Preparation of a semiquinonate-bridged diiron(II) complex and elucidation of its geometric and electronic structures
Amanda E. Baum; Sergey V. Lindeman; Adam T. Fiedler; Chem.Commun. 49 (2013) 6531–; doi:10.1039/c3cc42980f

data_7109496
_publ_section_title
;
 Preparation of a semiquinonate-bridged diiron(II) complex and elucidation
 of its geometric and electronic structures
;
_journal_name_full               Chem.Commun.
_journal_page_first              6531
_journal_paper_doi               10.1039/c3cc42980f
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety
'C98 H76 B2 Fe2 N12 O4, 1.04(F6 P), 0.96(C H2 Cl2)'
_chemical_formula_sum
'C98.96 H77.93 B2 Cl1.93 F6.22 Fe2 N12 O4 P1.04'
_chemical_formula_weight         1851.12
_chemical_name_systematic
;
?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-02
_audit_creation_method
;
Olex2 1.2
(compiled Dec 5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                103.453(3)
_cell_angle_beta                 104.559(3)
_cell_angle_gamma                97.098(3)
_cell_formula_units_Z            1
_cell_length_a                   9.7382(3)
_cell_length_b                   13.2530(4)
_cell_length_c                   18.0619(7)
_cell_measurement_reflns_used    20404
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.7422
_cell_measurement_theta_min      3.4921
_cell_volume                     2152.89(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
1 omega -49.00 33.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.6487 57.0000 -30.0000 82

2 omega -48.00 36.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.6487 37.0000 -180.0000 84

3 omega -40.00 36.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.6487 37.0000 -120.0000 76

4 omega -70.00 33.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.6487 57.0000 90.0000 103

5 omega 46.00 94.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 40.6487 -125.0000 -90.0000 48

6 omega 36.00 90.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 -30.0000 150.0000 54

7 omega 47.00 106.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 -94.0000 -30.0000 59

8 omega 31.00 128.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 -77.0000 90.0000 97

9 omega 33.00 88.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 -30.0000 90.0000 55

10 omega 44.00 103.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 -94.0000 60.0000 59

11 omega 60.00 120.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 -125.0000 -90.0000 60

12 omega 44.00 71.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 -30.0000 -30.0000 27

13 omega 41.00 87.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 -45.0000 -60.0000 46

14 omega 77.00 174.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 30.0000 0.0000 97

15 omega 30.00 89.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 -30.0000 -150.0000 59

16 omega 49.00 90.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 -94.0000 -90.0000 41

17 omega 28.00 113.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 -15.0000 0.0000 85

18 omega -115.00 -11.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.6487 -57.0000 -60.0000 104

19 omega -115.00 -11.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.6487 -57.0000 60.0000 104

20 omega -115.00 -11.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.6487 -57.0000 -180.0000 104

21 omega 1.00 83.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 40.6487 -99.0000 -150.0000 82

22 omega 7.00 119.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 40.6487 77.0000 60.0000 112

23 omega -140.00 -28.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- -61.5000 -77.0000 -60.0000 112

24 omega -140.00 -28.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- -61.5000 -77.0000 30.0000 112

25 omega -140.00 -28.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- -61.5000 -77.0000 -180.0000 112

26 omega 77.00 178.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 61.0000 -150.0000 101

27 omega 73.00 178.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 77.0000 -30.0000 105

28 omega 77.00 178.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 30.0000 150.0000 101

29 omega 73.00 178.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 77.0000 150.0000 105

30 omega 77.00 178.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 61.0000 90.0000 101

31 omega 77.00 178.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 30.0000 -60.0000 101

32 omega 77.00 178.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 30.0000 60.0000 101

33 omega 7.00 119.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 40.6487 77.0000 150.0000 112

34 omega 7.00 119.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 40.6487 77.0000 -120.0000 112

35 omega 23.00 98.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 40.6487 -125.0000 90.0000 75

36 omega 1.00 83.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 40.6487 -99.0000 -60.0000 82

37 omega 7.00 119.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 40.6487 77.0000 -30.0000 112

38 omega 23.00 109.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 -94.0000 60.0000 86

39 omega 77.00 178.00 1.0000 3.9000
omega____ theta____ kappa____ phi______ frames
- 107.0378 61.0000 -120.0000 101
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0678717000
_diffrn_orient_matrix_UB_12      -0.1169585000
_diffrn_orient_matrix_UB_13      -0.0151049000
_diffrn_orient_matrix_UB_21      -0.1487502000
_diffrn_orient_matrix_UB_22      0.0303189000
_diffrn_orient_matrix_UB_23      -0.0035100000
_diffrn_orient_matrix_UB_31      -0.0319311000
_diffrn_orient_matrix_UB_32      -0.0155553000
_diffrn_orient_matrix_UB_33      -0.0903235000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42432
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.91
_diffrn_reflns_theta_min         3.49
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.063
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             954
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.1945
_exptl_crystal_size_min          0.1358
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         8566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0566P)^2^+1.1484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                8283
_reflns_number_total             8566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc42980f.txt
_cod_data_source_block           complex[2]PF6
_cod_original_cell_volume        2152.89(13)
_cod_database_code               7109496
_chemical_oxdiff_formula         'Fe C45 B H34 N6 P F6 O2 C4 H4'
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
Fixed Uiso: H2(0.022) H5(0.026) H8(0.028) H11(0.024) H12(0.028) H13(0.029)
H14(0.028) H15(0.023) H17(0.04) H18(0.063) H19(0.064) H20(0.058) H21(0.039)
H23(0.031) H24(0.038) H25(0.035) H26(0.031) H27(0.026) H29(0.043) H30(0.065)
H31(0.077) H32(0.076) H33(0.048) H35(0.027) H36(0.031) H37(0.032) H38(0.029)
H39(0.024) H41(0.033) H42(0.042) H43(0.05) H44(0.056) H45(0.044) H48(0.021)
H49A(0.037) H49B(0.037) H49C(0.037) H1(0.019) H50A(0.082) H50B(0.082)
Fixed X: H2(-0.0806) H5(0.1542) H8(0.6858) H11(-0.1292) H12(-0.104)
H13(0.1253) H14(0.33) H15(0.3061) H17(-0.2481) H18(-0.3104) H19(-0.1417)
H20(0.0916) H21(0.1553) H23(0.4059) H24(0.5051) H25(0.4091) H26(0.2139)
H27(0.1168) H29(0.1671) H30(0.0497) H31(-0.1577) H32(-0.2456) H33(-0.1251)
H35(0.6371) H36(0.7012) H37(0.6697) H38(0.5757) H39(0.5104) H41(0.6898)
H42(0.7185) H43(0.5571) H44(0.3612) H45(0.3313) H48(-0.1645) H49A(0.2338)
H49B(0.3359) H49C(0.3562) H1(0.2764) H50A(0.4719) H50B(0.3685)
Fixed Y: H2(0.9196) H5(0.3388) H8(0.7976) H11(0.8219) H12(0.8576) H13(0.9087)
H14(0.9336) H15(0.9018) H17(0.8584) H18(0.8866) H19(0.8916) H20(0.8717)
H21(0.8422) H23(0.4392) H24(0.4873) H25(0.606) H26(0.6767) H27(0.6312)
H29(0.239) H30(0.1076) H31(0.1291) H32(0.2849) H33(0.421) H35(0.9654)
H36(1.0599) H37(0.9728) H38(0.7915) H39(0.6969) H41(0.6224) H42(0.5734)
H43(0.6061) H44(0.6809) H45(0.7319) H48(0.6176) H49A(0.3449) H49B(0.4206)
H49C(0.4387) H1(0.7201) H50A(0.945) H50B(0.9041)
Fixed Z: H2(0.3835) H5(0.3963) H8(0.3834) H11(0.5083) H12(0.6446) H13(0.7362)
H14(0.6925) H15(0.5566) H17(0.221) H18(0.0936) H19(0.0232) H20(0.079)
H21(0.204) H23(0.5279) H24(0.6657) H25(0.7468) H26(0.6896) H27(0.5516)
H29(0.2504) H30(0.1332) H31(0.0472) H32(0.0757) H33(0.1923) H35(0.5028)
H36(0.6369) H37(0.732) H38(0.6927) H39(0.5588) H41(0.2525) H42(0.1252)
H43(0.019) H44(0.0377) H45(0.1646) H48(0.0098) H49A(0.1111) H49B(0.1944)
H49C(0.1129) H1(0.485) H50A(0.9482) H50B(0.8585)
;