A series of mixed-ligand 2D and 3D coordination polymers assembled from a novel multifunctional pyridine-tricarboxylate building block: hydrothermal syntheses, structural and topological diversity, and magnetic and luminescent properties
Gu, Jinzhong; Cui, Yanhui; Wu, Jiang; Kirillov, Alexander M.; RSC Adv.  (2015) –; doi:10.1039/C5RA13582F

data_7222044
_publ_section_title
;
 A series of mixed-ligand 2D and 3D coordination polymers assembled from a
 novel multifunctional pyridine-tricarboxylate building block:
 hydrothermal syntheses, structural and topological diversity, and
 magnetic and luminescent properties
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA13582F
_journal_year                    2015
_chemical_formula_moiety         'C45 H27 N5 O8 Pb2, H2 O'
_chemical_formula_sum            'C45 H29 N5 O9 Pb2'
_chemical_formula_weight         1198.11
_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             2015-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-24 deposited with the CCDC.
2015-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                65.656(8)
_cell_angle_beta                 66.949(5)
_cell_angle_gamma                82.089(5)
_cell_formula_units_Z            2
_cell_length_a                   11.5662(5)
_cell_length_b                   14.0642(12)
_cell_length_c                   14.1354(10)
_cell_measurement_reflns_used    3342
_cell_measurement_temperature    290.92(10)
_cell_measurement_theta_max      27.7790
_cell_measurement_theta_min      3.6670
_cell_volume                     1926.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      290.92(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega   -9.00   21.00   1.2000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2008  -99.0000 -120.0000 25

  2 omega   -6.00   20.40   1.2000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2008  -99.0000  120.0000 22

  3 omega   67.00   94.60   1.2000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3415  178.0000   90.0000 23

  4 omega  -47.00   40.60   1.2000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3415  -57.0000 -150.0000 73

  5 omega  -34.00   41.60   1.2000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3415  -57.0000  -30.0000 63

  6 omega  -52.00   38.00   1.2000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3415  -38.0000   90.0000 75

  7 omega   -1.00   29.00   1.2000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3415   57.0000  120.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0018791000
_diffrn_orient_matrix_UB_12      0.0438780000
_diffrn_orient_matrix_UB_13      0.0131126000
_diffrn_orient_matrix_UB_21      -0.0244090000
_diffrn_orient_matrix_UB_22      0.0302994000
_diffrn_orient_matrix_UB_23      -0.0419858000
_diffrn_orient_matrix_UB_31      -0.0620161000
_diffrn_orient_matrix_UB_32      -0.0149431000
_diffrn_orient_matrix_UB_33      0.0397853000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11989
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.794
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.566
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         6812
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0324P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.1025
_reflns_number_gt                5364
_reflns_number_total             6812
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra13582f2.cif
_cod_data_source_block           218_11pb
_cod_original_cell_volume        1926.9(2)
_cod_database_code               7222044
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Riding coordinates:
 O9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15),
 C16(H16), C17(H17), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C32(H32), C33(H33), C36(H36), C37(H37), C38(H38),
 C41(H41), C42(H42), C45(H45), C46(H46)
;
_olex2_date_sample_data_collection 2014-12-19
_olex2_submission_special_instructions 'No special instructions were received'