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_1561559
_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 H14 N2 O8 Pb2, 8(H2 O)'
_chemical_formula_sum            'C11 H30 N2 O16 Pb2'
_chemical_formula_weight         860.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 108.208(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4941(3)
_cell_length_b                   22.7391(6)
_cell_length_c                   9.7704(3)
_cell_measurement_reflns_used    3193
_cell_measurement_temperature    153.00(10)
_cell_measurement_theta_max      28.4750
_cell_measurement_theta_min      3.4560
_cell_volume                     2214.73(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153.00(10)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_details
;
  1 omega  -87.00   47.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6309   19.0000   60.0000 134

  2 omega   73.00   99.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809 -178.0000   60.0000 26

  3 omega    4.00   82.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809   57.0000   90.0000 78
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0065068000
_diffrn_orient_matrix_UB_12      -0.0282867000
_diffrn_orient_matrix_UB_13      0.0278193000
_diffrn_orient_matrix_UB_21      0.0510837000
_diffrn_orient_matrix_UB_22      -0.0108174000
_diffrn_orient_matrix_UB_23      -0.0265574000
_diffrn_orient_matrix_UB_31      0.0491274000
_diffrn_orient_matrix_UB_32      0.0075094000
_diffrn_orient_matrix_UB_33      0.0660315000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9342
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.760
_diffrn_reflns_theta_min         3.377
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    15.262
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.717
_refine_diff_density_min         -2.434
_refine_diff_density_rms         0.260
_refine_ls_extinction_coef       0.00064(7)
_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   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5008
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0106P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4395
_reflns_number_total             5008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Cif3.cif
_cod_data_source_block           3
_cod_original_cell_volume        2214.74(12)
_cod_database_code               1561559
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H,H,H,H,H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O3W-H3WA = O3W-H3WB = O4W-H4WA = O4W-H4WB
 0.85 with sigma of 0.01
 O7W-H7WA = O7W-H7WB = O8W-H8WA = O8W-H8WB
 0.85 with sigma of 0.01
 H3WA-H3WB = H4WA-H4WB = H7WA-H7WB = H8WA-H8WB
 1.39 with sigma of 0.01
 H7WB-H8WB
 1.8 with sigma of 0.01
3.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C4(H4A,H4B), C6(H6A,H6B), C9(H9A,H9B), C10(H10A,H10B), C8(H8A,
 H8B), C2(H2A,H2B)
;
_shelx_res_checksum              69812
_shelx_hkl_checksum              16515