#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:06:25 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180123 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/21/7102162.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_7102162
loop_
_publ_author_name
'Meier, Roland'
'Maigut, Joachim'
'Kallies, Bernd'
'Lehnert, Nicolai'
'Paulat, Florian'
'Heinemann, Frank W'
'Zahn, Gernot'
'Feth, Martin P'
'Krautscheid, Harald'
'van Eldik, Rudi'
_publ_section_title
;
 [FeIII(tmdta)]--twist-boat/half-chair conformer ratio reliably deduced
 from DFT-calculated Raman spectra.
;
_journal_issue                   38
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3960
_journal_page_last               3962
_journal_paper_doi               10.1039/b708437d
_journal_year                    2007
_chemical_formula_sum            'C11 H14 Fe K N2 O8'
_chemical_formula_weight         397.19
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 97.577(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7684(7)
_cell_length_b                   12.4703(7)
_cell_length_c                   12.8511(10)
_cell_measurement_temperature    100(2)
_cell_volume                     1392.93(17)
_computing_cell_refinement       'Stoe, X-AREA '
_computing_data_collection       'Stoe, X-AREA'
_computing_data_reduction        'Stoe, X-AREA'
_computing_molecular_graphics    'Diamond 3, Crystal Impact'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12562
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         5.32
_exptl_absorpt_coefficient_mu    1.428
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.6500
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'optimized faces with STOE X-SHAPE'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0061(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0215
_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/[σ²(Fo²)+(0.0267P)²+0.6494P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0584
_reflns_number_gt                3395
_reflns_number_total             3661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708437d.txt
_cod_data_source_block           KFe(tmdta)_CCDC649047
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7102162
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y-1/2, -z-1/2'
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
Fe Fe 0.747801(16) 0.246580(12) 0.240721(12) 0.00644(6) Uani 1 1 d .
O1 O 0.57543(9) 0.20132(7) 0.13725(6) 0.01076(16) Uani 1 1 d .
O2 O 0.32886(10) 0.23484(7) 0.07486(7) 0.01532(17) Uani 1 1 d .
O3 O 0.69208(9) 0.15083(6) 0.35258(6) 0.01009(15) Uani 1 1 d .
O4 O 0.50945(10) 0.10650(7) 0.44878(6) 0.01214(16) Uani 1 1 d .
O5 O 0.93283(9) 0.16336(6) 0.22230(6) 0.00986(15) Uani 1 1 d .
O6 O 1.17178(9) 0.12226(7) 0.29602(7) 0.01272(17) Uani 1 1 d .
O7 O 0.81428(9) 0.36440(6) 0.15284(6) 0.00953(15) Uani 1 1 d .
O8 O 1.03287(10) 0.44474(7) 0.12649(7) 0.01307(17) Uani 1 1 d .
N1 N 0.56741(11) 0.34517(7) 0.29494(7) 0.00776(17) Uani 1 1 d .
N2 N 0.91443(11) 0.32610(7) 0.35963(7) 0.00786(17) Uani 1 1 d .
C1 C 0.61907(13) 0.45333(9) 0.33488(9) 0.0102(2) Uani 1 1 d .
H1A H 0.5269 0.4955 0.3460 0.012 Uiso 1 1 calc R
H1B H 0.6682 0.4901 0.2797 0.012 Uiso 1 1 calc R
C2 C 0.73163(13) 0.45527(9) 0.43690(9) 0.0124(2) Uani 1 1 d .
H2A H 0.7873 0.5245 0.4399 0.015 Uiso 1 1 calc R
H2B H 0.6704 0.4543 0.4963 0.015 Uiso 1 1 calc R
C3 C 0.85152(13) 0.36552(9) 0.45492(8) 0.0103(2) Uani 1 1 d .
H3A H 0.9384 0.3914 0.5058 0.012 Uiso 1 1 calc R
H3B H 0.8045 0.3041 0.4877 0.012 Uiso 1 1 calc R
C4 C 0.46026(13) 0.35931(9) 0.19655(8) 0.0103(2) Uani 1 1 d .
H4A H 0.4970 0.4187 0.1552 0.012 Uiso 1 1 calc R
H4B H 0.3571 0.3788 0.2139 0.012 Uiso 1 1 calc R
C5 C 0.44839(13) 0.25695(9) 0.13083(8) 0.0102(2) Uani 1 1 d .
C6 C 0.49306(12) 0.28027(9) 0.37156(8) 0.0096(2) Uani 1 1 d .
H6A H 0.3831 0.2702 0.3442 0.012 Uiso 1 1 calc R
H6B H 0.4985 0.3203 0.4385 0.012 Uiso 1 1 calc R
C7 C 0.56755(12) 0.17070(9) 0.39303(8) 0.00853(19) Uani 1 1 d .
C8 C 1.02237(13) 0.23695(9) 0.39110(8) 0.0097(2) Uani 1 1 d .
H8A H 0.9799 0.1912 0.4433 0.012 Uiso 1 1 calc R
H8B H 1.1218 0.2665 0.4244 0.012 Uiso 1 1 calc R
C9 C 1.04894(13) 0.16915(9) 0.29630(8) 0.00920(19) Uani 1 1 d .
C10 C 0.99270(13) 0.41013(9) 0.30425(8) 0.0102(2) Uani 1 1 d .
H10A H 1.1055 0.4012 0.3210 0.012 Uiso 1 1 calc R
H10B H 0.9655 0.4816 0.3299 0.012 Uiso 1 1 calc R
C11 C 0.94827(13) 0.40533(9) 0.18520(8) 0.00922(19) Uani 1 1 d .
K K 0.24392(2) 0.470479(19) -0.001680(17) 0.00892(7) Uani 1 1 d .
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'
N N 0.0061 0.0033 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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_1
_geom_angle_site_symmetry_3
O1 Fe O5 109.94(3) . .
O1 Fe O3 94.41(3) . .
O5 Fe O3 93.19(3) . .
O1 Fe O7 94.88(3) . .
O5 Fe O7 90.76(3) . .
O3 Fe O7 168.00(3) . .
O1 Fe N1 81.53(3) . .
O5 Fe N1 167.76(3) . .
O3 Fe N1 81.35(3) . .
O7 Fe N1 92.53(3) . .
O1 Fe N2 168.73(3) . .
O5 Fe N2 80.73(3) . .
O3 Fe N2 88.42(3) . .
O7 Fe N2 81.03(3) . .
N1 Fe N2 88.13(3) . .
C5 O1 Fe 117.72(7) . .
C5 O2 K 97.02(7) . .
C7 O3 Fe 118.60(7) . .
C7 O3 K 89.05(6) . 4_656
Fe O3 K 152.23(4) . 4_656
C7 O4 K 144.52(7) . 2
C7 O4 K 99.92(7) . 4_656
K O4 K 113.54(3) 2 4_656
C9 O5 Fe 117.49(7) . .
C9 O6 K 106.34(7) . 2_655
C11 O7 Fe 115.45(7) . .
C11 O7 K 90.43(6) . 3_665
Fe O7 K 152.64(4) . 3_665
C11 O8 K 163.05(8) . 1_655
C11 O8 K 87.52(7) . 3_665
K O8 K 102.24(3) 1_655 3_665
C4 N1 C6 110.18(8) . .
C4 N1 C1 108.38(8) . .
C6 N1 C1 113.78(8) . .
C4 N1 Fe 101.45(6) . .
C6 N1 Fe 107.63(6) . .
C1 N1 Fe 114.70(7) . .
C8 N2 C10 109.97(9) . .
C8 N2 C3 108.38(8) . .
C10 N2 C3 113.92(8) . .
C8 N2 Fe 101.11(6) . .
C10 N2 Fe 106.92(6) . .
C3 N2 Fe 115.73(7) . .
N1 C1 C2 116.12(9) . .
C3 C2 C1 117.97(9) . .
N2 C3 C2 115.94(9) . .
N1 C4 C5 111.20(9) . .
N1 C4 K 161.80(7) . .
C5 C4 K 86.18(6) . .
O2 C5 O1 125.15(11) . .
O2 C5 C4 120.33(10) . .
O1 C5 C4 114.45(10) . .
O2 C5 K 62.83(6) . .
O1 C5 K 143.91(7) . .
C4 C5 K 68.19(6) . .
N1 C6 C7 113.11(8) . .
O4 C7 O3 123.11(10) . .
O4 C7 C6 119.27(10) . .
O3 C7 C6 117.60(9) . .
O4 C7 K 57.93(6) . 4_656
O3 C7 K 67.19(6) . 4_656
C6 C7 K 163.71(7) . 4_656
N2 C8 C9 110.93(9) . .
N2 C8 K 171.04(7) . 2_655
C9 C8 K 76.34(6) . 2_655
O6 C9 O5 125.09(10) . .
O6 C9 C8 119.56(10) . .
O5 C9 C8 115.30(9) . .
O6 C9 K 53.38(6) . 2_655
O5 C9 K 142.91(7) . 2_655
C8 C9 K 77.77(6) . 2_655
N2 C10 C11 112.27(9) . .
O8 C11 O7 123.71(10) . .
O8 C11 C10 120.26(10) . .
O7 C11 C10 115.87(9) . .
O8 C11 K 69.34(6) . 3_665
O7 C11 K 65.01(6) . 3_665
C10 C11 K 140.99(7) . 3_665
O8 K O4 143.63(3) 1_455 2_554
O8 K O4 120.59(3) 1_455 4_666
O4 K O4 66.46(3) 2_554 4_666
O8 K O7 115.88(3) 1_455 3_665
O4 K O7 100.47(3) 2_554 3_665
O4 K O7 77.68(3) 4_666 3_665
O8 K O6 115.44(3) 1_455 2_454
O4 K O6 74.42(3) 2_554 2_454
O4 K O6 123.24(2) 4_666 2_454
O7 K O6 70.71(2) 3_665 2_454
O8 K O8 77.76(3) 1_455 3_665
O4 K O8 133.26(3) 2_554 3_665
O4 K O8 118.63(3) 4_666 3_665
O7 K O8 45.51(2) 3_665 3_665
O6 K O8 64.95(2) 2_454 3_665
O8 K O3 77.19(3) 1_455 4_666
O4 K O3 109.30(2) 2_554 4_666
O4 K O3 45.46(2) 4_666 4_666
O7 K O3 83.87(3) 3_665 4_666
O6 K O3 154.49(2) 2_454 4_666
O8 K O3 98.81(2) 3_665 4_666
O8 K C11 100.23(3) 1_455 3_665
O4 K C11 113.49(3) 2_554 3_665
O4 K C11 102.03(3) 4_666 3_665
O7 K C11 24.56(3) 3_665 3_665
O6 K C11 58.51(3) 2_454 3_665
O8 K C11 23.14(2) 3_665 3_665
O3 K C11 98.59(3) 4_666 3_665
O8 K O2 81.33(3) 1_455 .
O4 K O2 64.06(2) 2_554 .
O4 K O2 110.49(3) 4_666 .
O7 K O2 154.80(2) 3_665 .
O6 K O2 85.47(2) 2_454 .
O8 K O2 130.70(2) 3_665 .
O3 K O2 119.27(2) 4_666 .
C11 K O2 141.14(3) 3_665 .
O8 K C7 100.68(3) 1_455 4_666
O4 K C7 88.17(3) 2_554 4_666
O4 K C7 22.15(2) 4_666 4_666
O7 K C7 76.62(3) 3_665 4_666
O6 K C7 139.00(3) 2_454 4_666
O8 K C7 107.45(3) 3_665 4_666
O3 K C7 23.76(2) 4_666 4_666
C11 K C7 97.95(3) 3_665 4_666
O2 K C7 120.11(3) . 4_666
O8 K C4 81.14(3) 1_455 .
O4 K C4 66.42(3) 2_554 .
O4 K C4 73.39(3) 4_666 .
O7 K C4 151.03(3) 3_665 .
O6 K C4 125.15(3) 2_454 .
O8 K C4 158.88(3) 3_665 .
O3 K C4 77.13(3) 4_666 .
C11 K C4 175.16(3) 3_665 .
O2 K C4 43.55(3) . .
C7 K C4 77.22(3) 4_666 .
O8 K C9 95.19(3) 1_455 2_454
O4 K C9 90.02(3) 2_554 2_454
O4 K C9 143.35(3) 4_666 2_454
O7 K C9 79.70(3) 3_665 2_454
O6 K C9 20.28(2) 2_454 2_454
O8 K C9 57.87(3) 3_665 2_454
O3 K C9 156.66(3) 4_666 2_454
C11 K C9 60.63(3) 3_665 2_454
O2 K C9 80.51(3) . 2_454
C7 K C9 155.50(3) 4_666 2_454
C4 K C9 124.00(3) . 2_454
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe O1 1.9598(8) .
Fe O5 1.9663(8) .
Fe O3 1.9789(8) .
Fe O7 1.9869(8) .
Fe N1 2.1886(9) .
Fe N2 2.2056(9) .
O1 C5 1.3056(14) .
O2 C5 1.2219(14) .
O2 K 3.1565(10) .
O3 C7 1.2937(13) .
O3 K 2.9598(8) 4_656
O4 C7 1.2288(13) .
O4 K 2.6718(8) 2
O4 K 2.7619(9) 4_656
O5 C9 1.3003(13) .
O6 C9 1.2261(14) .
O6 K 2.8395(9) 2_655
O7 C11 1.2980(14) .
O7 K 2.8306(8) 3_665
O8 C11 1.2283(13) .
O8 K 2.6541(8) 1_655
O8 K 2.9248(9) 3_665
N1 C4 1.4831(14) .
N1 C6 1.4896(13) .
N1 C1 1.4921(14) .
N2 C8 1.4813(14) .
N2 C10 1.4847(14) .
N2 C3 1.4913(13) .
C1 C2 1.5338(16) .
C2 C3 1.5320(16) .
C4 C5 1.5265(16) .
C4 K 3.2765(11) .
C5 K 3.5213(11) .
C6 C7 1.5238(15) .
C7 K 3.2105(11) 4_656
C8 C9 1.5259(15) .
C8 K 3.4143(11) 2_655
C9 K 3.3948(11) 2_655
C10 C11 1.5293(15) .
C11 K 3.1229(11) 3_665
K O8 2.6541(8) 1_455
K O4 2.6718(8) 2_554
K O4 2.7620(9) 4_666
K O7 2.8306(8) 3_665
K O6 2.8395(9) 2_454
K O8 2.9248(9) 3_665
K O3 2.9599(8) 4_666
K C11 3.1229(11) 3_665
K C7 3.2106(11) 4_666
K C9 3.3948(11) 2_454
