Haloplumbate Salts as Reagents for the Non-Aqueous Electrodeposition of Lead
Bartlett, Philip N.; Burt, Jennifer; Hasan, Mahboba M.; Hector, Andrew L.; Levason, W.; Reid, Gillian; Richardson, Peter W.; RSC Adv.  (2016) –; doi:10.1039/C6RA12942K

data_7226048
_publ_section_title
;
 Haloplumbate Salts as Reagents for the Non-Aqueous Electrodeposition of
 Lead
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA12942K
_journal_year                    2016
_chemical_formula_moiety         'C24 H20 P, Br3 Pb'
_chemical_formula_sum            'C24 H20 Br3 P Pb'
_chemical_formula_weight         786.29
_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
;
2016-05-18 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                69.065(9)
_cell_angle_beta                 86.790(12)
_cell_angle_gamma                73.933(9)
_cell_formula_units_Z            2
_cell_length_a                   7.402(2)
_cell_length_b                   12.192(3)
_cell_length_c                   14.520(4)
_cell_measurement_reflns_used    3193
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.8
_cell_volume                     1174.7(5)
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10181
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    12.361
_exptl_absorpt_correction_T_max  0.5242
_exptl_absorpt_correction_T_min  0.4025
_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    2.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.751
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.855
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.855
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0087P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0410
_refine_ls_wR_factor_ref         0.0415
_reflns_number_gt                4549
_reflns_number_total             5254
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6ra12942k2.cif
_cod_data_source_block           2015JEBR18
_cod_database_code               7226048