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_4116781
_publ_section_title
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 Nitridomanganese(V) and -(VI) Complexes Containing Macrocyclic Amine
 Ligands
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_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     '[C10 H24 Mn N10]+, ClO4-'
_chemical_formula_sum            'C10 H24 Cl Mn N10 O4'
_chemical_formula_weight         438.78
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                79.45(2)
_cell_angle_beta                 81.07(2)
_cell_angle_gamma                63.50(2)
_cell_formula_units_Z            2
_cell_length_a                   9.462(1)
_cell_length_b                   9.511(1)
_cell_length_c                   11.434(1)
_cell_measurement_reflns_used    3128
_cell_measurement_temperature    100(2)
_cell_volume                     902.1(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(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  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4151
_diffrn_reflns_theta_max         25.89
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.921
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       'transparent octahedral'
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.311
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0109(16)
_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_all   1.168
_refine_ls_goodness_of_fit_obs   1.183
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.262
_refine_ls_restrained_S_obs      1.183
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_obs          0.0434
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.9590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1206
_refine_ls_wR_factor_obs         0.1106
_reflns_number_observed          2891
_reflns_number_total             3021
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja980686j_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.9590P] 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^)+(0.0000P)^2^+3.9590P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        902.1(3)
_cod_database_code               4116781