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_7056094
_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 H24 N4 O16 Pb4, 2(H2 O)'
_chemical_formula_sum            'C20 H28 N4 O18 Pb4'
_chemical_formula_weight         1441.22
_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             2017-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-18 deposited with the CCDC.
2017-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                71.442(7)
_cell_angle_beta                 89.744(5)
_cell_angle_gamma                76.903(6)
_cell_formula_units_Z            1
_cell_length_a                   8.4173(5)
_cell_length_b                   8.4523(6)
_cell_length_c                   11.0350(8)
_cell_measurement_reflns_used    2111
_cell_measurement_temperature    178.7(7)
_cell_measurement_theta_max      27.9920
_cell_measurement_theta_min      3.7350
_cell_volume                     722.96(9)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      178.7(7)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_details
;
  1 omega  -88.00    2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747  -57.0000  -90.0000 90

  2 omega  -44.00   50.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747   57.0000   60.0000 94

  3 omega    4.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747   57.0000 -180.0000 44

  4 omega  -91.00    3.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747  -57.0000  120.0000 94

  5 omega   67.00  102.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809 -178.0000    0.0000 35

  6 omega  -22.00    9.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809   99.0000  127.0000 31
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0143205000
_diffrn_orient_matrix_UB_12      -0.0763543000
_diffrn_orient_matrix_UB_13      -0.0164504000
_diffrn_orient_matrix_UB_21      -0.0187942000
_diffrn_orient_matrix_UB_22      -0.0456842000
_diffrn_orient_matrix_UB_23      0.0621881000
_diffrn_orient_matrix_UB_31      -0.0834710000
_diffrn_orient_matrix_UB_32      0.0196841000
_diffrn_orient_matrix_UB_33      -0.0220021000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5225
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.717
_diffrn_reflns_theta_min         3.051
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    23.309
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43887
_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    3.310
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.589
_refine_diff_density_min         -1.729
_refine_diff_density_rms         0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3250
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0081P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2730
_reflns_number_total             3250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00611j2.cif
_cod_data_source_block           exp_14372
_cod_database_code               7056094
_shelxl_version_number           2014-7
_reflns_odcompleteness_completeness 99.80
_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(C1) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
3.a Free rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C10(H10A,H10B), C8(H8A,H8B), C9(H9A,H9B), C6(H6A,H6B), C2(H2A,H2B)
;
_shelx_res_checksum              30785
_olex2_date_sample_data_collection 2016-08-07
_olex2_submission_special_instructions 'No special instructions were received'