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_4328854
_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            'C11 H10 Br Mn N2 O4'
_chemical_formula_weight         369.06
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.865(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4707(18)
_cell_length_b                   11.548(2)
_cell_length_c                   11.583(2)
_cell_measurement_reflns_used    4034
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      23.252
_cell_measurement_theta_min      2.528
_cell_volume                     1359.8(4)
_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      299(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5926
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    3.919
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.608908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0131(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         1951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0353P)^2^+0.7677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0670
_reflns_number_gt                1765
_reflns_number_total             1951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300196w_si_002_1.cif
_cod_data_source_block           Compound_1a_jt375brm
_cod_original_cell_volume        1359.7(4)
_cod_database_code               4328854