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_7051864
_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 H110 N6 O2 Pb2, 2(C7 H8), C7 H8'
_chemical_formula_sum            'C95 H134 N6 O2 Pb2'
_chemical_formula_weight         1806.46
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.058(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0458(2)
_cell_length_b                   24.5646(6)
_cell_length_c                   17.3771(4)
_cell_measurement_temperature    123(2)
_cell_volume                     4255.67(17)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0864
_diffrn_reflns_av_sigmaI/netI    0.0906
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35104
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.34
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.002
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORATV (Blessing, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.196
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8328
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+11.5693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                6160
_reflns_number_total             8328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718537e.txt
_cod_data_source_block           pbcygoab
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7051864