On the Importance of Unprecedented Lone Pair–Salt Bridge Interactions in Cu(II)–Malonate–2-Amino-5-Chloropyridine–Perchlorate Ternary System
Mitra, Monojit; Manna, Prankrishna; Das, Amrita; Seth, Saikat Kumar; Helliwell, Madeleine; Bauzá, Antonio; Choudhury, Somnath Ray; Frontera, Antonio; Mukhopadhyay, Subrata; The Journal of Physical Chemistry A 117 (2013) 5802–; doi:10.1021/jp4046066

data_1512139
_publ_section_title
;
 On the Importance of Unprecedented Lone Pair--Salt Bridge Interactions in
 Cu(II)--Malonate--2-Amino-5-Chloropyridine--Perchlorate Ternary System
;
_journal_issue                   28
_journal_name_full               'The Journal of Physical Chemistry A'
_journal_page_first              5802
_journal_paper_doi               10.1021/jp4046066
_journal_volume                  117
_journal_year                    2013
_chemical_formula_moiety         'C24 H24 Cu4 O36, 4(Cl O4), 12(C5 H6 Cl N2)'
_chemical_formula_sum            'C84 H96 Cl16 Cu4 N24 O52'
_chemical_formula_weight         3095.21
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                99.442(4)
_cell_angle_beta                 100.995(4)
_cell_angle_gamma                115.031(4)
_cell_formula_units_Z            2
_cell_length_a                   17.687(4)
_cell_length_b                   19.450(5)
_cell_length_c                   20.114(5)
_cell_measurement_reflns_used    885
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.79
_cell_measurement_theta_min      2.40
_cell_volume                     5917(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0809
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34025
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1682
_refine_ls_number_reflns         23472
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0587P)^2^+1.6302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1366
_reflns_number_gt                15667
_reflns_number_total             23472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp4046066_si_002.cif
_cod_data_source_block           pkm209a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        5917(2)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1512139