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_4336126
_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         'C16 H29 Cu N5, 2(Cl O4)'
_chemical_formula_sum            'C16 H29 Cl2 Cu N5 O8'
_chemical_formula_weight         553.88
_chemical_name_common            '[Cu(py333)](ClO4)2'
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0320(5)
_cell_length_b                   8.4710(2)
_cell_length_c                   14.1470(8)
_cell_measurement_reflns_used    14547
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2280.78(15)
_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_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1110
_diffrn_reflns_av_sigmaI/netI    0.1079
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9165
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       bloc
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.231
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4947
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1176P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.2128
_reflns_number_gt                3300
_reflns_number_total             4947
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400645t_si_002_3.cif
_cod_data_source_block           compound3
_cod_database_code               4336126