Intermolecular Binding Modes in a Novel [1 + 1] Condensation 1H-Pyrazole Azamacrocycle: A Solution and Solid State Study with Evidence for CO2 Fixation
Raquel Belda; Javier Pitarch-Jarque; Conxa Soriano; José M. Llinares; Salvador Blasco; Jesús Ferrando-Soria; Enrique García-España; Inorganic Chemistry 52 (2013) 10795–10803; doi:10.1021/ic400645t

data_4336127
_publ_contact_author_email       enrique.garcia-es@uv.es
_publ_contact_author_name        'Enrique Garc\'ia-Espa\~na'
_publ_contact_author_phone       '+34 963 544879'
_publ_section_title
;
 Intermolecular Binding Modes in a Novel [1 + 1] Condensation 1H-Pyrazole
 Azamacrocycle: A Solution and Solid State Study with Evidence for CO2
 Fixation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10795
_journal_page_last               10803
_journal_paper_doi               10.1021/ic400645t
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
'C56H109Cu4N24, 0.3(Cl2O8), 2.4(ClO4), 2(Br), 4.2(H2O)'
_chemical_formula_sum            'C56 H117.4 Br2 Cl3 Cu4 N24 O16.2'
_chemical_formula_weight         1906.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.329(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.2278(6)
_cell_length_b                   17.3890(10)
_cell_length_c                   19.1401(8)
_cell_measurement_reflns_used    7921
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      0.407
_cell_volume                     3943.1(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    Mercury
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0030856
_diffrn_orient_matrix_UB_12      0.0003056
_diffrn_orient_matrix_UB_13      0.0526986
_diffrn_orient_matrix_UB_21      -0.0843479
_diffrn_orient_matrix_UB_22      -0.0004361
_diffrn_orient_matrix_UB_23      -0.0114247
_diffrn_orient_matrix_UB_31      0.0006560
_diffrn_orient_matrix_UB_32      -0.0575052
_diffrn_orient_matrix_UB_33      0.0003667
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_sigmaI/netI    0.1692
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15183
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.08
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.255
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       prism
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         9607
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.2305
_refine_ls_R_factor_gt           0.0861
_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^)+(0.0970P)^2^+8.3764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.2479
_reflns_number_gt                3851
_reflns_number_total             9607
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400645t_si_002_4.cif
_cod_data_source_block           compound2
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_formula_sum        'C56 H117.40 Br2 Cl3 Cu4 N24 O16.20'
_cod_database_code               4336127