Crystal structures of three lead(II) acetate-bridged diaminobenzene coordination polymers
Geiger, David K.; Parsons, Dylan E.; Zick, Patricia L.; Acta Crystallographica Section E 70 (2014) 566–572; doi:10.1107/S1600536814025380

data_2240238
_publ_section_title
;
 Crystal structures of three lead(II) acetate-bridged diaminobenzene
 coordination polymers
;
_journal_coeditor_code           ZL2608
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              566
_journal_page_last               572
_journal_paper_doi               10.1107/S1600536814025380
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Pb2 (C2 H3 O2)4 (C6 H8 N2)]'
_chemical_formula_moiety         'C14 H20 N2 O8 Pb2'
_chemical_formula_sum            'C14 H20 N2 O8 Pb2'
_chemical_formula_weight         758.70
_chemical_name_systematic
Poly[tris(acetato-\k^2^<i>O</i>,<i>O</i>')(\m~3~-acetato-\k^3^<i>O</i>,<i>O</i>':<i>O</i>)tetrakis(\m~2~-acetato-\k^4^<i>O</i>,<i>O</i>':<i>O</i>:<i>O</i>')bis(benzene-1,2-diamine-\k<i>N</i>)tetralead(II)]
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.941(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.1447(14)
_cell_length_b                   29.694(4)
_cell_length_c                   11.8597(14)
_cell_measurement_reflns_used    426
_cell_measurement_temperature    200.(2)
_cell_measurement_theta_max      26.4955
_cell_measurement_theta_min      0.0997
_cell_volume                     3809.1(8)
_computing_cell_refinement
;
APEX2 (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009), Mercury (Macrae <i>et al.</i>, 2006) and
ORTEP-3 for
Windows (Farrugia, 2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200.(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART X2S benchtop'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'doubly curved silicon crystal'
_diffrn_radiation_type           'Mo Ka'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            26670
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         26.32
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    17.699
_exptl_absorpt_correction_T_max  0.27
_exptl_absorpt_correction_T_min  0.12
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            'clear colorless'
_exptl_crystal_density_diffrn    2.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.123
_refine_diff_density_min         -1.971
_refine_ls_extinction_coef       0.000185(12)
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         7708
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0015P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                5239
_reflns_number_total             7708
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2608sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-10-17
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C28 H40 N4 O16 Pb4'
_cod_original_formula_weight         1517.40
_cod_original_formula_moiety         'C28 H40 N4 O16 Pb4'
_cod_original_formula_iupac          '[Pb4 (C2 H3 O2)8 (C6 H8 N2)2]'
_cod_original_formula_units_Z            4
_cod_database_code               2240238
_cod_database_fobs_code          2240238
_shelx_hkl_checksum              4185
_shelx_res_checksum              77656