#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:46:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179262 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/82/4318277.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_4318277
loop_
_publ_author_name
'Arunashree Panda'
'Matthias Stender'
'Robert J. Wright'
'Marilyn M. Olmstead'
'Peter Klavins'
'Philip P. Power'
_publ_section_title
;
 Synthesis and Characterization of Three-Coordinate and Related
 β-Diketiminate Derivatives of Manganese, Iron, and Cobalt
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3909
_journal_page_last               3916
_journal_paper_doi               10.1021/ic025552s
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C35 H59 Fe N3 Si2'
_chemical_formula_weight         633.88
_chemical_name_common            NacNacFeN(SiMe3)2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.5030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0729(5)
_cell_length_b                   20.1860(10)
_cell_length_c                   20.2150(10)
_cell_measurement_reflns_used    7004
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.16
_cell_measurement_theta_min      2.25
_cell_volume                     3702.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL v. 5.10'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 5.10'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 5.10'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 5.10'
_computing_structure_solution    'XS, Bruker SHELXTL v. 5.10'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            51147
_diffrn_reflns_theta_full        31.49
_diffrn_reflns_theta_max         31.49
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        <0.01
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_T_max  0.8885
_exptl_absorpt_correction_T_min  0.8828
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS: an empirical absorption program by G. M. Sheldrick
using the method described by Blessing, R. H.; Acta Cryst.
A51, 1995, 33.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.00000(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         11824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          4.766
_refine_ls_shift/su_mean         0.064
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0509P)²+0.4022P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                9272
_reflns_number_total             11824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025552s_s1_2.cif
_cod_data_source_block           mas34
_cod_database_code               4318277
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.692779(18) 0.244671(8) 0.124034(8) 0.01283(5) Uani 1 1 d . . .
N1 N 0.60232(11) 0.16385(5) 0.08023(5) 0.01353(18) Uani 1 1 d . . .
N2 N 0.59235(11) 0.30871(5) 0.06409(5) 0.01340(18) Uani 1 1 d . . .
N3 N 0.81749(11) 0.25304(5) 0.20132(5) 0.01498(19) Uani 1 1 d . . .
Si1 Si 0.72666(4) 0.231231(16) 0.272141(17) 0.01602(7) Uani 1 1 d . . .
Si2 Si 1.00423(4) 0.265201(18) 0.194933(18) 0.01869(8) Uani 1 1 d . . .
C1 C 0.49272(13) 0.16791(6) 0.03644(6) 0.0149(2) Uani 1 1 d . . .
C2 C 0.42334(13) 0.22786(6) 0.01845(6) 0.0160(2) Uani 1 1 d . . .
H2A H 0.3314 0.2235 -0.0039 0.019 Uiso 1 1 calc R . .
C3 C 0.47126(13) 0.29295(6) 0.02903(6) 0.0143(2) Uani 1 1 d . . .
C4 C 0.43590(14) 0.10675(6) 0.00075(7) 0.0206(2) Uani 1 1 d . . .
H4A H 0.5123 0.0724 0.0012 0.031 Uiso 1 1 calc R . .
H4B H 0.4108 0.1182 -0.0451 0.031 Uiso 1 1 calc R . .
H4C H 0.3479 0.0901 0.0231 0.031 Uiso 1 1 calc R . .
C5 C 0.37978(14) 0.34734(6) -0.00223(6) 0.0181(2) Uani 1 1 d . . .
H5A H 0.4451 0.3800 -0.0226 0.027 Uiso 1 1 calc R . .
H5B H 0.3204 0.3690 0.0318 0.027 Uiso 1 1 calc R . .
H5C H 0.3146 0.3283 -0.0361 0.027 Uiso 1 1 calc R . .
C6 C 0.67304(13) 0.10114(6) 0.09265(6) 0.0154(2) Uani 1 1 d . . .
C7 C 0.81429(13) 0.09122(6) 0.06550(6) 0.0168(2) Uani 1 1 d . . .
C8 C 0.88837(15) 0.03225(6) 0.07982(7) 0.0214(3) Uani 1 1 d . . .
H8A H 0.9835 0.0248 0.0620 0.026 Uiso 1 1 calc R . .
C9 C 0.82490(16) -0.01576(6) 0.11976(7) 0.0240(3) Uani 1 1 d . . .
H9A H 0.8766 -0.0556 0.1291 0.029 Uiso 1 1 calc R . .
C10 C 0.68671(15) -0.00548(6) 0.14576(7) 0.0222(3) Uani 1 1 d . . .
H10A H 0.6444 -0.0387 0.1729 0.027 Uiso 1 1 calc R . .
C11 C 0.60730(14) 0.05265(6) 0.13325(6) 0.0179(2) Uani 1 1 d . . .
C12 C 0.45425(15) 0.05996(6) 0.16300(7) 0.0208(2) Uani 1 1 d . . .
H12A H 0.4137 0.1040 0.1494 0.025 Uiso 1 1 calc R . .
C13 C 0.34779(16) 0.00585(7) 0.13795(8) 0.0286(3) Uani 1 1 d . . .
H13A H 0.3470 0.0055 0.0895 0.043 Uiso 1 1 calc R . .
H13B H 0.2483 0.0151 0.1540 0.043 Uiso 1 1 calc R . .
H13C H 0.3804 -0.0374 0.1544 0.043 Uiso 1 1 calc R . .
C14 C 0.45815(17) 0.05712(7) 0.23913(7) 0.0278(3) Uani 1 1 d . . .
H14A H 0.5264 0.0908 0.2561 0.042 Uiso 1 1 calc R . .
H14B H 0.4913 0.0132 0.2535 0.042 Uiso 1 1 calc R . .
H14C H 0.3592 0.0656 0.2563 0.042 Uiso 1 1 calc R . .
C15 C 0.88197(13) 0.14309(6) 0.02001(6) 0.0183(2) Uani 1 1 d . . .
H15A H 0.8554 0.1876 0.0381 0.022 Uiso 1 1 calc R . .
C16 C 1.05016(15) 0.13986(7) 0.01695(7) 0.0251(3) Uani 1 1 d . . .
H16A H 1.0913 0.1411 0.0619 0.038 Uiso 1 1 calc R . .
H16B H 1.0871 0.1778 -0.0083 0.038 Uiso 1 1 calc R . .
H16C H 1.0799 0.0986 -0.0048 0.038 Uiso 1 1 calc R . .
C17 C 0.81809(15) 0.13894(7) -0.05033(7) 0.0254(3) Uani 1 1 d . . .
H17A H 0.7111 0.1455 -0.0490 0.038 Uiso 1 1 calc R . .
H17B H 0.8397 0.0953 -0.0691 0.038 Uiso 1 1 calc R . .
H17C H 0.8626 0.1734 -0.0778 0.038 Uiso 1 1 calc R . .
C18 C 0.65028(13) 0.37501(5) 0.05871(6) 0.0150(2) Uani 1 1 d . . .
C19 C 0.75661(13) 0.38748(6) 0.00975(6) 0.0165(2) Uani 1 1 d . . .
C20 C 0.81714(14) 0.45085(6) 0.00624(7) 0.0218(3) Uani 1 1 d . . .
H20A H 0.8887 0.4603 -0.0264 0.026 Uiso 1 1 calc R . .
C21 C 0.77437(15) 0.50034(6) 0.04983(8) 0.0255(3) Uani 1 1 d . . .
H21A H 0.8174 0.5431 0.0470 0.031 Uiso 1 1 calc R . .
C22 C 0.66984(15) 0.48749(6) 0.09704(7) 0.0239(3) Uani 1 1 d . . .
H22A H 0.6413 0.5218 0.1264 0.029 Uiso 1 1 calc R . .
C23 C 0.60473(14) 0.42492(6) 0.10278(6) 0.0183(2) Uani 1 1 d . . .
C24 C 0.49012(15) 0.41286(6) 0.15567(6) 0.0220(3) Uani 1 1 d . . .
H24A H 0.4505 0.3670 0.1497 0.026 Uiso 1 1 calc R . .
C25 C 0.36045(18) 0.46173(8) 0.15032(8) 0.0329(3) Uani 1 1 d . . .
H25A H 0.3206 0.4611 0.1051 0.049 Uiso 1 1 calc R . .
H25B H 0.3949 0.5065 0.1611 0.049 Uiso 1 1 calc R . .
H25C H 0.2832 0.4487 0.1813 0.049 Uiso 1 1 calc R . .
C26 C 0.5613(2) 0.41717(8) 0.22449(7) 0.0335(3) Uani 1 1 d . . .
H26A H 0.6430 0.3855 0.2276 0.050 Uiso 1 1 calc R . .
H26B H 0.4877 0.4066 0.2581 0.050 Uiso 1 1 calc R . .
H26C H 0.5987 0.4621 0.2319 0.050 Uiso 1 1 calc R . .
C27 C 0.80404(13) 0.33355(6) -0.03826(6) 0.0179(2) Uani 1 1 d . . .
H27A H 0.7968 0.2902 -0.0145 0.022 Uiso 1 1 calc R . .
C28 C 0.96358(15) 0.34110(7) -0.06115(7) 0.0248(3) Uani 1 1 d . . .
H28A H 1.0279 0.3487 -0.0227 0.037 Uiso 1 1 calc R . .
H28B H 0.9706 0.3788 -0.0915 0.037 Uiso 1 1 calc R . .
H28C H 0.9944 0.3006 -0.0840 0.037 Uiso 1 1 calc R . .
C29 C 0.70230(16) 0.32952(7) -0.09922(7) 0.0263(3) Uani 1 1 d . . .
H29A H 0.6024 0.3179 -0.0853 0.039 Uiso 1 1 calc R . .
H29B H 0.7391 0.2956 -0.1296 0.039 Uiso 1 1 calc R . .
H29C H 0.7004 0.3725 -0.1217 0.039 Uiso 1 1 calc R . .
C30 C 0.75619(17) 0.29028(7) 0.34291(7) 0.0257(3) Uani 1 1 d . . .
H30A H 0.7464 0.3359 0.3269 0.039 Uiso 1 1 calc R . .
H30B H 0.8551 0.2838 0.3616 0.039 Uiso 1 1 calc R . .
H30C H 0.6825 0.2819 0.3771 0.039 Uiso 1 1 calc R . .
C31 C 0.78588(15) 0.14745(7) 0.30299(7) 0.0244(3) Uani 1 1 d . . .
H31A H 0.8863 0.1503 0.3210 0.037 Uiso 1 1 calc R . .
H31B H 0.7835 0.1157 0.2663 0.037 Uiso 1 1 calc R . .
H31C H 0.7187 0.1327 0.3377 0.037 Uiso 1 1 calc R . .
C32 C 0.52300(15) 0.23175(6) 0.25360(7) 0.0217(3) Uani 1 1 d . . .
H32A H 0.4905 0.2773 0.2451 0.033 Uiso 1 1 calc R . .
H32B H 0.4696 0.2138 0.2915 0.033 Uiso 1 1 calc R . .
H32C H 0.5029 0.2044 0.2145 0.033 Uiso 1 1 calc R . .
C33 C 1.10943(16) 0.18537(8) 0.20327(8) 0.0305(3) Uani 1 1 d . . .
H33A H 1.0610 0.1510 0.1766 0.046 Uiso 1 1 calc R . .
H33B H 1.1117 0.1717 0.2498 0.046 Uiso 1 1 calc R . .
H33C H 1.2104 0.1918 0.1877 0.046 Uiso 1 1 calc R . .
C34 C 1.08022(17) 0.32374(9) 0.25888(8) 0.0347(4) Uani 1 1 d . . .
H34A H 1.0267 0.3658 0.2565 0.052 Uiso 1 1 calc R . .
H34B H 1.1850 0.3315 0.2505 0.052 Uiso 1 1 calc R . .
H34C H 1.0686 0.3044 0.3030 0.052 Uiso 1 1 calc R . .
C35 C 1.04710(16) 0.30284(7) 0.11270(7) 0.0267(3) Uani 1 1 d . . .
H35A H 0.9974 0.3458 0.1087 0.040 Uiso 1 1 calc R . .
H35B H 1.0125 0.2733 0.0773 0.040 Uiso 1 1 calc R . .
H35C H 1.1538 0.3091 0.1090 0.040 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
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
_geom_angle_publ_flag
N3 Fe1 N2 134.39(4) . . ?
N3 Fe1 N1 131.07(4) . . ?
N2 Fe1 N1 94.33(4) . . ?
C1 N1 C6 120.03(9) . . ?
C1 N1 Fe1 122.65(8) . . ?
C6 N1 Fe1 116.96(7) . . ?
C3 N2 C18 118.55(10) . . ?
C3 N2 Fe1 122.49(8) . . ?
C18 N2 Fe1 118.95(7) . . ?
Si1 N3 Si2 125.50(6) . . ?
Si1 N3 Fe1 111.77(5) . . ?
Si2 N3 Fe1 121.58(6) . . ?
N3 Si1 C30 113.96(6) . . ?
N3 Si1 C32 108.08(6) . . ?
C30 Si1 C32 106.33(6) . . ?
N3 Si1 C31 111.70(6) . . ?
C30 Si1 C31 106.24(6) . . ?
C32 Si1 C31 110.39(6) . . ?
N3 Si2 C35 109.73(6) . . ?
N3 Si2 C34 113.24(6) . . ?
C35 Si2 C34 106.14(7) . . ?
N3 Si2 C33 111.78(6) . . ?
C35 Si2 C33 108.56(7) . . ?
C34 Si2 C33 107.14(8) . . ?
N1 C1 C2 123.70(10) . . ?
N1 C1 C4 121.04(10) . . ?
C2 C1 C4 115.24(10) . . ?
C3 C2 C1 128.95(11) . . ?
N2 C3 C2 123.75(10) . . ?
N2 C3 C5 119.55(10) . . ?
C2 C3 C5 116.70(10) . . ?
C7 C6 C11 121.10(11) . . ?
C7 C6 N1 117.46(10) . . ?
C11 C6 N1 121.36(11) . . ?
C8 C7 C6 118.49(11) . . ?
C8 C7 C15 120.96(11) . . ?
C6 C7 C15 120.53(10) . . ?
C9 C8 C7 120.93(12) . . ?
C10 C9 C8 119.94(12) . . ?
C9 C10 C11 121.72(12) . . ?
C10 C11 C6 117.83(12) . . ?
C10 C11 C12 118.63(11) . . ?
C6 C11 C12 123.53(11) . . ?
C11 C12 C13 111.84(11) . . ?
C11 C12 C14 112.17(11) . . ?
C13 C12 C14 108.11(11) . . ?
C7 C15 C17 111.75(10) . . ?
C7 C15 C16 113.71(11) . . ?
C17 C15 C16 109.23(11) . . ?
C23 C18 C19 121.48(11) . . ?
C23 C18 N2 120.44(11) . . ?
C19 C18 N2 118.05(10) . . ?
C20 C19 C18 118.13(11) . . ?
C20 C19 C27 120.65(11) . . ?
C18 C19 C27 121.22(10) . . ?
C21 C20 C19 121.00(13) . . ?
C22 C21 C20 120.15(12) . . ?
C21 C22 C23 121.44(12) . . ?
C22 C23 C18 117.80(12) . . ?
C22 C23 C24 119.70(11) . . ?
C18 C23 C24 122.50(11) . . ?
C23 C24 C26 110.19(12) . . ?
C23 C24 C25 112.09(11) . . ?
C26 C24 C25 110.09(12) . . ?
C19 C27 C28 113.24(10) . . ?
C19 C27 C29 112.21(10) . . ?
C28 C27 C29 109.03(11) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 1.9284(10) . ?
Fe1 N2 1.9876(10) . ?
Fe1 N1 2.0265(9) . ?
N1 C1 1.3280(15) . ?
N1 C6 1.4402(14) . ?
N2 C3 1.3404(15) . ?
N2 C18 1.4424(14) . ?
N3 Si1 1.7156(11) . ?
N3 Si2 1.7179(11) . ?
Si1 C30 1.8795(14) . ?
Si1 C32 1.8822(14) . ?
Si1 C31 1.8793(13) . ?
Si2 C35 1.8717(14) . ?
Si2 C34 1.8780(15) . ?
Si2 C33 1.8797(15) . ?
C1 C2 1.4102(16) . ?
C1 C4 1.5180(16) . ?
C2 C3 1.3998(16) . ?
C3 C5 1.5115(16) . ?
C6 C7 1.4127(17) . ?
C6 C11 1.4129(17) . ?
C7 C8 1.3961(17) . ?
C7 C15 1.5260(17) . ?
C8 C9 1.3895(19) . ?
C9 C10 1.379(2) . ?
C10 C11 1.3987(17) . ?
C11 C12 1.5252(18) . ?
C12 C13 1.5408(18) . ?
C12 C14 1.5401(19) . ?
C15 C17 1.5331(18) . ?
C15 C16 1.5292(18) . ?
C18 C23 1.4090(16) . ?
C18 C19 1.4109(17) . ?
C19 C20 1.3942(16) . ?
C19 C27 1.5230(17) . ?
C20 C21 1.390(2) . ?
C21 C22 1.376(2) . ?
C22 C23 1.3996(17) . ?
C23 C24 1.5176(19) . ?
C24 C26 1.531(2) . ?
C24 C25 1.5384(19) . ?
C27 C28 1.5311(18) . ?
C27 C29 1.5353(18) . ?
