#------------------------------------------------------------------------------
#$Date: 2015-07-11 00:28:17 +0300 (Sat, 11 Jul 2015) $
#$Revision: 143539 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/52/7035228.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7035228
loop_
_publ_author_name
'Burt, Jennifer'
'Grantham, William'
'Levason, William'
'Reid, Gillian'
_publ_section_title
;
 Lead(ii) nitrate and hexafluorosilicate complexes with neutral
 diphosphine coordination.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11533
_journal_page_last               11541
_journal_paper_doi               10.1039/c5dt01448d
_journal_volume                  44
_journal_year                    2015
_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
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-16 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                93.580(6)
_cell_angle_beta                 93.952(3)
_cell_angle_gamma                100.854(6)
_cell_formula_units_Z            2
_cell_length_a                   6.6164(17)
_cell_length_b                   10.637(3)
_cell_length_c                   12.354(3)
_cell_measurement_reflns_used    2296
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_cell_volume                     849.3(4)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Superflip (Palatinus et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7661
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.15
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    10.250
_exptl_absorpt_correction_T_max  0.7485
_exptl_absorpt_correction_T_min  0.5339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.286
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3848
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0323P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0646
_reflns_number_gt                3557
_reflns_number_total             3848
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c5dt01448d1.cif
_cod_data_source_block           2014JEBR35a
_cod_depositor_comments
'Adding full bibliography for 7035226--7035231.cif.'
_cod_original_cell_volume        849.4(4)
_cod_database_code               7035228
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
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
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'
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
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_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_4
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
