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_7056095
_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 Br2 N4 O18 Pb5, 2(H2 O)'
_chemical_formula_sum            'C20 H32 Br2 N4 O20 Pb5'
_chemical_formula_weight         1844.27
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-08-09
_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                72.365(12)
_cell_angle_beta                 80.702(11)
_cell_angle_gamma                75.351(11)
_cell_formula_units_Z            1
_cell_length_a                   7.5998(10)
_cell_length_b                   8.8154(12)
_cell_length_c                   13.7290(18)
_cell_measurement_reflns_used    1367
_cell_measurement_temperature    176.8(3)
_cell_measurement_theta_max      27.5690
_cell_measurement_theta_min      3.2190
_cell_volume                     844.5(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      176.8(3)
_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  -59.00    7.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747  -38.0000 -120.0000 66

  2 omega  -44.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747   57.0000 -180.0000 87

  3 omega  -12.00   45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747   57.0000   90.0000 57

  4 omega  -91.00   13.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747  -77.0000   30.0000 104

  5 omega   -1.00   59.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809   57.0000  -90.0000 60

  6 omega   39.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809  -99.0000  -60.0000 26
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0387662000
_diffrn_orient_matrix_UB_12      0.0551913000
_diffrn_orient_matrix_UB_13      0.0300174000
_diffrn_orient_matrix_UB_21      -0.0069873000
_diffrn_orient_matrix_UB_22      -0.0665679000
_diffrn_orient_matrix_UB_23      0.0440350000
_diffrn_orient_matrix_UB_31      0.0885092000
_diffrn_orient_matrix_UB_32      -0.0016105000
_diffrn_orient_matrix_UB_33      0.0111334000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_unetI/netI     0.1296
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5116
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    27.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36994
_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    3.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.863
_refine_diff_density_min         -4.158
_refine_diff_density_rms         0.549
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         2969
_refine_ls_number_restraints     143
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0645
_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^)+(0.0294P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1439
_reflns_number_gt                2380
_reflns_number_total             2969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj00611j2.cif
_cod_data_source_block           exp_13255
_cod_original_cell_volume        844.46(19)
_cod_database_code               7056095
_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. Restrained distances
 H1WA-O1W = H1WB-O1W
 0.85 with sigma of 0.01
 H2WA-O2W = H2WB-O2W
 0.85 with sigma of 0.01
 H2WB-H2WA = H1WB-H1WA
 1.39 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
5.a Rotating group:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
;
_olex2_date_sample_data_collection 2016-05-14
_olex2_submission_special_instructions 'No special instructions were received'