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_4337739
_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_absolute_configuration ad
_chemical_formula_moiety
'C54 H66 Fe N O3, C36 H30 N P2, C4 H10 O2, C6 H6'
_chemical_formula_sum            'C100 H112 Fe N2 O5 P2'
_chemical_formula_weight         1539.71
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0427(8)
_cell_length_b                   26.2778(19)
_cell_length_c                   28.351(2)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.92
_cell_measurement_theta_min      2.46
_cell_volume                     8226.8(10)
_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      100(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  0.0618
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            118988
_diffrn_reflns_theta_full        27.15
_diffrn_reflns_theta_max         27.15
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2008'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack H D (1983), Acta Cryst. A39, 876-881
 8250 Friedel pairs used in the refinement of Flack parameter
;
_refine_ls_abs_structure_Flack   0.014(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1080
_refine_ls_number_reflns         18199
_refine_ls_number_restraints     289
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0654P)^2^+5.1861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                15953
_reflns_number_total             18199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4024053_si_002.cif
_cod_data_source_block           ma1201a
_cod_original_cell_volume        8226.7(10)
_cod_original_sg_symbol_Hall     P2ac2ab
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4337739