Azido{4,4'-dibromo-2,2'-[ethane-1,2-diylbis(nitrilomethanylylidene)]diphenolato-κ^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>'}manganese(III)
Liu, Yingxia; Acta Crystallographica Section E 67 (2011) m322–; doi:10.1107/S1600536811004594

data_2229476
_publ_section_title
;
 Azido{4,4'-dibromo-2,2'-[ethane-1,2-diylbis(nitrilomethanylylidene)]diphenolato-\k^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>'}manganese(III)
;
_journal_coeditor_code           PK2299
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m322
_journal_paper_doi               10.1107/S1600536811004594
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Mn (C16 H12 Br2 N2 O2) (N3)]'
_chemical_formula_moiety         'C16 H12 Br2 Mn N5 O2'
_chemical_formula_sum            'C16 H12 Br2 Mn N5 O2'
_chemical_formula_weight         521.06
_chemical_name_systematic
;
Azido{4,4'-dibromo-2,2'-[ethane-1,2-
diylbis(nitrilomethanylylidene)]diphenolato-
\k^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>'}manganese(III)
;
_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                 107.47(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7068(17)
_cell_length_b                   15.269(3)
_cell_length_c                   13.684(3)
_cell_measurement_reflns_used    19417
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     1735.3(7)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) and maXus (Mackay <i>et al.</i>, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_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  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7747
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.388
_exptl_absorpt_correction_T_max  0.583
_exptl_absorpt_correction_T_min  0.352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.994
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.901
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0376P)^2^+0.8161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0739
_reflns_number_gt                3093
_reflns_number_total             3961
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2299.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2017-04-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1735.4(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_moiety     'C32 H24 Br4 Mn2 N10 O4'
_cod_original_formula_sum        'C32 H24 Br4 Mn2 N10 O4'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1042.13
_cod_database_code               2229476
_cod_database_fobs_code          2229476