Structural‒Spectrochemical Correlations of Variable Dimensionality Crystalline Metal‒Organic Framework Materials in Hydrothermal Reactivity Patterns of Binary‒Ternary Systems of Pb(II) with (a)Cyclic (Poly)carboxylate and Aromatic Chelator Ligands
Gabriel, Catherine; Vangelis, Angelos A.; Raptopoulou, Catherine P.; Terzis, Aris; Psycharis, Vassilis; Zervou, Maria; Bertmer, Marko; Salifoglou, Athanasios; Crystal Growth & Design 15 (2015) 5310–; doi:10.1021/acs.cgd.5b00861

data_4516388
_publ_section_title
;
 Structural--Spectrochemical Correlations of Variable Dimensionality
 Crystalline Metal--Organic Framework Materials in Hydrothermal Reactivity
 Patterns of Binary--Ternary Systems of Pb(II) with (a)Cyclic
 (Poly)carboxylate and Aromatic Chelator Ligands
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5310
_journal_paper_doi               10.1021/acs.cgd.5b00861
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'C336 H380.6 N48 O130.3 Pb12'
_chemical_formula_weight         9662.57
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.1650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   24.6700(4)
_cell_length_b                   43.4593(8)
_cell_length_c                   17.0949(3)
_cell_measurement_reflns_used    192370
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      72.02
_cell_measurement_theta_min      6.59
_cell_volume                     18185.0(5)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            201963
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         6.59
_exptl_absorpt_coefficient_mu    11.394
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.354
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             9518
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         5.516
_refine_diff_density_min         -1.849
_refine_diff_density_rms         0.198
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.474(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     4741
_refine_ls_number_reflns         58192
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0955P)^2^+10.3326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                54590
_reflns_number_total             58192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5b00861_si_004.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      Pn
_cod_original_formula_sum        'C336 H380.60 N48 O130.30 Pb12'
_cod_database_code               4516388