Crystal structure of diaqua-bis(μ2-6-phenylpyridine-2-carboxylate-κ3N,O:O)-bis(6-phenylpyridine-2-carboxylato-κ2N,O)lead(II) – N,N-dimethylformamide – water (1/2/4), C54H58N6O16Pb2
Tai, Xi-Shi; Liang, Lei; Li, Xiang-Tao; Cao, Shu-Hua; Wang, Li-Hua; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 1199–1201; doi:10.1515/ncrs-2021-0277

data_8104565
_publ_section_title
;
 Crystal structure of
 diaqua-bis(\m2-6-phenylpyridine-2-carboxylate-\k3N,O:O)-bis(6-phenylpyridine-2-carboxylato-\k2N,O)lead(II)
 -- N,N-dimethylformamide -- water (1/2/4), C54H58N6O16Pb2
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_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1199
_journal_page_last               1201
_journal_paper_doi               10.1515/ncrs-2021-0277
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C24 H16 N2 O4 Pb, 3(H2 O), C3 H7 N O'
_chemical_formula_sum            'C27 H29 N3 O8 Pb'
_chemical_formula_weight         730.72
_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
_cell_angle_alpha                63.395(5)
_cell_angle_beta                 74.291(5)
_cell_angle_gamma                69.113(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4690(6)
_cell_length_b                   12.9374(6)
_cell_length_c                   13.2303(7)
_cell_measurement_reflns_used    5305
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      28.7990
_cell_measurement_theta_min      2.4340
_cell_volume                     1341.90(14)
_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      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -77.00  15.00   1.00    1.20    --  -11.27 -77.00  60.00   92
  2  \w    -53.00  38.00   1.00    1.20    --   11.90 -57.00-180.00   91
  3  \w    -12.00  85.00   1.00    1.20    --   11.90  57.00 -30.00   97
;
_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      -0.0798941000
_diffrn_orient_matrix_UB_12      0.0079081000
_diffrn_orient_matrix_UB_13      0.0141569000
_diffrn_orient_matrix_UB_21      0.0114469000
_diffrn_orient_matrix_UB_22      -0.0620319000
_diffrn_orient_matrix_UB_23      0.0147325000
_diffrn_orient_matrix_UB_31      0.0054718000
_diffrn_orient_matrix_UB_32      -0.0123705000
_diffrn_orient_matrix_UB_33      0.0569433000
_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  0.0349
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8804
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.323
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.341
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76259
_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    1.808
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.915
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         4741
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0484
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4320
_reflns_number_total             4741
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0277_suppl.cif
_cod_data_source_block           w008
_cod_original_cell_volume        1341.90(15)
_cod_database_code               8104565
_reflns_odcompleteness_completeness 99.95
_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 C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O7-H7B
 0.955 with sigma of 0.02
 O7-H7B = O7-H7A = O8-H8A = O8-H8B
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
4.a Free rotating group:
 O6(H6A,H6B)
4.b 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),
  C3S(H3S)
4.c Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              6938