#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:45:32 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179076 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/38/4303827.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_4303827
loop_
_publ_author_name
'Brenda A. Frazier'
'Peter T. Wolczanski'
'Emil B. Lobkovsky'
_publ_section_title
;
Aryl-Containing Chelates and Amine Debenzylation to Afford
1,3-Di-2-pyridyl-2-azaallyl (smif): Structures of
{κ-C,N,Npy2-(2-pyridylmethyl)2N(CH2(4-tBu-phenyl-2-yl))}FeBr and
(smif)CrN(TMS)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11576
_journal_page_last               11585
_journal_paper_doi               10.1021/ic901329z
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C18 H28 Cr N4 Si2'
_chemical_formula_sum            'C18 H28 Cr N4 Si2'
_chemical_formula_weight         408.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.2630(10)
_cell_angle_beta                 91.093(4)
_cell_angle_gamma                107.584(4)
_cell_formula_units_Z            2
_cell_length_a                   8.0101(4)
_cell_length_b                   11.5495(5)
_cell_length_c                   11.9921(7)
_cell_measurement_reflns_used    2342
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.75
_cell_measurement_theta_min      2.39
_cell_volume                     1051.84(10)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0743
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7678
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  0.8783
_exptl_absorpt_correction_T_min  0.7765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         7678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0340P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                5121
_reflns_number_total             7678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901329z_si_001_2.cif
_cod_data_source_block           bf5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1051.84(9)
_cod_database_code               4303827
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.22219(4) 0.13162(2) 0.35401(2) 0.02833(8) Uani 1 1 d . . .
Si1 Si 0.44593(7) 0.36577(4) 0.26179(4) 0.02908(14) Uani 1 1 d . . .
Si2 Si 0.08857(7) 0.24743(5) 0.14460(4) 0.02992(14) Uani 1 1 d . . .
N1 N 0.13326(18) 0.21937(12) 0.48978(11) 0.0275(4) Uani 1 1 d . . .
N2 N 0.24329(18) 0.02682(12) 0.47851(12) 0.0283(4) Uani 1 1 d . . .
N3 N 0.31113(18) -0.00185(12) 0.26774(12) 0.0305(4) Uani 1 1 d . . .
N4 N 0.25013(18) 0.25476(11) 0.24038(11) 0.0227(3) Uani 1 1 d . . .
C1 C 0.0707(3) 0.31454(16) 0.49230(16) 0.0341(5) Uani 1 1 d . . .
H1 H 0.0591(18) 0.3432(13) 0.4265(12) 0.016(4) Uiso 1 1 d . . .
C2 C 0.0239(3) 0.36657(17) 0.58878(17) 0.0382(5) Uani 1 1 d . . .
H2 H -0.0203(19) 0.4254(13) 0.5830(13) 0.024(5) Uiso 1 1 d . . .
C3 C 0.0451(3) 0.32046(18) 0.68894(18) 0.0433(6) Uani 1 1 d . . .
H3 H 0.013(2) 0.3581(14) 0.7484(14) 0.035(5) Uiso 1 1 d . . .
C4 C 0.1062(3) 0.22357(18) 0.68814(16) 0.0382(6) Uani 1 1 d . . .
H4 H 0.125(2) 0.1898(14) 0.7563(13) 0.035(5) Uiso 1 1 d . . .
C5 C 0.1493(2) 0.17042(16) 0.58807(15) 0.0302(5) Uani 1 1 d . . .
C6 C 0.2058(2) 0.06552(16) 0.58032(16) 0.0345(5) Uani 1 1 d . . .
H6 H 0.219(2) 0.0211(14) 0.6518(14) 0.040(5) Uiso 1 1 d . . .
C7 C 0.3008(2) -0.06666(16) 0.44873(16) 0.0346(5) Uani 1 1 d . . .
H7 H 0.325(2) -0.1184(16) 0.4926(15) 0.054(6) Uiso 1 1 d . . .
C8 C 0.3365(2) -0.08506(15) 0.33461(16) 0.0307(5) Uani 1 1 d . . .
C9 C 0.3950(3) -0.18137(17) 0.28926(19) 0.0398(6) Uani 1 1 d . . .
H9 H 0.414(2) -0.2295(14) 0.3419(13) 0.028(5) Uiso 1 1 d . . .
C10 C 0.4261(3) -0.19287(18) 0.17842(19) 0.0444(6) Uani 1 1 d . . .
H10 H 0.465(2) -0.2522(15) 0.1506(15) 0.042(6) Uiso 1 1 d . . .
C11 C 0.4029(3) -0.10923(19) 0.11153(18) 0.0449(6) Uani 1 1 d . . .
H11 H 0.408(2) -0.1142(16) 0.0440(15) 0.049(6) Uiso 1 1 d . . .
C12 C 0.3446(3) -0.01643(18) 0.15911(17) 0.0382(5) Uani 1 1 d . . .
H12 H 0.326(2) 0.0418(14) 0.1231(13) 0.031(5) Uiso 1 1 d . . .
C13 C 0.5957(2) 0.31325(17) 0.35223(16) 0.0401(6) Uani 1 1 d . . .
H13A H 0.5471 0.3012 0.4262 0.060 Uiso 1 1 calc R . .
H13B H 0.7113 0.3750 0.3605 0.060 Uiso 1 1 calc R . .
H13C H 0.6070 0.2360 0.3174 0.060 Uiso 1 1 calc R . .
C14 C 0.5573(3) 0.40503(19) 0.12963(16) 0.0494(6) Uani 1 1 d . . .
H14A H 0.5794 0.3325 0.0919 0.074 Uiso 1 1 calc R . .
H14B H 0.6689 0.4696 0.1469 0.074 Uiso 1 1 calc R . .
H14C H 0.4823 0.4336 0.0804 0.074 Uiso 1 1 calc R . .
C15 C 0.4311(3) 0.51118(16) 0.33512(18) 0.0473(6) Uani 1 1 d . . .
H15A H 0.3503 0.5412 0.2921 0.071 Uiso 1 1 calc R . .
H15B H 0.5475 0.5720 0.3418 0.071 Uiso 1 1 calc R . .
H15C H 0.3876 0.4969 0.4100 0.071 Uiso 1 1 calc R . .
C16 C 0.1331(3) 0.2003(2) -0.00226(16) 0.0546(7) Uani 1 1 d . . .
H16A H 0.2362 0.2615 -0.0265 0.082 Uiso 1 1 calc R . .
H16B H 0.0313 0.1935 -0.0520 0.082 Uiso 1 1 calc R . .
H16C H 0.1552 0.1211 -0.0053 0.082 Uiso 1 1 calc R . .
C17 C 0.0414(3) 0.39627(17) 0.13892(17) 0.0487(6) Uani 1 1 d . . .
H17A H 0.0168 0.4261 0.2141 0.073 Uiso 1 1 calc R . .
H17B H -0.0607 0.3843 0.0878 0.073 Uiso 1 1 calc R . .
H17C H 0.1433 0.4562 0.1119 0.073 Uiso 1 1 calc R . .
C18 C -0.1160(3) 0.13271(18) 0.18000(16) 0.0474(6) Uani 1 1 d . . .
H18A H -0.0975 0.0525 0.1778 0.071 Uiso 1 1 calc R . .
H18B H -0.2107 0.1290 0.1255 0.071 Uiso 1 1 calc R . .
H18C H -0.1479 0.1561 0.2554 0.071 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'
Cr Cr 0.3209 0.6236 '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
N4 Cr1 N2 168.76(6) . . ?
N4 Cr1 N3 101.74(6) . . ?
N2 Cr1 N3 78.35(6) . . ?
N4 Cr1 N1 101.04(6) . . ?
N2 Cr1 N1 78.80(6) . . ?
N3 Cr1 N1 157.07(6) . . ?
N4 Si1 C14 112.99(8) . . ?
N4 Si1 C15 113.80(8) . . ?
C14 Si1 C15 106.56(10) . . ?
N4 Si1 C13 109.39(8) . . ?
C14 Si1 C13 107.43(9) . . ?
C15 Si1 C13 106.26(9) . . ?
N4 Si2 C18 109.05(8) . . ?
N4 Si2 C16 114.22(9) . . ?
C18 Si2 C16 106.57(9) . . ?
N4 Si2 C17 113.31(8) . . ?
C18 Si2 C17 107.77(10) . . ?
C16 Si2 C17 105.51(10) . . ?
C1 N1 C5 118.80(15) . . ?
C1 N1 Cr1 129.05(12) . . ?
C5 N1 Cr1 112.12(12) . . ?
C7 N2 C6 128.48(17) . . ?
C7 N2 Cr1 115.77(13) . . ?
C6 N2 Cr1 115.65(13) . . ?
C12 N3 C8 117.41(16) . . ?
C12 N3 Cr1 129.57(13) . . ?
C8 N3 Cr1 113.02(12) . . ?
Si2 N4 Si1 126.67(8) . . ?
Si2 N4 Cr1 122.23(7) . . ?
Si1 N4 Cr1 110.97(7) . . ?
N1 C1 C2 122.90(18) . . ?
C1 C2 C3 118.7(2) . . ?
C4 C3 C2 119.3(2) . . ?
C3 C4 C5 120.76(19) . . ?
N1 C5 C4 119.42(18) . . ?
N1 C5 C6 116.80(16) . . ?
C4 C5 C6 123.76(18) . . ?
N2 C6 C5 116.29(17) . . ?
N2 C7 C8 116.89(17) . . ?
N3 C8 C9 120.16(18) . . ?
N3 C8 C7 115.94(17) . . ?
C9 C8 C7 123.89(18) . . ?
C10 C9 C8 120.3(2) . . ?
C9 C10 C11 119.7(2) . . ?
C10 C11 C12 118.1(2) . . ?
N3 C12 C11 124.21(19) . . ?
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
Cr1 N4 2.0260(12) . ?
Cr1 N2 2.0416(14) . ?
Cr1 N3 2.0864(15) . ?
Cr1 N1 2.0887(14) . ?
Si1 N4 1.6967(14) . ?
Si1 C14 1.858(2) . ?
Si1 C15 1.8606(19) . ?
Si1 C13 1.8690(19) . ?
Si2 N4 1.6913(14) . ?
Si2 C18 1.8545(19) . ?
Si2 C16 1.8685(19) . ?
Si2 C17 1.875(2) . ?
N1 C1 1.337(2) . ?
N1 C5 1.373(2) . ?
N2 C7 1.320(2) . ?
N2 C6 1.332(2) . ?
N3 C12 1.341(2) . ?
N3 C8 1.364(2) . ?
C1 C2 1.366(3) . ?
C2 C3 1.385(3) . ?
C3 C4 1.349(3) . ?
C4 C5 1.395(3) . ?
C5 C6 1.412(3) . ?
C7 C8 1.414(3) . ?
C8 C9 1.402(3) . ?
C9 C10 1.359(3) . ?
C10 C11 1.362(3) . ?
C11 C12 1.376(3) . ?
