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#$Date: 2016-03-25 15:42:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179932 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/27/7022771.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_7022771
loop_
_publ_author_name
'Farina, Paolo'
'Latter, Thomas'
'Levason, William'
'Reid, Gillian'
_publ_section_title
;
 Lead(II) tetrafluoroborate and hexafluorophosphate complexes with crown
 ethers, mixed O/S- and O/Se-donor macrocycles and unusual [BF(4)](-) and
 [PF(6)](-) coordination.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4714
_journal_page_last               4724
_journal_paper_doi               10.1039/c3dt32999b
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C12 H24 N O9 Pb 1+, F6 P 1-'
_chemical_formula_structural     '((C12 H24 O6) (N O3) Pb) (P F6)'
_chemical_formula_sum            'C12 H24 F6 N O9 P Pb'
_chemical_formula_weight         678.48
_chemical_name_systematic
;
1,4,7,10,13,16-hexaoxacyclooctadecane-nitrato-lead(II) hexafluorophosphate
;
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-22
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.958(5)
_cell_length_b                   8.475(3)
_cell_length_c                   9.296(3)
_cell_measurement_reflns_used    6273
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1020.9(6)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from ω-scans'
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_sigmaI/netI    0.1050
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6653
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.14
_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.441
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Jacobson, R.A. (1998). REQAB. Private communication to the
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.668
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.017(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2334
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                2041
_reflns_number_total             2334
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c3dt32999b.txt
_cod_data_source_block           12paf109ra
_cod_original_cell_volume        1020.8(5)
_cod_database_code               7022771
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-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 0.5000 0.13864(4) 0.49691(8) 0.02398(13) Uani 1 2 d S
O1 O 0.5000 -0.1647(11) 0.4030(11) 0.029(2) Uani 1 2 d S
O2 O 0.3159(4) 0.0077(7) 0.4162(7) 0.0260(14) Uani 1 1 d .
O3 O 0.3149(5) 0.2892(8) 0.5746(7) 0.0304(15) Uani 1 1 d .
O4 O 0.5000 0.4449(12) 0.6104(10) 0.029(2) Uani 1 2 d S
C1 C 0.4111(6) -0.2098(12) 0.3231(11) 0.028(2) Uani 1 1 d .
H1A H 0.4101 -0.3257 0.3097 0.033 Uiso 1 1 calc R
H1B H 0.4122 -0.1593 0.2271 0.033 Uiso 1 1 calc R
C2 C 0.3168(7) -0.1582(11) 0.4050(12) 0.030(2) Uani 1 1 d .
H2A H 0.2539 -0.1945 0.3545 0.036 Uiso 1 1 calc R
H2B H 0.3174 -0.2057 0.5023 0.036 Uiso 1 1 calc R
C3 C 0.2260(6) 0.0640(10) 0.487(2) 0.030(2) Uani 1 1 d .
H3A H 0.2240 0.0251 0.5872 0.036 Uiso 1 1 calc R
H3B H 0.1634 0.0262 0.4365 0.036 Uiso 1 1 calc R
C4 C 0.2299(6) 0.2392(10) 0.4850(19) 0.028(2) Uani 1 1 d .
H4A H 0.2399 0.2775 0.3853 0.034 Uiso 1 1 calc R
H4B H 0.1643 0.2832 0.5221 0.034 Uiso 1 1 calc R
C5 C 0.3177(7) 0.4544(11) 0.5883(12) 0.031(2) Uani 1 1 d .
H5A H 0.2529 0.4929 0.6324 0.038 Uiso 1 1 calc R
H5B H 0.3252 0.5040 0.4925 0.038 Uiso 1 1 calc R
C6 C 0.4090(7) 0.4973(13) 0.6828(13) 0.033(2) Uani 1 1 d .
H6A H 0.4116 0.6128 0.6980 0.039 Uiso 1 1 calc R
H6B H 0.4029 0.4450 0.7777 0.039 Uiso 1 1 calc R
N1 N 0.5000 -0.0532(14) 0.7480(12) 0.025(3) Uani 1 2 d S
O5 O 0.4167(5) -0.0088(10) 0.7025(9) 0.044(2) Uani 1 1 d .
O6 O 0.5000 -0.1576(12) 0.8519(13) 0.042(3) Uani 1 2 d S
P1 P 0.5000 0.3214(5) 0.1269(4) 0.0264(8) Uani 1 2 d S
F1 F 0.5000 0.5013(10) 0.0800(10) 0.041(2) Uani 1 2 d S
F2 F 0.5000 0.1401(9) 0.1769(10) 0.042(2) Uani 1 2 d S
F3 F 0.4131(5) 0.2865(8) 0.0145(12) 0.066(2) Uani 1 1 d .
F4 F 0.4141(6) 0.3581(8) 0.2475(9) 0.057(2) Uani 1 1 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'
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'
N N 0.0061 0.0033 '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
O5 Pb1 O5 50.6(3) . 4_655
O5 Pb1 O1 77.0(3) . .
O5 Pb1 O1 77.0(3) 4_655 .
O5 Pb1 O2 68.6(2) . .
O5 Pb1 O2 112.3(2) 4_655 .
O1 Pb1 O2 61.82(13) . .
O5 Pb1 O2 112.3(2) . 4_655
O5 Pb1 O2 68.6(2) 4_655 4_655
O1 Pb1 O2 61.82(13) . 4_655
O2 Pb1 O2 121.4(3) . 4_655
O5 Pb1 O4 100.0(3) . .
O5 Pb1 O4 100.0(3) 4_655 .
O1 Pb1 O4 176.6(3) . .
O2 Pb1 O4 118.62(13) . .
O2 Pb1 O4 118.62(13) 4_655 .
O5 Pb1 O3 70.5(2) . .
O5 Pb1 O3 113.3(2) 4_655 .
O1 Pb1 O3 120.82(15) . .
O2 Pb1 O3 60.7(2) . .
O2 Pb1 O3 176.87(19) 4_655 .
O4 Pb1 O3 58.85(14) . .
C1 O1 C1 108.2(10) . 4_655
C1 O1 Pb1 115.0(6) . .
C1 O1 Pb1 115.0(6) 4_655 .
C2 O2 C3 112.1(7) . .
C2 O2 Pb1 114.7(5) . .
C3 O2 Pb1 116.9(6) . .
C5 O3 C4 111.4(7) . .
C5 O3 Pb1 116.9(5) . .
C4 O3 Pb1 111.7(6) . .
C6 O4 C6 111.3(11) 4_655 .
C6 O4 Pb1 117.7(6) 4_655 .
C6 O4 Pb1 117.7(6) . .
O1 C1 C2 108.4(8) . .
O1 C1 H1A 110.0 . .
C2 C1 H1A 110.0 . .
O1 C1 H1B 110.0 . .
C2 C1 H1B 110.0 . .
H1A C1 H1B 108.4 . .
O2 C2 C1 109.5(8) . .
O2 C2 H2A 109.8 . .
C1 C2 H2A 109.8 . .
O2 C2 H2B 109.8 . .
C1 C2 H2B 109.8 . .
H2A C2 H2B 108.2 . .
O2 C3 C4 107.6(8) . .
O2 C3 H3A 110.2 . .
C4 C3 H3A 110.2 . .
O2 C3 H3B 110.2 . .
C4 C3 H3B 110.2 . .
H3A C3 H3B 108.5 . .
O3 C4 C3 108.2(8) . .
O3 C4 H4A 110.1 . .
C3 C4 H4A 110.1 . .
O3 C4 H4B 110.1 . .
C3 C4 H4B 110.1 . .
H4A C4 H4B 108.4 . .
O3 C5 C6 108.1(8) . .
O3 C5 H5A 110.1 . .
C6 C5 H5A 110.1 . .
O3 C5 H5B 110.1 . .
C6 C5 H5B 110.1 . .
H5A C5 H5B 108.4 . .
O4 C6 C5 107.2(9) . .
O4 C6 H6A 110.3 . .
C5 C6 H6A 110.3 . .
O4 C6 H6B 110.3 . .
C5 C6 H6B 110.3 . .
H6A C6 H6B 108.5 . .
O5 N1 O5 124.6(13) . 4_655
O5 N1 O6 117.7(6) . .
O5 N1 O6 117.7(6) 4_655 .
N1 O5 Pb1 92.2(7) . .
F3 P1 F3 92.1(8) . 4_655
F3 P1 F1 89.9(4) . .
F3 P1 F1 89.9(4) 4_655 .
F3 P1 F2 90.7(4) . .
F3 P1 F2 90.7(4) 4_655 .
F1 P1 F2 179.1(5) . .
F3 P1 F4 177.7(5) . 4_655
F3 P1 F4 90.2(5) 4_655 4_655
F1 P1 F4 90.3(4) . 4_655
F2 P1 F4 89.0(4) . 4_655
F3 P1 F4 90.2(5) . .
F3 P1 F4 177.7(5) 4_655 .
F1 P1 F4 90.3(4) . .
F2 P1 F4 89.0(4) . .
F4 P1 F4 87.4(7) 4_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O5 2.525(7) .
Pb1 O5 2.525(7) 4_655
Pb1 O1 2.715(9) .
Pb1 O2 2.736(6) .
Pb1 O2 2.736(6) 4_655
Pb1 O4 2.801(10) .
Pb1 O3 2.811(6) .
O1 C1 1.423(10) .
O1 C1 1.423(10) 4_655
O2 C2 1.410(10) .
O2 C3 1.420(10) .
O3 C5 1.406(12) .
O3 C4 1.445(13) .
O4 C6 1.429(10) 4_655
O4 C6 1.429(10) .
C1 C2 1.504(13) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.486(13) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.517(14) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
N1 O5 1.219(8) .
N1 O5 1.219(8) 4_655
N1 O6 1.310(16) .
P1 F3 1.564(9) .
P1 F3 1.564(9) 4_655
P1 F1 1.586(9) .
P1 F2 1.605(9) .
P1 F4 1.610(7) 4_655
P1 F4 1.610(7) .
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
Pb1 F2 2.975(9)
Pb1 F4 3.174(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
C1 O1 C1 C2 -178.4(5) 4_655
Pb1 O1 C1 C2 -48.4(10) .
C3 O2 C2 C1 177.3(10) .
Pb1 O2 C2 C1 -46.4(9) .
O1 C1 C2 O2 63.1(11) .
C2 O2 C3 C4 -176.7(9) .
Pb1 O2 C3 C4 48.0(13) .
C5 O3 C4 C3 -174.7(8) .
Pb1 O3 C4 C3 52.5(11) .
O2 C3 C4 O3 -66.9(14) .
C4 O3 C5 C6 -179.7(10) .
Pb1 O3 C5 C6 -49.6(9) .
C6 O4 C6 C5 172.8(6) 4_655
Pb1 O4 C6 C5 -46.9(10) .
O3 C5 C6 O4 62.2(11) .
