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_4333333
_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_sum            'C70 H112 Cu4 F12 N14 O21 S4'
_chemical_formula_weight         2096.14
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.036(2)
_cell_angle_beta                 113.422(2)
_cell_angle_gamma                103.114(2)
_cell_formula_units_Z            2
_cell_length_a                   15.2221(6)
_cell_length_b                   17.3423(6)
_cell_length_c                   18.8869(7)
_cell_measurement_temperature    153(2)
_cell_volume                     4422.9(3)
_computing_cell_refinement       'Bruker SAINT program Vers. 5.0'
_computing_data_collection       'Bruker SMART CCD area detector system'
_computing_data_reduction        'Bruker SAINT program Vers. 5.0'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            'Smart 1000 CCD area detector'
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'four-circle diffractometer Bruker P4'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans,
 in omega at 0.3 deg scan width, three runs with 98, 67 and 67 frames, phi=0 deg
 in phi at 0.3 deg scan width, two runs with 1207 frames, omega=-32 deg
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0896
_diffrn_reflns_av_sigmaI/netI    0.1381
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55012
_diffrn_reflns_theta_full        31.54
_diffrn_reflns_theta_max         31.54
_diffrn_reflns_theta_min         1.48
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           220
_diffrn_source_power             45
_diffrn_source_size              '10 mm x 0.5 mm fine focus'
_diffrn_source_type              'MACScience Co. M18X-HF'
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.787688
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2.1 2003 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.087
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.858
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1194
_refine_ls_number_reflns         26983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.858
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0555P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                14053
_reflns_number_total             26983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700692tsup1.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_measurement_specimen_suppport' tag replaced with
'_diffrn_measurement_specimen_support'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4333333