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_4304006
_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(F6 P)'
_chemical_formula_sum            'C56 H64 Cu4 F24 N24 P4'
_chemical_formula_weight         1907.35
_chemical_name_common            'complex 16 (RX-14 vv)'
_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                   15.8728(16)
_cell_length_b                   48.079(5)
_cell_length_c                   12.0564(12)
_cell_measurement_temperature    173(2)
_cell_volume                     9200.8(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1454
_diffrn_reflns_av_sigmaI/netI    0.1753
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            49932
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    1.076
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Siemens SADABS program, multi-scan method,
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.076(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1025
_refine_ls_number_reflns         15409
_refine_ls_number_restraints     456
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.1435
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1599
_reflns_number_gt                7785
_reflns_number_total             15409
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701117a-file004_5.cif
_cod_data_source_block           complex16
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_original_cell_volume        9200.7(16)
_cod_original_sg_symbol_Hall     'P 2c -2n '
_cod_database_code               4304006