#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:07:26 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180124 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/22/7102242.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7102242
loop_
_publ_author_name
'Spikes, Geoffrey H'
'Bill, Eckhard'
'Weyhermüller, Thomas'
'Wieghardt, Karl'
_publ_section_title
;
 Unusual mixed valent FeIIIFeII complex (St = 3/2) stabilised by a
 reduced bulky 1,2-diketone.
;
_journal_issue                   42
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4339
_journal_page_last               4341
_journal_paper_doi               10.1039/b713062g
_journal_year                    2007
_chemical_formula_moiety         'C26 H34 O2'
_chemical_formula_sum            'C26 H34 O2'
_chemical_formula_weight         378.53
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   9.6205(3)
_cell_length_b                   13.8569(5)
_cell_length_c                   16.7988(6)
_cell_measurement_temperature    100(2)
_cell_volume                     2239.45(13)
_computing_cell_refinement       'Bruker AXS Collect Software'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        'Bruker AXS Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius Kappa-CCD'
_diffrn_measurement_method
'244 images at 2.0 deg stepwise rotation in omega and phi, 180 sec./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  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23895
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0457P)²+0.8133P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                2031
_reflns_number_total             2561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b713062g.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7102242
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
O1 O 0.42272(9) 0.08424(6) 0.56209(5) 0.0235(2) Uani 1 1 d .
C1 C 0.47143(11) 0.00678(9) 0.54304(7) 0.0171(3) Uani 1 1 d .
C2 C 0.48000(12) -0.07849(8) 0.59832(7) 0.0176(3) Uani 1 1 d .
C3 C 0.38534(12) -0.15429(9) 0.58727(7) 0.0192(3) Uani 1 1 d .
C4 C 0.39006(13) -0.23213(9) 0.63979(8) 0.0238(3) Uani 1 1 d .
H4A H 0.3266 -0.2841 0.6336 0.029 Uiso 1 1 calc R
C5 C 0.48678(14) -0.23411(10) 0.70101(8) 0.0261(3) Uani 1 1 d .
H5A H 0.4889 -0.2874 0.7365 0.031 Uiso 1 1 calc R
C6 C 0.58033(13) -0.15897(9) 0.71080(7) 0.0230(3) Uani 1 1 d .
H6A H 0.6466 -0.1619 0.7526 0.028 Uiso 1 1 calc R
C7 C 0.57880(12) -0.07921(9) 0.66033(7) 0.0185(3) Uani 1 1 d .
C8 C 0.27524(12) -0.14950(9) 0.52206(7) 0.0209(3) Uani 1 1 d .
H8A H 0.2936 -0.0899 0.4902 0.025 Uiso 1 1 calc R
C9 C 0.28209(15) -0.23507(10) 0.46512(8) 0.0308(3) Uani 1 1 d .
H9A H 0.3738 -0.2371 0.4398 0.046 Uiso 1 1 calc R
H9B H 0.2103 -0.2281 0.4242 0.046 Uiso 1 1 calc R
H9C H 0.2666 -0.2950 0.4948 0.046 Uiso 1 1 calc R
C10 C 0.12945(14) -0.13983(12) 0.55761(9) 0.0356(4) Uani 1 1 d .
H10A H 0.1255 -0.0823 0.5915 0.053 Uiso 1 1 calc R
H10B H 0.1083 -0.1972 0.5895 0.053 Uiso 1 1 calc R
H10C H 0.0612 -0.1338 0.5146 0.053 Uiso 1 1 calc R
C11 C 0.68474(12) 0.00167(9) 0.67009(7) 0.0208(3) Uani 1 1 d .
H11A H 0.6483 0.0598 0.6416 0.025 Uiso 1 1 calc R
C12 C 0.70934(14) 0.02989(10) 0.75722(8) 0.0294(3) Uani 1 1 d .
H12A H 0.6199 0.0431 0.7830 0.044 Uiso 1 1 calc R
H12B H 0.7677 0.0878 0.7594 0.044 Uiso 1 1 calc R
H12C H 0.7561 -0.0232 0.7850 0.044 Uiso 1 1 calc R
C13 C 0.82321(13) -0.02649(10) 0.63119(9) 0.0271(3) Uani 1 1 d .
H13A H 0.8071 -0.0443 0.5755 0.041 Uiso 1 1 calc R
H13B H 0.8635 -0.0815 0.6597 0.041 Uiso 1 1 calc R
H13C H 0.8875 0.0283 0.6336 0.041 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
O1 C1 C2 123.53(11) .
O1 C1 C1 119.17(13) 5_656
C2 C1 C1 117.30(12) 5_656
C3 C2 C7 122.01(11) .
C3 C2 C1 118.08(10) .
C7 C2 C1 119.89(10) .
C4 C3 C2 118.32(11) .
C4 C3 C8 120.71(11) .
C2 C3 C8 120.90(11) .
C5 C4 C3 120.42(12) .
C5 C4 H4A 119.8 .
C3 C4 H4A 119.8 .
C6 C5 C4 120.57(12) .
C6 C5 H5A 119.7 .
C4 C5 H5A 119.7 .
C5 C6 C7 121.13(12) .
C5 C6 H6A 119.4 .
C7 C6 H6A 119.4 .
C6 C7 C2 117.53(11) .
C6 C7 C11 120.74(11) .
C2 C7 C11 121.67(11) .
C9 C8 C3 112.75(10) .
C9 C8 C10 110.64(11) .
C3 C8 C10 111.10(10) .
C9 C8 H8A 107.4 .
C3 C8 H8A 107.4 .
C10 C8 H8A 107.4 .
C8 C9 H9A 109.5 .
C8 C9 H9B 109.5 .
H9A C9 H9B 109.5 .
C8 C9 H9C 109.5 .
H9A C9 H9C 109.5 .
H9B C9 H9C 109.5 .
C8 C10 H10A 109.5 .
C8 C10 H10B 109.5 .
H10A C10 H10B 109.5 .
C8 C10 H10C 109.5 .
H10A C10 H10C 109.5 .
H10B C10 H10C 109.5 .
C7 C11 C12 113.17(10) .
C7 C11 C13 110.36(10) .
C12 C11 C13 109.72(10) .
C7 C11 H11A 107.8 .
C12 C11 H11A 107.8 .
C13 C11 H11A 107.8 .
C11 C12 H12A 109.5 .
C11 C12 H12B 109.5 .
H12A C12 H12B 109.5 .
C11 C12 H12C 109.5 .
H12A C12 H12C 109.5 .
H12B C12 H12C 109.5 .
C11 C13 H13A 109.5 .
C11 C13 H13B 109.5 .
H13A C13 H13B 109.5 .
C11 C13 H13C 109.5 .
H13A C13 H13C 109.5 .
H13B C13 H13C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C1 1.2141(15) .
C1 C2 1.5051(17) .
C1 C1 1.558(2) 5_656
C2 C3 1.4025(17) .
C2 C7 1.4103(16) .
C3 C4 1.3943(18) .
C3 C8 1.5251(17) .
C4 C5 1.3871(19) .
C4 H4A 0.9500 .
C5 C6 1.3861(18) .
C5 H5A 0.9500 .
C6 C7 1.3930(17) .
C6 H6A 0.9500 .
C7 C11 1.5237(17) .
C8 C9 1.5248(18) .
C8 C10 1.5303(17) .
C8 H8A 1.0000 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.5335(18) .
C11 C13 1.5342(17) .
C11 H11A 1.0000 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
