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_4337736
_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 Fe N3 O2, 1.84(C4 H8 O), 0.46(C4 H10 O)'
_chemical_formula_sum            'C59.2 H80.31 Fe N3 O4.3'
_chemical_formula_weight         958.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 109.178(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.968(2)
_cell_length_b                   21.6574(18)
_cell_length_c                   18.0292(14)
_cell_measurement_reflns_used    9587
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.81
_cell_measurement_theta_min      2.37
_cell_volume                     10683.3(14)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0949
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            79425
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4135
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.602
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         10521
_refine_ls_number_restraints     209
_refine_ls_restrained_S_all      1.620
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0694
_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^)+(0.0750P)^2^+2.7340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1955
_refine_ls_wR_factor_ref         0.2101
_reflns_number_gt                7177
_reflns_number_total             10521
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4024053_si_002.cif
_cod_data_source_block           jh1206
_cod_original_cell_volume        10683.3(15)
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C59.20 H80.31 Fe N3 O4.30'
_cod_database_code               4337736