Synthesis and characterization of manganese(II) and iron(III) d5 tripodal imidazole complexes. Effect of oxidation state, protonation state and ligand conformation on coordination number and spin state.
Brewer, Cynthia; Brewer, Greg; Butcher, Ray J.; Carpenter, Everett E.; Cuenca, Luciann; Noll, Bruce C.; Scheidt, W. Robert; Viragh, Carol; Zavalij, Peter Y.; Zielaski, Daniel; Dalton transactions (Cambridge, England : 2003)  (2006) 1009–1019; doi:10.1039/b513282g

data_7006715
_publ_section_title
;
 Synthesis and characterization of manganese(II) and iron(III) d5
 tripodal imidazole complexes. Effect of oxidation state, protonation
 state and ligand conformation on coordination number and spin state.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1009
_journal_page_last               1019
_journal_paper_doi               10.1039/b513282g
_journal_year                    2006
_chemical_formula_moiety         'C24 H36 Mn N10, 2(Cl O4)'
_chemical_formula_sum            'C24 H36 Cl2 Mn N10 O8'
_chemical_formula_weight         718.47
_chemical_name_common            'Mn-complex perchlorate'
_chemical_name_systematic
;
Mn-complex perchlorate
;
_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-97 & ZCIF'
_cell_angle_alpha                78.863(1)
_cell_angle_beta                 70.789(1)
_cell_angle_gamma                67.400(1)
_cell_formula_units_Z            2
_cell_length_a                   11.8154(5)
_cell_length_b                   12.2056(6)
_cell_length_c                   12.3982(6)
_cell_measurement_reflns_used    4886
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      29.1
_cell_measurement_theta_min      2.2
_cell_volume                     1554.20(13)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Platon (Spek, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      NFRAMES=645,606,606,50
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '/w scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0353365
_diffrn_orient_matrix_UB_12      -0.0329681
_diffrn_orient_matrix_UB_13      0.0788239
_diffrn_orient_matrix_UB_21      -0.0166345
_diffrn_orient_matrix_UB_22      0.0759628
_diffrn_orient_matrix_UB_23      0.0314922
_diffrn_orient_matrix_UB_31      -0.0871852
_diffrn_orient_matrix_UB_32      0.0326304
_diffrn_orient_matrix_UB_33      -0.0115499
_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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14610
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.61
_diffrn_source_current           35
_diffrn_source_voltage           50
_diffrn_standards_decay_%        -0.05
_exptl_absorpt_coefficient_mu    0.660
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             746
_exptl_crystal_id                'Brewer LLC21'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         7042
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.015P)^2^+1.615P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                6321
_reflns_number_total             7042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b513282g.txt
_cod_data_source_block           1232
_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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7006715
_diffrn_measurement_total_frames-ccd 1907
_diffrn_measurement_frame_width-ccd 0.30
_diffrn_detector_distance-ccd    4.99
_diffrn_measurement_frame_time-ccd 15
_diffrn_measurement_total_time-ccd 11.7
_diffrn_measurement_frame_size-ccd 512