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_7056093
_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 H28 Cl2 N4 O18 Pb5, 2(H2 O)'
_chemical_formula_sum            'C20 H32 Cl2 N4 O20 Pb5'
_chemical_formula_weight         1755.34
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-08
_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                72.888(4)
_cell_angle_beta                 81.027(4)
_cell_angle_gamma                75.571(4)
_cell_formula_units_Z            1
_cell_length_a                   7.5204(4)
_cell_length_b                   8.8464(4)
_cell_length_c                   13.5079(5)
_cell_measurement_reflns_used    98
_cell_measurement_temperature    173
_cell_measurement_theta_max      33.5373
_cell_measurement_theta_min      2.9949
_cell_volume                     828.46(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_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  -40.00  -14.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8810  135.0000  -57.0000 26

  2 omega  -94.00   -3.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8810  135.0000  122.0000 91

  3 omega   45.00   79.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       30.4435 -135.0000   57.0000 34

  4 omega   36.00   61.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       30.4435 -135.0000 -122.0000 25

  5 omega  -98.00    4.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8810  -77.0000  120.0000 102

  6 omega -101.00  -33.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8810  -38.0000 -150.0000 68

  7 omega  -25.00    3.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8810  -38.0000 -150.0000 28

  8 omega  -28.00   17.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       30.4435  -38.0000   30.0000 45

  9 omega   59.00  110.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       30.4435  179.0000   30.0000 51

 10 omega   81.00  110.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       30.4435  179.0000 -150.0000 29

 11 omega  -42.00   25.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       30.4435  -38.0000  -30.0000 67

 12 omega  -43.00   17.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       30.4435  -38.0000  120.0000 60
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0566527633
_diffrn_orient_matrix_UB_12      0.0537548651
_diffrn_orient_matrix_UB_13      0.0005578720
_diffrn_orient_matrix_UB_21      0.0066562722
_diffrn_orient_matrix_UB_22      0.0244469731
_diffrn_orient_matrix_UB_23      -0.0550665458
_diffrn_orient_matrix_UB_31      -0.0784539382
_diffrn_orient_matrix_UB_32      0.0618090237
_diffrn_orient_matrix_UB_33      -0.0001298519
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9640
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.808
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    25.570
_exptl_absorpt_correction_T_max  0.2342
_exptl_absorpt_correction_T_min  0.1141
_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    3.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.011
_refine_diff_density_min         -2.515
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3244
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0398P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2903
_reflns_number_total             3244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00611j2.cif
_cod_data_source_block           sad
_cod_database_code               7056093
_shelxl_version_number           2014-7
_shelx_estimated_absorpt_t_max   0.234
_shelx_estimated_absorpt_t_min   0.114
_reflns_odcompleteness_completeness 75.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups, {H1Wa,H1Wb} of C10
 At 1.2 times of:
  {H2a,H2b} of C2, {H4a,H4b} of C4, {H6a,H6b} of C6, {H9a,H9b} of C9, {H8a,
  H8b} of C8, {H10a,H10b} of C10
2. Restrained distances
 H1Wa-O1W = H1Wb-O1W
 0.85 with sigma of 0.01
 H1Wa-H1Wb
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4.a Free rotating group:
 O2W(H2Wa,H2Wb)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C4(H4a,H4b), C6(H6a,H6b), C9(H9a,H9b), C8(H8a,H8b), C10(H10a,H10b)
;
_shelx_res_checksum              23096
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'