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_4341608
_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 H37 B Br2 Fe N6 O3, C2 H4 Cl2'
_chemical_formula_sum            'C57 H41 B Br2 Cl2 Fe N6 O3'
_chemical_formula_weight         1155.34
_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     iterative
_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                 92.1962(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.78560(14)
_cell_length_b                   37.3826(4)
_cell_length_c                   13.41213(14)
_cell_measurement_reflns_used    20656
_cell_measurement_temperature    100.05(10)
_cell_measurement_theta_max      73.7160
_cell_measurement_theta_min      3.4650
_cell_volume                     4902.70(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      100.05(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0047284000
_diffrn_orient_matrix_UB_12      0.0232262000
_diffrn_orient_matrix_UB_13      0.0949858000
_diffrn_orient_matrix_UB_21      0.0025201000
_diffrn_orient_matrix_UB_22      0.0340230000
_diffrn_orient_matrix_UB_23      -0.0647405000
_diffrn_orient_matrix_UB_31      -0.1573998000
_diffrn_orient_matrix_UB_32      0.0012416000
_diffrn_orient_matrix_UB_33      -0.0025543000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            46439
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.66
_diffrn_reflns_theta_min         3.50
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.811
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.217
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.7594
_exptl_crystal_size_mid          0.0753
_exptl_crystal_size_min          0.0259
_refine_diff_density_max         1.577
_refine_diff_density_min         -1.830
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         9717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0508P)^2^+24.7199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1624
_reflns_number_gt                8956
_reflns_number_total             9717
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502564r_si_002.cif
_cod_data_source_block           complex2
_cod_original_cell_volume        4902.71(10)
_cod_database_code               4341608
_chemical_oxdiff_formula         'Fe C55 H37 N6 O3 Br2 B C2 H4 Cl2'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.024) H5(0.025) H8(0.025) H11(0.029) H12(0.033) H13(0.035)
 H14(0.032) H15(0.026) H17(0.031) H18(0.04) H19(0.043) H20(0.043) H21(0.034)
 H23(0.028) H24(0.034) H25(0.035) H26(0.035) H27(0.027) H29(0.036) H30(0.047)
 H31(0.044) H32(0.042) H33(0.037) H35(0.026) H36(0.029) H37(0.034) H38(0.032)
 H39(0.027) H41(0.027) H42(0.032) H43(0.034) H44(0.032) H45(0.027) H51(0.072)
 H52(0.084) H53(0.057) H1(0.021) H1SA(0.091) H1SB(0.091) H2SA(0.082) H2SB(0.082)
 Fixed X: H2(-0.2697) H5(-0.1731) H8(0.4579) H11(-0.1721) H12(-0.2293) H13(-
 0.309) H14(-0.3397) H15(-0.2825) H17(-0.3235) H18(-0.3211) H19(-0.1148)
 H20(0.0896) H21(0.0891) H23(-0.3522) H24(-0.4356) H25(-0.2874) H26(-0.0573)
 H27(0.0271) H29(-0.0565) H30(-0.0325) H31(0.0053) H32(0.0159) H33(-0.0222)
 H35(0.4011) H36(0.3663) H37(0.1615) H38(-0.0081) H39(0.0298) H41(0.6029)
 H42(0.7584) H43(0.7023) H44(0.4923) H45(0.3363) H51(0.3582) H52(0.1788)
 H53(0.0568) H1(-0.0341) H1SA(0.3045) H1SB(0.4586) H2SA(0.2332) H2SB(0.3878)
 Fixed Y: H2(0.3193) H5(0.3235) H8(0.2633) H11(0.2484) H12(0.1878) H13(0.1585)
 H14(0.1902) H15(0.2509) H17(0.3876) H18(0.4423) H19(0.4709) H20(0.4447)
 H21(0.3908) H23(0.2717) H24(0.2133) H25(0.1647) H26(0.1743) H27(0.2324)
 H29(0.3741) H30(0.4309) H31(0.4802) H32(0.4726) H33(0.416) H35(0.2092)
 H36(0.1475) H37(0.1224) H38(0.1591) H39(0.2204) H41(0.3173) H42(0.3645)
 H43(0.4169) H44(0.4216) H45(0.3745) H51(0.5293) H52(0.5243) H53(0.4715)
 H1(0.2617) H1SA(0.43) H1SB(0.4414) H2SA(0.4532) H2SB(0.4639)
 Fixed Z: H2(0.2845) H5(0.8612) H8(0.5133) H11(0.2579) H12(0.2488) H13(0.389)
 H14(0.5361) H15(0.5465) H17(0.2891) H18(0.2039) H19(0.1765) H20(0.2313)
 H21(0.32) H23(0.7735) H24(0.7913) H25(0.7747) H26(0.7442) H27(0.7302)
 H29(0.9439) H30(1.0134) H31(0.9116) H32(0.7388) H33(0.668) H35(0.6053)
 H36(0.614) H37(0.5534) H38(0.4807) H39(0.4645) H41(0.5998) H42(0.5974)
 H43(0.5106) H44(0.4223) H45(0.4246) H51(0.5521) H52(0.4319) H53(0.4152)
 H1(0.5647) H1SA(0.9498) H1SB(0.98) H2SA(1.0971) H2SB(1.1273)
;
_olex2_submission_special_instructions 'No special instructions were received'