Crystal structure of bis[(μ2-4⋯O,O′:O′)-(4-hydroxybenzoato-κ2 O,O′)-(1,10-phenanthroline-κ2 N,N′)]-di-lead(II)μ-4-hydroxybenzoato-κ3 O,O′:O′;κ3 O,O′:O′-bis-[(4-hydroxybenzoato-κ2 O,O′)bis(1,10-phenanthroline-κ2 N,N′)di-lead(II)] monohydrate, C52H36N4O12Pb2 ⋅ H2O
Dai, Ben-Cai; Liu, Chang-Chun; Zhou, Yang; Chen, Jin; Fu, Yang; Zhao, Pei-Zheng; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 589–591; doi:10.1515/ncrs-2019-0835

data_8105228
_publ_section_title
;
 Crystal structure of
 bis[(\m2-4&#x22EF;O,O&#x2032;:O&#x2032;)-(4-hydroxybenzoato-\k2
 O,O&#x2032;)-(1,10-phenanthroline-\k2
 N,N&#x2032;)]-di-lead(II)\m-4-hydroxybenzoato-\k3
 O,O&#x2032;:O&#x2032;;\k3
 O,O&#x2032;:O&#x2032;-bis-[(4-hydroxybenzoato-\k2
 O,O&#x2032;)bis(1,10-phenanthroline-\k2 N,N&#x2032;)di-lead(II)]
 monohydrate, C52H36N4O12Pb2 &#x22C5; H2O
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              589
_journal_page_last               591
_journal_paper_doi               10.1515/ncrs-2019-0835
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C26 H18 N2 O6 Pb, H2 O'
_chemical_formula_sum            'C26 H20 N2 O7 Pb'
_chemical_formula_weight         679.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 93.1490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.77670(10)
_cell_length_b                   7.99250(10)
_cell_length_c                   21.2490(2)
_cell_measurement_reflns_used    10012
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      71.3390
_cell_measurement_theta_min      4.1710
_cell_volume                     2336.20(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_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   -105.00 -17.00   1.00    1.00    --  -35.62 -39.00-175.00   88
  2  \w    -54.00  33.00   1.00    1.00    --  -35.62  39.00 -21.00   87
  3  \w    -33.00  54.00   1.00    1.00    --   35.62 -39.00-175.00   87
  4  \w     17.00 105.00   1.00    1.00    --   35.62  39.00 -21.00   88
  5  \w     89.00 176.00   1.00    1.00    --  107.12  39.00 -21.00   87
  6  \w     38.00 126.00   1.00    1.00    --  107.12 -39.00-175.00   88
  7  \w   -103.00 -19.00   1.00    1.00    --  -35.62 -57.00-180.00   84
  8  \w     17.00 105.00   1.00    1.00    --   35.62  38.00  60.00   88
  9  \w     57.00 108.00   1.00    1.00    --   35.62 178.00-150.00   51
 10  \w      1.00  75.00   1.00    1.00    --   35.62 -99.00 -60.00   74
 11  \w     38.00 110.00   1.00    1.00    --  107.12 -95.00   0.00   72
 12  \w     40.00 125.00   1.00    1.00    --  107.12 -61.00 120.00   85
 13  \w     89.00 174.00   1.00    1.00    --  107.12  61.00-150.00   85
 14  \w     40.00 134.00   1.00    1.00    --  107.12 -77.00-120.00   94
 15  \w    100.00 171.00   1.00    1.00    --  107.12 111.00 -60.00   71
 16  \w     40.00  66.00   1.00    1.00    --  107.12 -77.00 -30.00   26
 17  \w    104.00 130.00   1.00    1.00    --  107.12 -77.00 -30.00   26
 18  \w     40.00 115.00   1.00    1.00    --  107.12 -45.00   0.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1117346000
_diffrn_orient_matrix_UB_12      -0.0142772000
_diffrn_orient_matrix_UB_13      -0.0031505000
_diffrn_orient_matrix_UB_21      0.0030302000
_diffrn_orient_matrix_UB_22      -0.0951332000
_diffrn_orient_matrix_UB_23      -0.0629626000
_diffrn_orient_matrix_UB_31      0.0078358000
_diffrn_orient_matrix_UB_32      -0.1669230000
_diffrn_orient_matrix_UB_33      0.0360216000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13530
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.421
_diffrn_reflns_theta_min         3.732
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.489
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.932
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.7854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0582
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4280
_reflns_number_total             4473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0835_suppl.cif
_cod_data_source_block           mxf-20
_cod_database_code               8105228
_chemical_oxdiff_formula         'C1 H1 O1 Pb1 N1'
_diffrn_oxdiff_digest_frames
;
011db6dba4491c76faf19e2d858ac4944800035fead
;
_diffrn_oxdiff_digest_hkl
;
01247dca86dc5c7fee92fa7b9367c029dc0172
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C5(H5), C6(H6A), C8(H8), C9(H9), C10(H10), C14(H14),
 C15(H15), C17(H17), C18(H18), C21(H21), C22(H22), C24(H24), C25(H25)
2.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6)
;