Crystal structure of diaqua-bis(μ2-5-chloro-salicylato-κ3 O,O′:O′)-bis(5-chloro-salicylato-κ2 O,O′)-bis(1,10-phenanthroline-κ2 N,N′) dilead(II) – water (1/2), C52H36C14N4O14Pb2·2(H2O)
Tang, Zhiwei; Wen, Decai; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 235–237; doi:10.1515/ncrs-2020-0473

data_8104931
_publ_section_title
;
 Crystal structure of diaqua-bis(\m2-5-chloro-salicylato-\k3
 O,O&#x2032;:O&#x2032;)-bis(5-chloro-salicylato-\k2
 O,O&#x2032;)-bis(1,10-phenanthroline-\k2 N,N&#x2032;) dilead(II) -- water
 (1/2), C52H36C14N4O14Pb2&#x00B7;2(H2O)
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              235
_journal_page_last               237
_journal_paper_doi               10.1515/ncrs-2020-0473
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C52 H36 Cl4 N4 O14 Pb2, 2(H2 O)'
_chemical_formula_sum            'C52 H40 Cl4 N4 O16 Pb2'
_chemical_formula_weight         1533.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                63.504(4)
_cell_angle_beta                 79.400(4)
_cell_angle_gamma                77.198(4)
_cell_formula_units_Z            1
_cell_length_a                   9.1186(4)
_cell_length_b                   12.8031(6)
_cell_length_c                   13.0111(6)
_cell_measurement_reflns_used    5030
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.6000
_cell_measurement_theta_min      2.2950
_cell_volume                     1319.34(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1151
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     -1.00  83.00   1.00    9.54    --   16.03  57.00 120.00   84
  2  \w      2.00  38.00   1.00    9.54    --   16.03  57.00 -30.00   36
  3  \w    -10.00  25.00   1.00    9.54    --   16.03  77.00-150.00   35
  4  \w      0.00  28.00   1.00    9.54    --   16.03 -57.00 -30.00   28
  5  \w    -35.00  -2.00   1.00    9.54    --  -17.44 -77.00   0.00   33
  6  \w    -35.00  52.00   1.00    9.54    --  -17.44  38.00   0.00   87
  7  \w    -87.00   0.00   1.00    9.54    --  -17.44 -38.00-180.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0523364000
_diffrn_orient_matrix_UB_12      -0.0488365000
_diffrn_orient_matrix_UB_13      -0.0030323000
_diffrn_orient_matrix_UB_21      0.0181314000
_diffrn_orient_matrix_UB_22      0.0340154000
_diffrn_orient_matrix_UB_23      -0.0596945000
_diffrn_orient_matrix_UB_31      0.0579338000
_diffrn_orient_matrix_UB_32      0.0197159000
_diffrn_orient_matrix_UB_33      0.0131658000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11401
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.271
_diffrn_reflns_theta_min         1.757
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.650
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent light colourless'
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0139P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0554
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5334
_reflns_number_total             6095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0473_suppl.cif
_cod_data_source_block           exp_41
_cod_original_cell_volume        1319.34(12)
_cod_database_code               8104931
_chemical_oxdiff_formula         'Pb C H O N Cl'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24)
2.b Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6)
;