Lone-Pair Activity in Lead(II) Complexes with Unsymmetrical Lariat Ethers
Esteban-Gómez, David; Platas-Iglesias, Carlos; Enríquez-Pérez, Teresa; Avecilla, Fernando; de Blas, Andrés; Rodríguez-Blas, Teresa; Inorganic Chemistry 45 (2006) 5407–5416; doi:10.1021/ic060252m

data_4332330
_publ_section_title
;
 Lone-Pair Activity in Lead(II) Complexes with Unsymmetrical Lariat Ethers
;
_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5407
_journal_page_last               5416
_journal_paper_doi               10.1021/ic060252m
_journal_volume                  45
_journal_year                    2006
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C31 H39 N4 O4 Pb, Cl O4'
_chemical_formula_sum            'C31 H39 Cl N4 O8 Pb'
_chemical_formula_weight         838.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7050(18)
_cell_length_b                   14.721(2)
_cell_length_c                   16.220(2)
_cell_measurement_temperature    298(2)
_cell_volume                     3272.4(7)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1490
_diffrn_reflns_av_sigmaI/netI    0.2494
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20723
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    5.292
_exptl_absorpt_correction_T_max  0.7419
_exptl_absorpt_correction_T_min  0.4665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'North et al., 1968'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.936
_refine_diff_density_min         -1.579
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details 'Flack H D (1983), 1888 Friedel pairs'
_refine_ls_abs_structure_Flack   0.498(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7647
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.2302
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                3042
_reflns_number_total             7647
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060252msup1.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     P2ac2ab
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4332330