#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:21:19 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180258 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/44/7114474.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_7114474
loop_
_publ_author_name
'Tipparaju, Suresh Kumar'
'Mandal, Sunil K.'
'Sur, Surojit'
'Puranik, Vedavati G.'
'Sarkar, Amitabha'
_publ_section_title
;
 Cleavage of Si???Ar bond vs Si???Me bond: a remarkable counterion effect
 on reactivityElectronic supplementary information (ESI) available:
 spectroscopic data and experimental section. See
 http://www.rsc.org/suppdata/cc/b2/b205373j/
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1924
_journal_paper_doi               10.1039/b205373j
_journal_year                    2002
_chemical_formula_moiety         'C23 H22 Cr O4 Si'
_chemical_formula_sum            'C23 H22 Cr O4 Si'
_chemical_formula_weight         442.50
_chemical_name_common            'Chromoum Complex'
_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                90.000(11)
_cell_angle_beta                 107.161(11)
_cell_angle_gamma                90.000(9)
_cell_formula_units_Z            4
_cell_length_a                   12.4880(16)
_cell_length_b                   9.1030(9)
_cell_length_c                   20.682(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      9
_cell_volume                     2246.4(5)
_computing_cell_refinement       'Enraf-Nonius MACH-3'
_computing_data_collection       'Enraf-Nonius MACH-3'
_computing_data_reduction        MACH-3
_computing_molecular_graphics    ORTEP
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  MACH-3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            3546
_diffrn_reflns_theta_full        24.91
_diffrn_reflns_theta_max         24.91
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        <4%
_diffrn_standards_interval_count '1 Hr'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.587
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0091(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0341
_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)+(0.0412P)²+0.9471P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                3045
_reflns_number_total             3546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205373j.txt
_cod_data_source_block           C23H22CrO4Si
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7114474
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
Cr Cr 0.35549(3) 0.58453(4) 0.117021(18) 0.03667(13) Uani 1 1 d .
Si Si 0.17129(5) 0.91834(8) 0.08372(4) 0.04304(18) Uani 1 1 d .
O1 O 0.13562(17) 0.4800(2) 0.02430(11) 0.0749(6) Uani 1 1 d .
O2 O 0.2964(2) 0.4146(3) 0.22534(12) 0.0917(8) Uani 1 1 d .
O3 O 0.46223(18) 0.3131(2) 0.08315(11) 0.0732(6) Uani 1 1 d .
O4 O 0.17373(12) 0.90283(18) 0.00419(8) 0.0431(4) Uani 1 1 d .
C1 C 0.2193(2) 0.5238(3) 0.05831(14) 0.0495(6) Uani 1 1 d .
C2 C 0.3185(2) 0.4801(3) 0.18303(14) 0.0555(7) Uani 1 1 d .
C3 C 0.4198(2) 0.4178(3) 0.09582(13) 0.0465(6) Uani 1 1 d .
C4 C 0.4820(2) 0.7167(3) 0.19213(14) 0.0526(7) Uani 1 1 d .
H4 H 0.5259 0.6913 0.2354 0.063 Uiso 1 1 calc R
C5 C 0.3760(2) 0.7809(3) 0.18246(13) 0.0478(6) Uani 1 1 d .
H5 H 0.3497 0.7957 0.2196 0.057 Uiso 1 1 calc R
C6 C 0.30922(19) 0.8230(3) 0.11793(12) 0.0409(6) Uani 1 1 d .
C7 C 0.35169(18) 0.7976(2) 0.06152(12) 0.0382(5) Uani 1 1 d .
C8 C 0.45634(19) 0.7317(3) 0.07070(13) 0.0457(6) Uani 1 1 d .
H8 H 0.4830 0.7146 0.0339 0.055 Uiso 1 1 calc R
C9 C 0.5209(2) 0.6914(3) 0.13661(14) 0.0519(7) Uani 1 1 d .
H9 H 0.5905 0.6473 0.1430 0.062 Uiso 1 1 calc R
C10 C 0.27781(18) 0.8584(3) -0.00604(12) 0.0402(5) Uani 1 1 d .
C11 C 0.2563(2) 0.7483(3) -0.06270(12) 0.0434(6) Uani 1 1 d .
H11 H 0.3184 0.7122 -0.0737 0.052 Uiso 1 1 calc R
C12 C 0.1577(2) 0.6988(3) -0.09802(12) 0.0469(6) Uani 1 1 d .
H12 H 0.0963 0.7335 -0.0858 0.056 Uiso 1 1 calc R
C13 C 0.1338(2) 0.5941(3) -0.15495(12) 0.0499(6) Uani 1 1 d .
C14 C 0.0310(3) 0.5217(3) -0.17438(15) 0.0640(8) Uani 1 1 d .
H14 H -0.0212 0.5393 -0.1512 0.077 Uiso 1 1 calc R
C15 C 0.0058(4) 0.4242(4) -0.22767(19) 0.0870(12) Uani 1 1 d .
H15 H -0.0630 0.3764 -0.2401 0.104 Uiso 1 1 calc R
C16 C 0.0814(5) 0.3971(4) -0.26250(19) 0.1003(15) Uani 1 1 d .
H16 H 0.0637 0.3315 -0.2986 0.120 Uiso 1 1 calc R
C17 C 0.1835(4) 0.4667(4) -0.24418(17) 0.0907(12) Uani 1 1 d .
H17 H 0.2352 0.4473 -0.2675 0.109 Uiso 1 1 calc R
C18 C 0.2095(3) 0.5659(3) -0.19101(15) 0.0654(8) Uani 1 1 d .
H18 H 0.2782 0.6141 -0.1793 0.078 Uiso 1 1 calc R
C19 C 0.3371(2) 0.9962(3) -0.02342(14) 0.0497(6) Uani 1 1 d .
H19A H 0.3606 1.0585 0.0163 0.060 Uiso 1 1 calc R
H19B H 0.4040 0.9652 -0.0344 0.060 Uiso 1 1 calc R
C20 C 0.2657(3) 1.0842(4) -0.08098(16) 0.0647(8) Uani 1 1 d .
H20 H 0.2359 1.0349 -0.1217 0.078 Uiso 1 1 calc R
C21 C 0.2415(3) 1.2198(4) -0.0801(2) 0.0805(10) Uani 1 1 d .
H21A H 0.2692 1.2742 -0.0407 0.097 Uiso 1 1 calc R
H21B H 0.1960 1.2645 -0.1190 0.097 Uiso 1 1 calc R
C22 C 0.0458(2) 0.8293(4) 0.09437(16) 0.0680(8) Uani 1 1 d .
H22A H -0.0192 0.8860 0.0717 0.102 Uiso 1 1 calc R
H22B H 0.0521 0.8228 0.1417 0.102 Uiso 1 1 calc R
H22C H 0.0389 0.7323 0.0753 0.102 Uiso 1 1 calc R
C23 C 0.1796(3) 1.1130(3) 0.11143(17) 0.0717(9) Uani 1 1 d .
H23A H 0.2459 1.1572 0.1056 0.108 Uiso 1 1 calc R
H23B H 0.1823 1.1173 0.1583 0.108 Uiso 1 1 calc R
H23C H 0.1147 1.1651 0.0847 0.108 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
Cr Cr 0.3209 0.6236 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C3 Cr C2 88.45(12)
C3 Cr C1 88.75(11)
C2 Cr C1 87.08(12)
C3 Cr C9 87.51(11)
C2 Cr C9 121.32(11)
C1 Cr C9 151.22(11)
C3 Cr C5 146.88(10)
C2 Cr C5 88.43(11)
C1 Cr C5 123.99(11)
C9 Cr C5 66.34(10)
C3 Cr C4 110.25(11)
C2 Cr C4 92.52(11)
C1 Cr C4 160.98(11)
C9 Cr C4 36.66(10)
C5 Cr C4 37.04(10)
C3 Cr C8 92.97(10)
C2 Cr C8 158.04(11)
C1 Cr C8 114.86(11)
C9 Cr C8 37.02(9)
C5 Cr C8 78.46(10)
C4 Cr C8 66.44(10)
C3 Cr C7 122.57(10)
C2 Cr C7 148.98(11)
C1 Cr C7 92.61(10)
C9 Cr C7 65.89(9)
C5 Cr C7 66.17(9)
C4 Cr C7 78.03(9)
C8 Cr C7 36.35(8)
C3 Cr C6 159.25(10)
C2 Cr C6 111.91(11)
C1 Cr C6 96.01(10)
C9 Cr C6 78.60(9)
C5 Cr C6 36.66(9)
C4 Cr C6 66.52(9)
C8 Cr C6 66.69(9)
C7 Cr C6 37.25(8)
O4 Si C22 110.33(12)
O4 Si C23 111.81(12)
C22 Si C23 110.90(15)
O4 Si C6 92.94(9)
C22 Si C6 118.23(13)
C23 Si C6 111.40(13)
C10 O4 Si 116.88(14)
O1 C1 Cr 176.3(2)
O2 C2 Cr 179.1(3)
O3 C3 Cr 178.8(3)
C9 C4 C5 119.7(2)
C9 C4 Cr 71.46(14)
C5 C4 Cr 71.29(14)
C6 C5 C4 121.3(2)
C6 C5 Cr 73.11(14)
C4 C5 Cr 71.67(14)
C5 C6 C7 118.1(2)
C5 C6 Si 135.19(19)
C7 C6 Si 106.67(16)
C5 C6 Cr 70.23(14)
C7 C6 Cr 71.36(13)
Si C6 Cr 130.92(12)
C8 C7 C6 120.9(2)
C8 C7 C10 124.4(2)
C6 C7 C10 114.5(2)
C8 C7 Cr 71.47(14)
C6 C7 Cr 71.39(13)
C10 C7 Cr 133.91(16)
C7 C8 C9 119.2(2)
C7 C8 Cr 72.18(13)
C9 C8 Cr 70.42(14)
C4 C9 C8 120.9(2)
C4 C9 Cr 71.88(15)
C8 C9 Cr 72.57(14)
O4 C10 C11 109.94(18)
O4 C10 C7 107.17(18)
C11 C10 C7 113.0(2)
O4 C10 C19 108.72(19)
C11 C10 C19 110.2(2)
C7 C10 C19 107.63(19)
C12 C11 C10 125.8(2)
C11 C12 C13 127.0(2)
C18 C13 C14 118.2(3)
C18 C13 C12 122.5(3)
C14 C13 C12 119.2(3)
C15 C14 C13 120.6(3)
C16 C15 C14 120.5(4)
C15 C16 C17 120.0(4)
C16 C17 C18 120.1(4)
C17 C18 C13 120.6(3)
C20 C19 C10 113.9(2)
C21 C20 C19 126.8(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cr C3 1.830(3)
Cr C2 1.831(3)
Cr C1 1.858(3)
Cr C9 2.210(2)
Cr C5 2.211(2)
Cr C4 2.216(2)
Cr C8 2.238(2)
Cr C7 2.247(2)
Cr C6 2.248(2)
Si O4 1.6601(17)
Si C22 1.834(3)
Si C23 1.856(3)
Si C6 1.871(2)
O1 C1 1.146(3)
O2 C2 1.157(3)
O3 C3 1.158(3)
O4 C10 1.435(3)
C4 C9 1.392(4)
C4 C5 1.406(4)
C5 C6 1.403(3)
C6 C7 1.436(3)
C7 C8 1.399(3)
C7 C10 1.533(3)
C8 C9 1.412(4)
C10 C11 1.504(3)
C10 C19 1.552(3)
C11 C12 1.312(3)
C12 C13 1.475(4)
C13 C18 1.390(4)
C13 C14 1.393(4)
C14 C15 1.377(5)
C15 C16 1.368(6)
C16 C17 1.373(6)
C17 C18 1.385(4)
C19 C20 1.493(4)
C20 C21 1.272(4)
