Synthesis and Spectroscopic Characterization of High-Spin Mononuclear Iron(II) p-Semiquinonate Complexes.
Baum, Amanda E.; Park, Heaweon; Lindeman, Sergey V.; Fiedler, Adam T.; Inorganic chemistry  (2014) 141113104938005–; doi:10.1021/ic502564r

data_4341607
_publ_section_title
;
 Synthesis and Spectroscopic Characterization of High-Spin Mononuclear
 Iron(II) p-Semiquinonate Complexes.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141113104938005
_journal_paper_doi               10.1021/ic502564r
_journal_year                    2014
_chemical_formula_moiety         'C55 H39 B Fe N6 O3'
_chemical_formula_sum            'C55 H39 B Fe N6 O3'
_chemical_formula_weight         898.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.703(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4080(3)
_cell_length_b                   30.9033(9)
_cell_length_c                   13.4858(4)
_cell_measurement_reflns_used    11459
_cell_measurement_temperature    101.2
_cell_measurement_theta_max      29.4864
_cell_measurement_theta_min      3.5455
_cell_volume                     4335.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      101.2
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details
;
  1 omega   -3.00   76.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697   37.0000   30.0000 79

  2 omega  -59.00   36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697  -37.0000 -150.0000 95

  3 omega   38.00   64.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.8259   37.0000  -90.0000 26

  4 omega  -67.00   11.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697  -77.0000   60.0000 78
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0672127000
_diffrn_orient_matrix_UB_12      0.0031221000
_diffrn_orient_matrix_UB_13      -0.0041520000
_diffrn_orient_matrix_UB_21      -0.0117222000
_diffrn_orient_matrix_UB_22      0.0198813000
_diffrn_orient_matrix_UB_23      -0.0249015000
_diffrn_orient_matrix_UB_31      0.0020768000
_diffrn_orient_matrix_UB_32      0.0110114000
_diffrn_orient_matrix_UB_33      0.0461300000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32339
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.55
_diffrn_reflns_theta_min         3.59
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         10656
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+3.6924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                8935
_reflns_number_total             10656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502564r_si_002.cif
_cod_data_source_block           complex1
_cod_database_code               4341607
_chemical_oxdiff_formula         'Fe C55 H39 N6 O3 B'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H48(0.052) H47(0.048) H52(0.071) H51(0.077) H50(0.053) H2(0.024)
 H5(0.029) H8(0.024) H11(0.027) H12(0.035) H13(0.04) H14(0.039) H15(0.031)
 H17(0.031) H18(0.041) H19(0.043) H20(0.038) H21(0.03) H23(0.032) H24(0.039)
 H25(0.04) H26(0.036) H27(0.029) H35(0.031) H36(0.041) H37(0.048) H38(0.042)
 H39(0.03) H41(0.034) H42(0.042) H43(0.04) H44(0.036) H45(0.029) H1(0.02)
 H29(0.039) H30(0.047) H31(0.038) H32(0.045) H33(0.042) H29A(0.058) H30A(0.065)
 H31A(0.037) H32A(0.044) H33A(0.039)
 Fixed X: H48(-0.1193) H47(-0.0521) H52(0.2028) H51(0.1346) H50(0.0399)
 H2(0.4788) H5(0.5675) H8(-0.1031) H11(0.6445) H12(0.7055) H13(0.5525)
 H14(0.3381) H15(0.2759) H17(0.3705) H18(0.3491) H19(0.3404) H20(0.3572)
 H21(0.3799) H23(0.5023) H24(0.5748) H25(0.65) H26(0.6611) H27(0.5913) H35(-
 0.0038) H36(0.0538) H37(0.2319) H38(0.3487) H39(0.2905) H41(-0.2362) H42(-
 0.408) H43(-0.3962) H44(-0.2135) H45(-0.0443) H1(0.3613) H29(0.6083)
 H30(0.5989) H31(0.4039) H32(0.2211) H33(0.2278) H29A(0.5157) H30A(0.4862)
 H31A(0.361) H32A(0.2553) H33A(0.2894)
 Fixed Y: H48(0.5096) H47(0.5766) H52(0.498) H51(0.4304) H50(0.4191)
 H2(0.6693) H5(0.6718) H8(0.7535) H11(0.7384) H12(0.8107) H13(0.8653)
 H14(0.8485) H15(0.7764) H17(0.6006) H18(0.5286) H19(0.4736) H20(0.4902)
 H21(0.5621) H23(0.7583) H24(0.8296) H25(0.8641) H26(0.8263) H27(0.7545)
 H35(0.8203) H36(0.8931) H37(0.9146) H38(0.8636) H39(0.7908) H41(0.7008)
 H42(0.6532) H43(0.5835) H44(0.5621) H45(0.6107) H1(0.7456) H29(0.5793)
 H30(0.5161) H31(0.4925) H32(0.5338) H33(0.5962) H29A(0.5599) H30A(0.4974)
 H31A(0.5007) H32A(0.5642) H33A(0.6267)
 Fixed Z: H48(0.4549) H47(0.4139) H52(0.0115) H51(0.0581) H50(0.2104)
 H2(0.4883) H5(-0.0827) H8(0.1506) H11(0.4075) H12(0.4304) H13(0.4164)
 H14(0.3795) H15(0.3569) H17(0.5528) H18(0.6013) H19(0.4837) H20(0.3153)
 H21(0.2657) H23(-0.1152) H24(-0.1219) H25(0.0225) H26(0.172) H27(0.1793)
 H35(0.2357) H36(0.2302) H37(0.142) H38(0.0547) H39(0.0573) H41(0.2446)
 H42(0.2594) H43(0.1942) H44(0.1109) H45(0.0896) H1(0.1859) H29(-0.0408) H30(-
 0.1336) H31(-0.2034) H32(-0.1846) H33(-0.0874) H29A(0.0214) H30A(-0.076) H31A(-
 0.2212) H32A(-0.2652) H33A(-0.1696)
;
_olex2_submission_special_instructions 'No special instructions were received'