Pb3[C6(CH3)3(CO2)3H6]2[DMF]3: first layered Pb-Kemp's triacid complex
Saet Byeol Kim; Dong Woo Lee; Suk-Kyu Chang; Kang Min Ok; Chem.Commun. 51 (2015) 13166–; doi:10.1039/C5cc05360A

data_7117640
_publ_section_title
;
 Pb3[C6(CH3)3(CO2)3H6]2[DMF]3: first layered Pb-Kemp's triacid complex
;
_journal_name_full               Chem.Commun.
_journal_page_first              13166
_journal_paper_doi               10.1039/C5cc05360A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C11  H17  N  O5  Pb'
_chemical_formula_sum            'C11 H17 N O5 Pb'
_chemical_formula_weight         450.46
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2015-06-29 deposited with the CCDC.
2015-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   14.4445(6)
_cell_length_b                   14.4445(6)
_cell_length_c                   34.0453(10)
_cell_measurement_temperature    173.0(2)
_cell_volume                     6151.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173.0(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART BREEZE'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1255
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            23965
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.734
_exptl_absorpt_coefficient_mu    12.353
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 

 SADABS(Blessing, 1995) 

;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3816
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.014
_refine_diff_density_max         2.013
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.253
_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   0.771
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.771
_refine_ls_R_factor_all          0.1398
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                1560
_reflns_number_total             3412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc05360a2.cif
_cod_data_source_block           Pb3(Kemp)2(DMF)3
_cod_original_cell_volume        6151.7(6)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C11  H17  N  O5  Pb'
_cod_database_code               7117640