1,4,8,11-Tetraazoniacyclotetradecane diaquatetrachloridomanganese(II) dichloride dihydrate
Pojarová, Michaela; Fejfarová, Karla; El Bali, Brahim; Acta Crystallographica Section E 66 (2010) m1103–; doi:10.1107/S1600536810031958

data_2227204
_publ_section_title
;
 1,4,8,11-Tetraazoniacyclotetradecane diaquatetrachloridomanganese(II)
 dichloride dihydrate
;
_journal_coeditor_code           BT5316
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1103
_journal_paper_doi               10.1107/S1600536810031958
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C10 H28 N4) [Mn Cl4 (H2 O)2] Cl2, 2H2 O'
_chemical_formula_moiety
'C10 H28 N4 4+, Cl4 H4 Mn O2 2-, 2(Cl -), 2(H2 O)'
_chemical_formula_sum            'C10 H36 Cl6 Mn N4 O4'
_chemical_formula_weight         544.1
_chemical_name_systematic
;
1,4,8,11-Tetraazoniacyclotetradecane diaquatetrachloridomanganese(II)
dichloride dihydrate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8492(2)
_cell_length_b                   19.3511(3)
_cell_length_c                   7.87720(10)
_cell_measurement_reflns_used    16479
_cell_measurement_temperature    292
_cell_measurement_theta_max      26.4995
_cell_measurement_theta_min      2.5081
_cell_volume                     2263.50(5)
_computing_cell_refinement       'Crysalis RED (Oxford Diffraction, 2005)'
_computing_data_collection       'Crysalis CCD (Oxford Diffraction, 2005)'
_computing_data_reduction        'Crysalis RED(Oxford Diffraction, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material
'JANA2006 (Pet\<r\'i\<cek <i>et al.</i>, 2006) and publCIF (Westrip, 2010)'
_computing_structure_refinement
'JANA2006 (Pet\<r\'i\<cek <i>et al.</i>, 2006)'
_computing_structure_solution    'SIR2002 (Burla <i>et al.</i>, 2003)'
_diffrn_ambient_temperature      292
_diffrn_detector_area_resol_mean 8.3438
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Oxford Diffraction CCD'
_diffrn_measurement_method       'Rotation method data acquisition using \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0109
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            26200
_diffrn_reflns_reduction_process
;
Integration of the CCD images was done by program Crysalis RED
(Oxford Diffraction, 2005).
;
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    1.314
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2005)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.59606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.3598
_exptl_crystal_size_mid          0.2190
_exptl_crystal_size_min          0.1588
_refine_diff_density_max         0.14
_refine_diff_density_min         -0.10
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2429
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0179
_refine_ls_shift/su_max          0.0096
_refine_ls_shift/su_mean         0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[\s^2^(I)+0.0016I^2^]
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0589
_reflns_number_gt                1999
_reflns_number_total             2429
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            bt5316.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C10 H36 Cl6 Mn1 N4 O4'
_cod_database_code               2227204