Nitridomanganese(V) and -(VI) Complexes Containing Macrocyclic Amine Ligands
Karsten Meyer; Jesper Bendix; Nils Metzler-Nolte; Thomas Weyhermüller; Karl Wieghardt; Journal of the American Chemical Society 120 (1998) 7260–7270; doi:10.1021/ja980686j

data_4116782
_publ_section_title
;
 Nitridomanganese(V) and -(VI) Complexes Containing Macrocyclic Amine
 Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7260
_journal_page_last               7270
_journal_paper_doi               10.1021/ja980686j
_journal_volume                  120
_journal_year                    1998
_chemical_formula_structural     '[C20 H48 Mn2 N13]3+, 3 (ClO4)-, 3 H2O'
_chemical_formula_sum            'C20 H54 Cl3 Mn2 N13 O15'
_chemical_formula_weight         932.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.752(3)
_cell_length_b                   25.009(5)
_cell_length_c                   18.764(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_volume                     7861(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART CCD Detector'
_diffrn_measurement_method       '\w-scan, 0.3 deg./frame'
_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  0.0745
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            45187
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.924
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       'Transparent hexagons'
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.63
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.192
_refine_ls_goodness_of_fit_obs   1.237
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         5121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_restrained_S_obs      1.237
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_obs          0.0941
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+73.5425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2257
_refine_ls_wR_factor_obs         0.2198
_reflns_number_observed          4684
_reflns_number_total             5272
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja980686j_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+73.5425P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+73.5425P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7861.2(25)
_cod_database_code               4116782