A novel bridged asymmetric binuclear manganese(II) complex with DTPB [DTPB is 1,1,4,7,7-pentakis(1<i>H</i>-benzimidazol-2-ylmethyl)-1,4,7-triazaheptane]
Yan, Xu-Xiu; Lu, Li-Ping; Zhu, Miao-Li; Acta Crystallographica Section C 60 (2004) m221–m223; doi:10.1107/S0108270104007668

data_2013910
_publ_section_title
;
 A novel bridged asymmetric binuclear manganese(II) complex with DTPB
 [DTPB is
 1,1,4,7,7-pentakis(1<i>H</i>-benzimidazol-2-ylmethyl)-1,4,7-triazaheptane]
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m221
_journal_page_last               m223
_journal_paper_doi               10.1107/S0108270104007668
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Mn2 Cl4 (C44 H43 N15)] , 5C H4  O, 4H2 O'
_chemical_formula_moiety         'C44 H43 Cl4 Mn2 N13 , 5C H4 O , 4H2 O'
_chemical_formula_sum            'C49 H71 Cl4 Mn2 N13 O9'
_chemical_formula_weight         1237.87
_chemical_name_systematic
;
tetrachloro[\m-1,1,4,7,7-pentakis(1H-benzimidazol-2-ylmethyl)-1,4,7-
triazaheptane]dimanganese(II) methanol pentasolvate tetrahydrate
;
_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           SHELXL97
_cell_angle_alpha                72.882(3)
_cell_angle_beta                 67.976(2)
_cell_angle_gamma                75.191(3)
_cell_formula_units_Z            2
_cell_length_a                   14.254(3)
_cell_length_b                   15.173(3)
_cell_length_c                   15.852(3)
_cell_measurement_reflns_used    3090
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.12
_cell_measurement_theta_min      2.22
_cell_volume                     2996.3(10)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1999)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2000)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2000)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 27.12
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12285
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.42
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.227
_refine_diff_density_min         -0.928
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         10238
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1017P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1811
_refine_ls_wR_factor_ref         0.1986
_reflns_number_gt                6528
_reflns_number_total             10238
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            av1176.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2996.5(10)
_cod_database_code               2013910
_cod_database_fobs_code          2013910