Low-Coordinate Tin and Lead Cations
Taylor, Morgan J.; Saunders, Amy J.; Coles, Martyn P.; Fulton, J. Robin; Organometallics 30 (2011) 1334–; doi:10.1021/om100712a

data_4063638
_publ_section_title
;
 Low-Coordinate Tin and Lead Cations
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1334
_journal_paper_doi               10.1021/om100712a
_journal_volume                  30
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C29.64 H42.28 Cl 1.28 Pb, C24 B F20, C5 H12'
_chemical_formula_sum            'C58.64 H54.28 B Cl1.28 F20 N2 Pb'
_chemical_formula_weight         1430.40
_chemical_name_systematic
;
'C29 H41 N2 Pb, C24 B F20, C H2 Cl2, C5 H12'
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2010-11-24T12:58:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 126.654(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7961(4)
_cell_length_b                   18.4707(3)
_cell_length_c                   22.4317(4)
_cell_measurement_reflns_used    62882
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     5915.4(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.102293E-1
_diffrn_orient_matrix_UB_12      -0.74909E-2
_diffrn_orient_matrix_UB_13      -0.549324E-1
_diffrn_orient_matrix_UB_21      0.389256E-1
_diffrn_orient_matrix_UB_22      0.382003E-1
_diffrn_orient_matrix_UB_23      -0.31081E-2
_diffrn_orient_matrix_UB_31      0.415558E-1
_diffrn_orient_matrix_UB_32      -0.376264E-1
_diffrn_orient_matrix_UB_33      0.77807E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            92559
_diffrn_reflns_theta_full        27.1
_diffrn_reflns_theta_max         27.1
_diffrn_reflns_theta_min         3.45
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.042
_exptl_absorpt_correction_T_max  0.7079
_exptl_absorpt_correction_T_min  0.6246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            'Pale orange'
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rhombohedral
_exptl_crystal_F_000             2668
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.636
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         13031
_refine_ls_number_restraints     750
_refine_ls_restrained_S_all      1.01
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+21.8082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1318
_reflns_number_gt                10117
_reflns_number_total             13031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100712a_si_001.cif
_cod_data_source_block           (5)-oct309b-revised
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4063638