Transformations of lead 1,3-propylenediaminetetraacetate to its MOF products for the selective adsorption of methanol
Dai, Jun-Wei; Li, Xing; Zheng, Jian-Mei; Dong, Xin; Zhou, Zhao-Hui; Journal of Solid State Chemistry 237 (2016) 364–370; doi:10.1016/j.jssc.2016.02.026

data_1561557
_publ_section_title
;
 Transformations of lead 1,3-propylenediaminetetraacetate to its MOF
 products for the selective adsorption of methanol
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              364
_journal_page_last               370
_journal_paper_doi               10.1016/j.jssc.2016.02.026
_journal_volume                  237
_journal_year                    2016
_chemical_formula_moiety         'C11 H20 K2 N2 O11 Pb'
_chemical_formula_sum            'C11 H20 K2 N2 O11 Pb'
_chemical_formula_weight         641.68
_chemical_name_common            'Potassium lead propylenediaminetetraacetate'
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 99.580(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8983(3)
_cell_length_b                   9.8333(3)
_cell_length_c                   22.4579(7)
_cell_measurement_reflns_used    3193
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.4750
_cell_measurement_theta_min      3.4560
_cell_volume                     1937.65(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8049
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         3.112
_exptl_absorpt_coefficient_mu    9.194
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.200
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.415
_exptl_transmission_factor_min   0.399
_refine_diff_density_max         1.644
_refine_diff_density_min         -1.707
_refine_diff_density_rms         0.199
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4259
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0178P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0680
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3811
_reflns_number_total             4259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Cif1.cif
_cod_data_source_block           sda
_cod_depositor_comments
;

2022-09-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C22 H40 K4 N4 O22 Pb2'
_cod_original_formula_weight         1283.36
_cod_original_formula_moiety         'C22 H40 K4 N4 O22 Pb2'
_cod_original_formula_units_Z            2
_cod_database_code               1561557
_shelx_estimated_absorpt_t_max   0.460
_shelx_estimated_absorpt_t_min   0.460
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H,H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O1W-H1Wa = O1W-H1Wb
 0.85 with sigma of 0.01
 O2W-H2Wa = O2W-H2Wb = O3W-H3Wa = O3W-H3Wb
 0.85 with sigma of 0.01
 H2Wa-H2Wb = H3Wa-H3Wb
 1.39 with sigma of 0.01
 C11-H11a = C11-H11b
 0.99 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C9(H9a,H9b), C4(H4a,H4b), C10(H10a,H10b), C8(H8a,H8b), C6(H6a,H6b)
3.b Tetrahedral OH refined with riding coordinates:
 O3W(H3Wa)
;
_shelx_res_checksum              19467
_shelx_hkl_checksum              11943