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.
Farina, Paolo; Latter, Thomas; Levason, William; Reid, Gillian; Dalton transactions (Cambridge, England : 2003) 42 (2013) 4714–4724; doi:10.1039/c3dt32999b

data_7022771
_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 \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from \w-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/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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>2\s(I)
_cod_data_source_file            c3dt32999b.txt
_cod_data_source_block           12paf109ra
_cod_original_cell_volume        1020.8(5)
_cod_database_code               7022771