Thermally stable lead(ii) amidinates and guanidinates
Stasch, Andreas; Forsyth, Craig M.; Jones, Cameron; Junk, Peter C.; New Journal of Chemistry 32 (2008) 829–; doi:10.1039/b718537e

data_7051867
_publ_section_title
;
 Thermally stable lead(ii) amidinates and guanidinates
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              829
_journal_paper_doi               10.1039/b718537e
_journal_volume                  32
_journal_year                    2008
_chemical_formula_moiety         'C74 H112 Cl2 N6 Pb2, 2(C7 H8), C7 H8'
_chemical_formula_sum            'C95 H136 Cl2 N6 Pb2'
_chemical_formula_weight         1847.38
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                63.026(1)
_cell_angle_beta                 80.217(1)
_cell_angle_gamma                79.878(1)
_cell_formula_units_Z            1
_cell_length_a                   13.2064(3)
_cell_length_b                   13.3847(3)
_cell_length_c                   13.9367(4)
_cell_measurement_temperature    123(2)
_cell_volume                     2149.88(9)
_computing_cell_refinement       'Denzo SMN (Otwinoski and Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo SMN (Otwinoski and Minor, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Enraf Nonius KAPPA CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19429
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.021
_exptl_absorpt_correction_T_max  0.45
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             946
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.211
_refine_diff_density_min         -1.877
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         9765
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0410
_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/[\s^2^(Fo^2^)+(0.0531P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                8359
_reflns_number_total             9765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718537e.txt
_cod_data_source_block           pbcygcl
_cod_database_code               7051867