#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:17:29 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178944 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/73/4117396.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_4117396
loop_
_publ_author_name
'Ramachandran Azhakar'
'Rajendra S. Ghadwal'
'Herbert W. Roesky'
'Hilke Wolf'
'Dietmar Stalke'
_publ_section_title
;
 Stabilization of Low Valent Silicon Fluorides in the Coordination Sphere
 of Transition Metals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2423
_journal_page_last               2428
_journal_paper_doi               10.1021/ja210697p
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C7 H8, C20 H23 Cl Cr N2 O5 Si'
_chemical_formula_sum            'C27 H31 Cl Cr N2 O5 Si'
_chemical_formula_weight         579.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 98.60(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.896(3)
_cell_length_b                   13.060(5)
_cell_length_c                   11.577(4)
_cell_measurement_reflns_used    4182
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.23
_cell_measurement_theta_min      2.34
_cell_volume                     1479.4(9)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2011.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_computing_structure_refinement  'SHELXL in SHELXTL Version 2008/3'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/3'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'INCOATEC Ag Microsource'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13702
_diffrn_reflns_theta_full        20.28
_diffrn_reflns_theta_max         20.28
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_T_max  0.9630
_exptl_absorpt_correction_T_min  0.9175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3068
_refine_ls_number_restraints     363
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0510P)²+0.3796P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                2625
_reflns_number_total             3068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210697p_si_002.cif
_cod_data_source_block           test
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4117396
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.42570(4) 0.2500 1.05661(3) 0.03441(13) Uani 1 2 d S . .
O1 O 0.7098(2) 0.2500 1.19423(18) 0.0584(5) Uani 1 2 d S . .
Cl1 Cl 0.03510(7) 0.2500 1.02580(6) 0.05216(19) Uani 1 2 d S . .
Si1 Si 0.20920(7) 0.2500 0.94188(5) 0.03304(16) Uani 1 2 d S . .
N1 N 0.15877(14) 0.16805(10) 0.81459(11) 0.0330(3) Uani 1 1 d . . .
C1 C 0.1399(2) 0.2500 0.74453(18) 0.0306(5) Uani 1 2 d S . .
C2 C 0.1149(2) 0.2500 0.61489(18) 0.0311(5) Uani 1 2 d S . .
O2 O 0.51695(16) 0.08649(11) 0.90040(12) 0.0571(4) Uani 1 1 d . . .
C3 C 0.2262(3) 0.2500 0.5550(2) 0.0415(6) Uani 1 2 d S . .
H3 H 0.3164 0.2500 0.5968 0.050 Uiso 1 2 calc SR . .
O3 O 0.31735(17) 0.41075(11) 1.20781(12) 0.0614(4) Uani 1 1 d . . .
C4 C 0.2054(3) 0.2500 0.4347(2) 0.0506(7) Uani 1 2 d S . .
H4 H 0.2816 0.2500 0.3936 0.061 Uiso 1 2 calc SR . .
C5 C 0.0745(3) 0.2500 0.3736(2) 0.0509(7) Uani 1 2 d S . .
H5 H 0.0608 0.2500 0.2906 0.061 Uiso 1 2 calc SR . .
C6 C -0.0360(3) 0.2500 0.4325(2) 0.0463(6) Uani 1 2 d S . .
H6 H -0.1259 0.2500 0.3900 0.056 Uiso 1 2 calc SR . .
C7 C -0.0172(3) 0.2500 0.5536(2) 0.0380(5) Uani 1 2 d S . .
H7 H -0.0937 0.2500 0.5943 0.046 Uiso 1 2 calc SR . .
C8 C 0.13474(19) 0.05720(13) 0.78883(15) 0.0420(4) Uani 1 1 d . . .
C9 C -0.0173(2) 0.04049(17) 0.7476(2) 0.0673(6) Uani 1 1 d . . .
H9A H -0.0433 0.0735 0.6714 0.101 Uiso 1 1 calc R . .
H9B H -0.0701 0.0704 0.8043 0.101 Uiso 1 1 calc R . .
H9BC H -0.0361 -0.0331 0.7404 0.101 Uiso 1 1 calc R . .
C10 C 0.2207(3) 0.01871(15) 0.69899(18) 0.0601(6) Uani 1 1 d . . .
H10A H 0.2113 -0.0558 0.6914 0.090 Uiso 1 1 calc R . .
H10B H 0.3168 0.0362 0.7245 0.090 Uiso 1 1 calc R . .
H10C H 0.1893 0.0510 0.6233 0.090 Uiso 1 1 calc R . .
C11 C 0.1751(2) 0.00132(14) 0.90496(17) 0.0499(5) Uani 1 1 d . . .
H11A H 0.1568 -0.0720 0.8940 0.075 Uiso 1 1 calc R . .
H11B H 0.1218 0.0284 0.9630 0.075 Uiso 1 1 calc R . .
H11C H 0.2727 0.0118 0.9324 0.075 Uiso 1 1 calc R . .
C12 C 0.6012(3) 0.2500 1.1444(2) 0.0432(6) Uani 1 2 d S . .
C13 C 0.48112(19) 0.14786(14) 0.95857(15) 0.0417(4) Uani 1 1 d . . .
C14 C 0.3592(2) 0.35116(14) 1.15044(14) 0.0427(4) Uani 1 1 d . . .
C1T C 0.6142(15) 0.3268(9) 0.5714(12) 0.073(3) Uani 0.308(4) 1 d PDU A -1
C2T C 0.6439(14) 0.2732(10) 0.6756(10) 0.073(3) Uani 0.308(4) 1 d PDU A -1
H2T H 0.6599 0.3093 0.7476 0.087 Uiso 0.308(4) 1 calc PR A -1
C3T C 0.6503(17) 0.1665(10) 0.6754(11) 0.070(3) Uani 0.308(4) 1 d PDU A -1
H3T H 0.6697 0.1297 0.7467 0.084 Uiso 0.308(4) 1 calc PR A -1
C4T C 0.6286(13) 0.1160(9) 0.5719(12) 0.074(3) Uani 0.308(4) 1 d PDU A -1
H4T H 0.6382 0.0436 0.5708 0.089 Uiso 0.308(4) 1 calc PR A -1
C5T C 0.5927(14) 0.1682(10) 0.4677(10) 0.076(3) Uani 0.308(4) 1 d PDU A -1
H5T H 0.5700 0.1316 0.3965 0.091 Uiso 0.308(4) 1 calc PR A -1
C6T C 0.590(2) 0.2726(10) 0.4683(11) 0.063(3) Uani 0.308(4) 1 d PDU A -1
H6T H 0.5720 0.3085 0.3963 0.076 Uiso 0.308(4) 1 calc PR A -1
C7T C 0.5916(15) 0.4397(9) 0.5465(15) 0.126(5) Uani 0.308(4) 1 d PDU A -1
H7T1 H 0.5564 0.4494 0.4635 0.190 Uiso 0.308(4) 1 calc PR A -1
H7T2 H 0.6784 0.4764 0.5659 0.190 Uiso 0.308(4) 1 calc PR A -1
H7T3 H 0.5254 0.4665 0.5939 0.190 Uiso 0.308(4) 1 calc PR A -1
C1S C 0.6698(18) 0.2629(18) 0.7004(12) 0.058(4) Uani 0.192(4) 1 d PDU A -2
C2S C 0.649(2) 0.3586(16) 0.6460(17) 0.059(4) Uani 0.192(4) 1 d PDU A -2
H2S H 0.6697 0.4197 0.6895 0.071 Uiso 0.192(4) 1 calc PR A -2
C3S C 0.597(2) 0.3633(14) 0.5293(18) 0.068(4) Uani 0.192(4) 1 d PDU A -2
H3S H 0.5802 0.4278 0.4918 0.081 Uiso 0.192(4) 1 calc PR A -2
C4S C 0.571(4) 0.2746(16) 0.4674(17) 0.059(5) Uani 0.192(4) 1 d PDU A -2
H4S H 0.5384 0.2770 0.3859 0.071 Uiso 0.192(4) 1 calc PR A -2
C5S C 0.591(2) 0.1826(14) 0.5228(17) 0.057(4) Uani 0.192(4) 1 d PDU A -2
H5S H 0.5731 0.1221 0.4776 0.069 Uiso 0.192(4) 1 calc PR A -2
C6S C 0.636(3) 0.1725(16) 0.6414(18) 0.064(4) Uani 0.192(4) 1 d PDU A -2
H6S H 0.6440 0.1078 0.6794 0.076 Uiso 0.192(4) 1 calc PR A -2
C7S C 0.7382(13) 0.2721(18) 0.8179(10) 0.084(7) Uani 0.192(4) 1 d PDU A -2
H7S1 H 0.7065 0.3341 0.8535 0.126 Uiso 0.192(4) 1 calc PR A -2
H7S2 H 0.8370 0.2766 0.8177 0.126 Uiso 0.192(4) 1 calc PR A -2
H7S3 H 0.7179 0.2121 0.8631 0.126 Uiso 0.192(4) 1 calc PR A -2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0998 0.0984 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.2496 0.3992 '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
C12 Cr1 C13 89.84(8) . .
C12 Cr1 C13 89.84(8) . 4_565
C13 Cr1 C13 90.07(11) . 4_565
C12 Cr1 C14 93.57(8) . 4_565
C13 Cr1 C14 90.52(8) . 4_565
C13 Cr1 C14 176.54(8) 4_565 4_565
C12 Cr1 C14 93.57(8) . .
C13 Cr1 C14 176.54(8) . .
C13 Cr1 C14 90.52(8) 4_565 .
C14 Cr1 C14 88.70(11) 4_565 .
C12 Cr1 Si1 178.34(8) . .
C13 Cr1 Si1 88.99(6) . .
C13 Cr1 Si1 88.99(6) 4_565 .
C14 Cr1 Si1 87.61(6) 4_565 .
C14 Cr1 Si1 87.61(6) . .
N1 Si1 N1 71.62(9) . 4_565
N1 Si1 Cl1 103.23(6) . .
N1 Si1 Cl1 103.23(6) 4_565 .
N1 Si1 C1 35.86(4) . .
N1 Si1 C1 35.86(4) 4_565 .
Cl1 Si1 C1 108.54(7) . .
N1 Si1 Cr1 124.90(5) . .
N1 Si1 Cr1 124.90(5) 4_565 .
Cl1 Si1 Cr1 118.75(4) . .
C1 Si1 Cr1 132.71(6) . .
C1 N1 C8 130.67(14) . .
C1 N1 Si1 90.97(10) . .
C8 N1 Si1 138.23(11) . .
N1 C1 N1 106.12(18) 4_565 .
N1 C1 C2 126.84(9) 4_565 .
N1 C1 C2 126.85(9) . .
N1 C1 Si1 53.16(9) 4_565 .
N1 C1 Si1 53.16(9) . .
C2 C1 Si1 172.21(16) . .
C3 C2 C7 120.1(2) . .
C3 C2 C1 118.7(2) . .
C7 C2 C1 121.2(2) . .
C4 C3 C2 119.7(2) . .
C3 C4 C5 120.3(3) . .
C6 C5 C4 120.1(2) . .
C5 C6 C7 120.4(2) . .
C6 C7 C2 119.4(2) . .
N1 C8 C10 111.62(15) . .
N1 C8 C9 108.80(15) . .
C10 C8 C9 111.36(18) . .
N1 C8 C11 105.95(14) . .
C10 C8 C11 110.08(16) . .
C9 C8 C11 108.86(16) . .
O1 C12 Cr1 177.6(2) . .
O2 C13 Cr1 178.74(17) . .
O3 C14 Cr1 178.60(17) . .
C6T C1T C2T 118.7(11) . .
C6T C1T C7T 109.5(11) . .
C2T C1T C7T 131.6(13) . .
C1T C2T C3T 120.4(11) . .
C4T C3T C2T 119.1(11) . .
C3T C4T C5T 121.1(11) . .
C6T C5T C4T 119.4(11) . .
C5T C6T C1T 121.1(11) . .
C6S C1S C2S 122.2(13) . .
C6S C1S C7S 126.0(16) . .
C2S C1S C7S 111.7(16) . .
C3S C2S C1S 119.5(14) . .
C4S C3S C2S 119.4(15) . .
C5S C4S C3S 119.8(16) . .
C4S C5S C6S 123.7(16) . .
C1S C6S C5S 115.3(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 C12 1.877(3) .
Cr1 C13 1.885(2) .
Cr1 C13 1.885(2) 4_565
Cr1 C14 1.8901(19) 4_565
Cr1 C14 1.8901(19) .
Cr1 Si1 2.3459(10) .
O1 C12 1.141(3) .
Cl1 Si1 2.1007(11) .
Si1 N1 1.8292(14) .
Si1 N1 1.8293(14) 4_565
Si1 C1 2.285(2) .
N1 C1 1.3390(18) .
N1 C8 1.490(2) .
C1 N1 1.3390(18) 4_565
C1 C2 1.484(3) .
C2 C3 1.386(3) .
C2 C7 1.391(3) .
O2 C13 1.137(2) .
C3 C4 1.377(3) .
O3 C14 1.140(2) .
C4 C5 1.380(4) .
C5 C6 1.372(4) .
C6 C7 1.386(3) .
C8 C10 1.524(3) .
C8 C9 1.524(3) .
C8 C11 1.529(2) .
C1T C6T 1.378(12) .
C1T C2T 1.388(11) .
C1T C7T 1.513(14) .
C2T C3T 1.395(12) .
C3T C4T 1.357(12) .
C4T C5T 1.384(12) .
C5T C6T 1.364(12) .
C1S C6S 1.380(13) .
C1S C2S 1.401(13) .
C1S C7S 1.431(15) .
C2S C3S 1.372(13) .
C3S C4S 1.368(13) .
C4S C5S 1.362(13) .
C5S C6S 1.386(13) .
