Synthesis and characterization of divalent manganese, iron, and cobalt complexes in tripodal phenolate/n-heterocyclic carbene ligand environments.
Käß, Martina; Hohenberger, Johannes; Adelhardt, Mario; Zolnhofer, Eva M.; Mossin, Susanne; Heinemann, Frank W.; Sutter, Jörg; Meyer, Karsten; Inorganic chemistry 53 (2014) 2460–2470; doi:10.1021/ic4024053

data_4337735
_publ_section_title
;
 Synthesis and characterization of divalent manganese, iron, and cobalt
 complexes in tripodal phenolate/n-heterocyclic carbene ligand
 environments.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2460
_journal_page_last               2470
_journal_paper_doi               10.1021/ic4024053
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
'C50 H61 Mn N3 O2, 1.5(C4 H10 O2), 0.5(C4 H8 O)'
_chemical_formula_sum            'C58 H80 Mn N3 O5.5'
_chemical_formula_weight         962.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 106.599(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.366(2)
_cell_length_b                   21.614(3)
_cell_length_c                   27.656(3)
_cell_measurement_reflns_used    9819
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.41
_cell_volume                     10521(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            142581
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.304
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.765
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1232
_refine_ls_number_reflns         18540
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.784
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0830P)^2^+3.3157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2419
_refine_ls_wR_factor_ref         0.2621
_reflns_number_gt                12878
_reflns_number_total             18540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4024053_si_002.cif
_cod_data_source_block           jh1202
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C58 H80 Mn N3 O5.50'
_cod_database_code               4337735