O2 N1 C7 70.5(18) 2_655 3_655 ?
C7 N1 C7 131(3) 4 3_655 ?
C7 N1 C7 174(3) . 3_655 ?
O2 N1 C7 70.5(18) 3_655 2_655 ?
O2 N1 C7 115.7(19) . 2_655 ?
O2 N1 C7 115.3(19) 4 2_655 ?
O2 N1 C7 58.3(16) 2_655 2_655 ?
C7 N1 C7 174(3) 4 2_655 ?
C7 N1 C7 131(3) . 2_655 ?
C7 N1 C7 49(3) 3_655 2_655 ?
O2 O2 N1 60.9(10) 3_655 . ?
O2 O2 C7 128.9(16) 3_655 . ?
N1 O2 C7 69.5(14) . . ?
O2 O2 C7 111(2) 3_655 4 ?
N1 O2 C7 61.6(13) . 4 ?
C7 O2 C7 49(3) . 4 ?
C7 C7 O2 76(3) 4 . ?
C7 C7 N1 65.4(13) 4 . ?
O2 C7 N1 52.2(10) . . ?
C7 C7 O2 55(2) 4 4 ?
O2 C7 O2 97.1(16) . 4 ?
N1 C7 O2 47.9(9) . 4 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C1 C1 P1 54.2(18) . . 2_655 2_655 ?
P2 C4 C4 P2 180.000(1) . . 17_765 17_765 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.635
_refine_diff_density_min         -1.554
_refine_diff_density_rms         0.113


#===END
