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_4336124
_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         'C29 H56 Cu3 N12 O4, 2(Cl O4), 8(H2 O)'
_chemical_formula_sum            'C29 H72 Cl2 Cu3 N12 O20'
_chemical_formula_weight         1170.51
_chemical_name_common            Cu2(pz333)2CO3
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-05-27 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 116.231(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.5744(7)
_cell_length_b                   10.3781(3)
_cell_length_c                   23.7191(9)
_cell_measurement_reflns_used    14140
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      32.4165
_cell_measurement_theta_min      3.1515
_cell_volume                     4763.8(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    Mercury
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Sir92
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) x-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            45251
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.49
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    1.525
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       block
_exptl_crystal_F_000             2444
_exptl_crystal_size_max          0.4299
_exptl_crystal_size_mid          0.3063
_exptl_crystal_size_min          0.2513
_refine_diff_density_max         2.131
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         15663
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0649
_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^)+(0.0530P)^2^+27.6996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.1877
_reflns_number_gt                12217
_reflns_number_total             15663
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400645t_si_002_1.cif
_cod_data_source_block           Compound4
_cod_original_sg_symbol_Hall     -P2yn
_cod_database_code               4336124