High spin d5 complexes of tris(6-hydroxymethyl-2-pyridylmethyl)amine (H3L): hepta-coordinated [Mn(H3L)]Cl2 and linear trinuclear [Fe3L2](ClO4)3
Guisado-Barrios, Gregorio; Li, Yang; Slawin, Alexandra M. Z.; Richens, David T.; Gass, Ian A.; Murray, Paul R.; Yellowlees, Lesley J.; Brechin, Euan K.; Dalton Transactions  (2008) 551–558; doi:10.1039/b712188a

data_7003107
_publ_section_title
;
 High spin d5 complexes of tris(6-hydroxymethyl-2-pyridylmethyl)amine
 (H3L): hepta-coordinated [Mn(H3L)]Cl2 and linear trinuclear
 [Fe3L2](ClO4)3
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              551
_journal_page_last               558
_journal_paper_doi               10.1039/b712188a
_journal_year                    2008
_chemical_formula_sum            'C21 H30 Cl2 Mn N4 O6'
_chemical_formula_weight         560.33
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   13.0657(18)
_cell_length_b                   13.0657(18)
_cell_length_c                   54.299(11)
_cell_measurement_reflns_used    7046
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      1.89
_cell_volume                     8028(2)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            13439
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3492
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.561
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1566
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0781
_refine_ls_shift/su_max          0.004
_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^+97.4248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.2079
_reflns_number_gt                1266
_reflns_number_total             1566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b712188a.txt
_cod_data_source_block           Mn
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
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 
;
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               7003107