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_4337742
_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         'C98 H148 Co2 N2 Na2 O8, 4(C6 H6)'
_chemical_formula_sum            'C122 H172 Co2 N2 Na2 O8'
_chemical_formula_weight         1958.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 115.288(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.6042(16)
_cell_length_b                   27.0532(17)
_cell_length_c                   15.9969(14)
_cell_measurement_reflns_used    213
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     5714.6(9)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_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      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 \f- and \w-rotations with 1.20 \% and 96 sec per frame
;
_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  0.0781
_diffrn_reflns_av_sigmaI/netI    0.0813
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            110523
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack H D (1983), Acta Cryst. A39, 876-881
 11829 Friedel pairs used in the refinement of Flack parameter
;
_refine_ls_abs_structure_Flack   0.038(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1321
_refine_ls_number_reflns         24207
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                18340
_reflns_number_total             24207
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4024053_si_002.cif
_cod_data_source_block           sm0902a
_cod_original_sg_symbol_Hall     P2yb
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4337742