C-Donor lariat ether 'scorpionates'
Arya, Pious; Channa, Asif; Cragg, Peter J.; Prince, Paul D.; Steed, Jonathan W.; New Journal of Chemistry 26 (2002) 440–; doi:10.1039/b108522k

data_7050728
_publ_section_title
;
 C-Donor lariat ether 'scorpionates'
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              440
_journal_paper_doi               10.1039/b108522k
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C26 H52 N6 O21 Pb2'
_chemical_formula_weight         1199.12
_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                90.671(5)
_cell_angle_beta                 96.212(4)
_cell_angle_gamma                96.610(4)
_cell_formula_units_Z            2
_cell_length_a                   7.6545(5)
_cell_length_b                   12.0537(4)
_cell_length_c                   21.6309(4)
_cell_measurement_temperature    100(2)
_cell_volume                     1970.28(15)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    RES2INS
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  KappaCCD
_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  0.105
_diffrn_reflns_av_sigmaI/netI    0.1309
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20988
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    8.621
_exptl_absorpt_correction_T_max  0.4793
_exptl_absorpt_correction_T_min  0.1818
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.356
_refine_diff_density_min         -4.349
_refine_diff_density_rms         0.320
_refine_ls_extinction_coef       0.0026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         7646
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0670
_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^)+(0.0973P)^2^+6.7496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.1892
_reflns_number_gt                5869
_reflns_number_total             7646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108522k.txt
_cod_data_source_block           alpbno3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050728