Syntheses and molecular structures of some saturated N-heterocyclic plumbylenes
Charmant, Jonathan P. H.; Haddow, Mairi F.; Hahn, F. Ekkehardt; Heitmann, Dennis; Fröhlich, Roland; Mansell, Stephen M.; Russell, Christopher A.; Wass, Duncan F.; Dalton Transactions  (2008) 6055–6059; doi:10.1039/b808717b

data_7004571
_publ_section_title
;
 Syntheses and molecular structures of some saturated N-heterocyclic
 plumbylenes
;
_journal_issue                   43
_journal_name_full               'Dalton Transactions'
_journal_page_first              6055
_journal_page_last               6059
_journal_paper_doi               10.1039/b808717b
_journal_year                    2008
_chemical_formula_sum            'C26 H38 N2 Pb'
_chemical_formula_weight         585.77
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 102.915(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.2881(5)
_cell_length_b                   6.5360(1)
_cell_length_c                   20.2042(6)
_cell_measurement_reflns_used    2864
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      0.41
_cell_volume                     2611.36(11)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9680
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    6.474
_exptl_absorpt_correction_T_max  0.6974
_exptl_absorpt_correction_T_min  0.2103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.518
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         3178
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0103P)^2^+39.4163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1216
_reflns_number_gt                2565
_reflns_number_total             3178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b808717b.txt
_cod_data_source_block           plumbylene-1
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7004571