Self-assembly of Ligands Designed for the Building of a New Type of [2 x 2] Metallic Grid. Anion Encapsulation and Diffusion NMR Spectroscopy
Blanca R. Manzano; Félix A. Jalón; Isabel M. Ortiz; M. Laura Soriano; Felipe Gómez de la Torre; José Elguero; Miguel A. Maestro; Kurt Mereiter; Tim D. W. Claridge; Inorganic Chemistry 47 (2008) 413–428; doi:10.1021/ic701117a

data_4304002
_publ_contact_author_address
;
 Blanca R. Manzano
 Departamento de Quimica Inorganica, Organica y Bioquimica,
 Facultad de Quimicas, Universidad de Castilla-La Mancha,
 Avda Camilo Jose Cela 10, E-13071 Ciudad Real, Spain
;
_publ_contact_author_email       Blanca.Manzano@uclm.es
_publ_contact_author_fax         +34-926/295318
_publ_contact_author_name        'Blanca R. Manzano'
_publ_contact_author_phone       +34-926/295300
_publ_section_title
;
Self-assembly of Ligands Designed for the Building of a New Type of [2 x
2] Metallic Grid. Anion Encapsulation and Diffusion NMR Spectroscopy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              413
_journal_page_last               428
_journal_paper_doi               10.1021/ic701117a
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C56 H64 Cu4 N24, 4(C7 H7 O3 S)'
_chemical_formula_sum            'C84 H92 Cu4 N24 O12 S4'
_chemical_formula_weight         2012.22
_chemical_name_common            'complex 18 (R-173 - 1026fj)'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.7310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4233(6)
_cell_length_b                   33.8902(15)
_cell_length_c                   22.0612(9)
_cell_measurement_reflns_used    8713
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.77
_cell_measurement_theta_min      2.37
_cell_volume                     9891.6(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            119571
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS V2.10'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bipyramid
_exptl_crystal_F_000             4160
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.291
_refine_diff_density_min         -1.255
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         21477
_refine_ls_number_restraints     396
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0557
_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^)+(0.1014P)^2^+5.9983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1670
_reflns_number_gt                16615
_reflns_number_total             21477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701117a-file004_1.cif
_cod_data_source_block           complex18
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4304002