The crystal structure of tetrakis(6-phenylpyridine-2-carboxylate-κ 2 N,O)-bis(μ2-6-phenylpyridine-2-carboxylate-κ 2 O:O′)-bis(μ2-6-phenylpyridine-2-carboxylate-κ 3N,O:O)tetralead(II) C48H32N4O8Pb2
Li-Hua, Wang; Hao-Wen, Tai; Qiu-Shi, Li; Yu-Pei, Xia; Xi-Shi, Tai; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 1113–1116; doi:10.1515/ncrs-2022-0378

data_8107307
_publ_section_title
;
 The crystal structure of tetrakis(6-phenylpyridine-2-carboxylate-\k 2
 N,O)-bis(\m2-6-phenylpyridine-2-carboxylate-\k 2
 O:O&#x2032;)-bis(\m2-6-phenylpyridine-2-carboxylate-\k
 3N,O:O)tetralead(II) C48H32N4O8Pb2
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1113
_journal_page_last               1116
_journal_paper_doi               10.1515/ncrs-2022-0378
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C48 H32 N4 O8 Pb2'
_chemical_formula_sum            'C48 H32 N4 O8 Pb2'
_chemical_formula_weight         1207.15
_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   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                76.089(7)
_cell_angle_beta                 77.068(7)
_cell_angle_gamma                74.717(7)
_cell_formula_units_Z            2
_cell_length_a                   9.2712(8)
_cell_length_b                   14.5959(13)
_cell_length_c                   16.6178(13)
_cell_measurement_reflns_used    5640
_cell_measurement_temperature    249.99(10)
_cell_measurement_theta_max      28.4060
_cell_measurement_theta_min      2.4640
_cell_volume                     2074.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      249.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -58.00  39.00   1.00    4.00    --   12.05 -57.00 -30.00   97
  2  \w    -16.00  79.00   1.00    4.00    --   12.05  77.00-120.00   95
  3  \w    -11.00  81.00   1.00    4.00    --   12.05  57.00 120.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0628763000
_diffrn_orient_matrix_UB_12      -0.0392960000
_diffrn_orient_matrix_UB_13      0.0066517000
_diffrn_orient_matrix_UB_21      0.0362042000
_diffrn_orient_matrix_UB_22      0.0141835000
_diffrn_orient_matrix_UB_23      -0.0419027000
_diffrn_orient_matrix_UB_31      0.0348738000
_diffrn_orient_matrix_UB_32      0.0298444000
_diffrn_orient_matrix_UB_33      0.0138562000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13595
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.132
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.167
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    1.933
_exptl_crystal_description       needle
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.296
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7291
_refine_ls_number_restraints     533
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0960P)^2^+16.6046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1783
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5570
_reflns_number_total             7291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0378_suppl.cif
_cod_data_source_block           05
_cod_database_code               8107307
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
3. Rigid body (RIGU) restrains
 Pb1, Pb2, O1, O2, O3, O4, O5, O6, O7, O8, N1, N2, N3, N4, C1, C2, H2, C3, H3,
 C4, H4, C5, C6, C7, C8, H8, C9, H9, C10, H10, C11, H11, C12, H12, C13, C14,
 C15, H15, C16, H16, C17, H17, C18, C19, C20, H20, C21, H21, C22, H22, C23, H23,
  C24, H24, C25, C26, C27, H27, C28, H28, C29, H29, C30, C31, C32, H32, C33,
 H33, C34, H34, C35, H35, C36, H36, C37, C38, H38, C39, H39, C40, H40, C41, C42,
  C43, C44, H44, C45, H45, C46, H46, C47, H47, C48, H48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C27(H27), C28(H28), C29(H29), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C38(H38), C39(H39), C40(H40), C44(H44), C45(H45), C46(H46), C47(H47),
  C48(H48)
;
_shelx_res_checksum              72572