Macrocycle Formation by Proton-Template-Induced Dimerization of Complexes with (Alkoxoimino)pyridine
Celedonio M. Álvarez; Raúl García-Rodríguez; Jose M. Martín-Alvarez; Daniel Miguel; José A. Turiel; Inorganic Chemistry 51 (2012) 3938–3940; doi:10.1021/ic300196w

data_4328855
_publ_contact_author
;
     DANIEL MIGUEL
     IU CINQUIMA/Quimica Inorganica
     Facultad de Ciencias
     Universidad de Valladolid
     C/ Prado de la Magdalena s/n
     47005 Valladolid
     SPAIN
;
_publ_contact_author_email       dmsj@qi.uva.es
_publ_contact_author_fax         +34-983-423013
_publ_contact_author_phone       +34-983-184096
_publ_section_title
;
 Macrocycle Formation by Proton-Template-Induced Dimerization of Complexes
 with (Alkoxoimino)pyridine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3938
_journal_page_last               3940
_journal_paper_doi               10.1021/ic300196w
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C23 H21 Cl3 Mn2 N4 O12'
_chemical_formula_weight         761.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.731(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.618(6)
_cell_length_b                   11.135(4)
_cell_length_c                   16.783(6)
_cell_measurement_reflns_used    1086
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.953
_cell_measurement_theta_min      2.764
_cell_volume                     3099.0(19)
_computing_cell_refinement       'Bruker SMART'
_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
;
 M. C. Burla, M. Camalli, B. Carrozzini, G. L. Cascarano, C. Giacovazzo, 
G. Polidori and R. Spagna. J. Appl. Cryst. (2003). 36, 1103.'
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0874
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13727
_diffrn_reflns_theta_full        23.55
_diffrn_reflns_theta_max         23.55
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.863217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         4533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0742P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                2465
_reflns_number_total             4533
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300196w_si_002_2.cif
_cod_data_source_block           Compound_4a_jt376a
_cod_original_cell_volume        3098.9(18)
_cod_database_code               4328855