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_7006714
_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_absolute_configuration ad
_chemical_formula_moiety
'(C21 H28 N10 Fe), 0.525(I3), 0.475(I), 2.625(H2 O)'
_chemical_formula_sum            'C21 H33.25 Fe I2.05 N10 O2.625'
_chemical_formula_weight         783.82
_chemical_name_common
;Fe(3+) . NL3(3-)H(1+) . I3(1-)1-x . I(1-)x . nH2O x=0.475,
n=2.625
;
_chemical_name_systematic
;
Fe(3+) . NL3(3-)H(1+) . I3(1-)1-x . I(1-)x . nH2O
x=0.475, n=2.625
;
_space_group_IT_number           219
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'F -4a 2 3'
_symmetry_space_group_name_H-M   'F -4 3 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            32
_cell_length_a                   29.6863(3)
_cell_length_b                   29.6863(3)
_cell_length_c                   29.6863(3)
_cell_measurement_reflns_used    9240
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.4
_cell_volume                     26161.8(5)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      NFRAMES=606,606,606,50
_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      -0.0034604
_diffrn_orient_matrix_UB_12      -0.0295793
_diffrn_orient_matrix_UB_13      -0.0157210
_diffrn_orient_matrix_UB_21      -0.0334632
_diffrn_orient_matrix_UB_22      0.0021847
_diffrn_orient_matrix_UB_23      0.0032623
_diffrn_orient_matrix_UB_31      -0.0018472
_diffrn_orient_matrix_UB_32      0.0159527
_diffrn_orient_matrix_UB_33      -0.0296138
_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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0113
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            54720
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.74
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.16
_exptl_absorpt_coefficient_mu    2.432
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP (Sheldrick, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             12317
_exptl_crystal_id                'Greg Brawer DZ3'
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   -0.01(5)
_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     132
_refine_ls_number_reflns         2516
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.067P)^2^+243.5P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.882
_reflns_number_gt                1927
_reflns_number_total             2516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b513282g.txt
_cod_data_source_block           1215
_cod_original_sg_symbol_Hall     'F -4c 2 3'
_cod_database_code               7006714
_diffrn_measurement_total_frames-ccd 1868
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_detector_distance-ccd    4.890
_diffrn_measurement_frame_time-ccd 23
_diffrn_measurement_total_time-ccd 15.6
_diffrn_measurement_frame_size-ccd 512