Structural and Kinetic Study of Reversible CO2Fixation by Dicopper Macrocyclic Complexes. From Intramolecular Binding to Self-Assembly of Molecular Boxes
Company, Anna; Jee, Joo-Eun; Ribas, Xavi; Lopez-Valbuena, Josep Maria; Gómez, Laura; Corbella, Montserrat; Llobet, Antoni; Mahía, José; Benet-Buchholz, Jordi; Costas, Miquel; van Eldik, Rudi; Inorganic Chemistry 46 (2007) 9098–9110; doi:10.1021/ic700692t

data_4333334
_publ_section_title
;
 Structural and Kinetic Study of Reversible CO2Fixation by Dicopper
 Macrocyclic Complexes. From Intramolecular Binding to Self-Assembly of
 Molecular Boxes
;
_journal_issue                   22
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9098
_journal_page_last               9110
_journal_paper_doi               10.1021/ic700692t
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         C64H92N12Cu4+(CO3)2+(ClO4)4+(H2O)4+(C3H6O)2
_chemical_formula_sum            'C64 H112 Cl4 Cu4 N12 O28'
_chemical_formula_weight         1893.62
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 112.867(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.797(4)
_cell_length_b                   13.879(2)
_cell_length_c                   19.063(3)
_cell_measurement_temperature    173(2)
_cell_volume                     4338.6(14)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens CCD'
_diffrn_measurement_method       '\w 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  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18062
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        0.32
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.733974
_exptl_absorpt_correction_type   Sadabs
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.351
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.048
_refine_ls_goodness_of_fit_obs   1.157
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7729
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.062
_refine_ls_restrained_S_obs      1.175
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_obs          0.0857
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0948P)^2^+33.6420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2337
_refine_ls_wR_factor_obs         0.2143
_reflns_number_observed          5399
_reflns_number_total             7729
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic700692tsup1.cif
_cod_data_source_block           8
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0948P)^2^+33.6420P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0948P)^2^+33.6420P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4338.6(13)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4333334