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_4336125
_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         '4(C28 H55 Cu2 N12), 12(Cl O4), 15(H2 O)'
_chemical_formula_sum            'C112 H250 Cl12 Cu8 N48 O63'
_chemical_formula_weight         4211.32
_chemical_name_common            'compound 1'
_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
_audit_update_record
;
2013-06-24 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.9950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   13.4590(2)
_cell_length_b                   17.8670(4)
_cell_length_c                   18.5920(4)
_cell_measurement_reflns_used    14766
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      0.998
_cell_volume                     4468.14(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_molecular_graphics    Mercury
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Sir92(Altomare,Giacovazzo,1993)
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27627
_diffrn_reflns_theta_full        27.28
_diffrn_reflns_theta_max         27.28
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_T_max  0.4445
_exptl_absorpt_correction_T_min  0.4350
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             2198
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.2
_exptl_crystal_size_rad          0.4000
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         9884
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0778P)^2^+3.9232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1770
_reflns_number_gt                5938
_reflns_number_total             9884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400645t_si_002_2.cif
_cod_data_source_block           Compound1
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4336125
_exptl_absorpt_correction_t_ave  0.4400