Halide assisted formations of polymeric ethylenediaminetetraacetato lead(II) complexes
Dai, Jun-Wei; zheng, jianmei; Li, Haiyan; Zhou, Jin-Mei; Dong, Xin; Zhou, Zhao-Hui; New J. Chem. 41 (2017) 5198–5204; doi:10.1039/C7NJ00611J

data_7056092
_publ_section_title
;
 Halide assisted formations of polymeric ethylenediaminetetraacetato
 lead(II) complexes
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              5198
_journal_page_last               5204
_journal_paper_doi               10.1039/C7NJ00611J
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C20 H22 N4 O16 Pb4, 2(H2 O)'
_chemical_formula_sum            'C20 H28 N4 O18 Pb4'
_chemical_formula_weight         1441.22
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-02-18 deposited with the CCDC.
2017-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.1011(5)
_cell_length_b                   9.06660(19)
_cell_length_c                   32.4789(8)
_cell_measurement_reflns_used    3847
_cell_measurement_temperature    175.6(8)
_cell_measurement_theta_max      27.2550
_cell_measurement_theta_min      3.6110
_cell_volume                     5624.8(2)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      175.6(8)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -91.00    3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747  -57.0000 -120.0000 94

  2 omega  -42.00   52.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747   77.0000    0.0000 94

  3 omega   -5.00   49.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747   63.0000  -89.0000 54

  4 omega  -92.00   13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747  -77.0000  150.0000 105

  5 omega  -81.00  -50.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747    0.0000 -150.0000 31

  6 omega  -29.00   -4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747    0.0000 -150.0000 25

  7 omega   23.00   52.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747    0.0000 -150.0000 29

  8 omega  -67.00  -32.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747  -57.0000 -180.0000 35

  9 omega    5.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809  -99.0000   60.0000 60
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0252562000
_diffrn_orient_matrix_UB_12      -0.0209116000
_diffrn_orient_matrix_UB_13      0.0149055000
_diffrn_orient_matrix_UB_21      -0.0213661000
_diffrn_orient_matrix_UB_22      0.0603505000
_diffrn_orient_matrix_UB_23      -0.0059188000
_diffrn_orient_matrix_UB_31      -0.0168555000
_diffrn_orient_matrix_UB_32      -0.0451561000
_diffrn_orient_matrix_UB_33      -0.0148328000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1117
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            46569
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.10
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    23.967
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15957
_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    3.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5184
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.285
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5515
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0132P)^2^+0.3905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                4153
_reflns_number_total             5515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj00611j2.cif
_cod_data_source_block           exp_10248
_cod_database_code               7056092
_shelxl_version_number           2014-7
_reflns_odcompleteness_completeness 99.67
_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
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.001
Uanis(O16) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.001
Uanis(C17) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.001
3.a Free rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C19(H19A,H19B), C10(H10A,H10B), C16(H16A,H16B), C20(H20A,H20B),
 C4(H4A,H4B), C12(H12A,H12B), C14(H14A,H14B), C2(H2A,H2B), C8(H8A,H8B),
 C18(H18A,H18B)
;
_olex2_submission_special_instructions 'No special instructions were received'