Pb2+ Complexes of Small-Cavity Azamacrocyclic Ligands. Thermodynamic and Kinetic Studies
Liberato, Andrea; Aguinaco, Almudena; Clares, Maria Paz; Delgado-Pinar, Estefania; Blasco, Salvador; Pitarch-Jarque, Javier; Basallote, Manuel G.; García-España, Enrique; Verdejo, Begoña; Dalton Trans.  (2017) –; doi:10.1039/C7DT00680B

data_7042740
_publ_section_title
;
 Pb2+ Complexes of Small-Cavity Azamacrocyclic Ligands. Thermodynamic and
 Kinetic Studies
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00680B
_journal_year                    2017
_chemical_formula_moiety         'C11 H18 N4 Pb, 2(Cl O4)'
_chemical_formula_sum            'C11 H18 Cl2 N4 O8 Pb'
_chemical_formula_weight         612.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-14
_audit_creation_method
;
Olex2 1.2
(compiled Nov 22 2016 12:06:14 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-01-24 deposited with the CCDC.
2017-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.1503(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8925(3)
_cell_length_b                   15.1543(5)
_cell_length_c                   13.5209(5)
_cell_measurement_reflns_used    4043
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1787.68(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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    'SIR2011 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0476636
_diffrn_orient_matrix_UB_12      0.0023027
_diffrn_orient_matrix_UB_13      0.0732740
_diffrn_orient_matrix_UB_21      -0.1035306
_diffrn_orient_matrix_UB_22      -0.0066205
_diffrn_orient_matrix_UB_23      0.0176872
_diffrn_orient_matrix_UB_31      0.0121190
_diffrn_orient_matrix_UB_32      -0.0656145
_diffrn_orient_matrix_UB_33      0.0007869
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7721
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         3.071
_exptl_absorpt_coefficient_mu    9.785
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.275
_exptl_crystal_description       prism
_exptl_crystal_F_000             1168
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.722
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0460
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1630
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2212
_reflns_number_total             4065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00680b2.cif
_cod_data_source_block           import
_cod_database_code               7042740
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2), N3(H3), N4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C11(H11A,H11B), C8(H8A,H8B), C10(H10A,H10B), C7(H7A,H7B), C9(H9A,
 H9B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3A), C4(H4A)
;
_shelx_res_checksum              10767
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'