Hydrogen and Copper Ion Induced Molecular Reorganizations in Two New Scorpiand-Like Ligands Appended with Pyridine Rings
Salvador Blasco; Begoña Verdejo; M. Paz Clares; Carmen E. Castillo; Andrés G. Algarra; Julio Latorre; M. Angeles Máñez; Manuel G. Basallote; Conxa Soriano; Enrique García-España; Inorganic Chemistry 49 (2010) 7016–7027; doi:10.1021/ic100609h

data_4316123
_publ_section_title
;
 Hydrogen and Copper Ion Induced Molecular Reorganizations in Two New
 Scorpiand-Like Ligands Appended with Pyridine Rings
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7016
_journal_page_last               7027
_journal_paper_doi               10.1021/ic100609h
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C19 H28 Cu1 N6, 2(Cl1 O4)'
_chemical_formula_sum            'C19 H28 Cl2 Cu N6 O8'
_chemical_formula_weight         602.91
_chemical_name_common            Cu(pytren-2py)
_chemical_name_systematic
; 
 ? 
;
_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                   15.6650(9)
_cell_length_b                   18.4090(12)
_cell_length_c                   8.8550(5)
_cell_measurement_reflns_used    4123
_cell_measurement_temperature    288(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      0.998
_cell_volume                     2553.6(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      288(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1043
_diffrn_reflns_av_sigmaI/netI    0.1234
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            9731
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.30
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         3526
_refine_ls_number_restraints     209
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1947
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1451P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2035
_refine_ls_wR_factor_ref         0.2669
_reflns_number_gt                1581
_reflns_number_total             3526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100609h_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               4316123