Structure refinement of a twinned pseudo-symmetric crystal of [Mn(C~10~H~24~N~4~)(NCO)~2~]^+^·ClO_4^-
A. David Rae; Susanne Mossin; Henning O. Sørensen; Acta Crystallographica Section B 61 (2005) 407–417; doi:10.1107/S0108768105015211

data_2100160
_publ_section_title
;
 Structure refinement of a twinned pseudo-symmetric crystal of
 [Mn(C~10~H~24~N~4~)(NCO)~2~]^+^&#x00B7;ClO_4^-
;
_journal_coeditor_code           CK5009
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              407
_journal_page_last               417
_journal_paper_doi               10.1107/S0108768105015211
_journal_volume                  61
_journal_year                    2005
_chemical_formula_moiety         'C12 H24 Mn N6 O2, Cl O4'
_chemical_formula_sum            'C12 H24 Cl Mn N6 O6'
_chemical_formula_weight         438.76
_chemical_name_systematic
;
trans-dicyanato-(1,4,8,11-tetraazacyclotetradecane)mangan(III)perchlorate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1 (1/2*x+1/2*y,1/2*x-1/2*y,-z)'
_symmetry_space_group_name_H-M   'C -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 and manual editing'
_cell_angle_alpha                90.180(2)
_cell_angle_beta                 111.561(2)
_cell_angle_gamma                90.083(2)
_cell_formula_units_Z            16
_cell_length_a                   30.5936(10)
_cell_length_b                   18.8967(3)
_cell_length_c                   12.8288(5)
_cell_measurement_reflns_used    976
_cell_measurement_temperature    122.0(10)
_cell_measurement_theta_max      33.27
_cell_measurement_theta_min      4.01
_cell_volume                     6897.5(4)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
;
EvalCCD (Duisenberg, 1998) and DREAD (Blessing, 1987)
;
_computing_molecular_graphics    'Platon (Spek, 1990)'
_computing_publication_material  'RAELS2000 and manual editing'
_computing_structure_refinement  'RAELS2000 (Rae, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      122.0(10)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans with \k offsets'
_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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            152267
_diffrn_reflns_theta_full        34.65
_diffrn_reflns_theta_max         34.65
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.966
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.00
_refine_diff_density_min         -1.01
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.31
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         27998
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.086
_refine_ls_R_factor_gt           0.041
_refine_ls_shift/su_max          0.1
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'calc w=1/[\s^2^(Fo)+(0.02Fo)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.054
_refine_ls_wR_factor_ref         0.061
_reflns_number_gt                17584
_reflns_number_total             27998
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            ck5009.cif
_cod_data_source_block           large
_cod_original_cell_volume        6897.9(4)
_cod_original_sg_symbol_H-M      C-1
_cod_database_code               2100160