#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178647 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/58/4075888.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_4075888
loop_
_publ_author_name
'Braband, Henrik'
'Abram, Ulrich'
_publ_section_title
;
 Nitridotechnetium(V) Complexes with N-Heterocyclic Carbenes and
 Unexpected (OSiMe2OSiMe2O)2-Coligands
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3362
_journal_paper_doi               10.1021/om050245q
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C22 H44 N5 O3 Si2 Tc'
_chemical_formula_sum            'C22 H44 N5 O3 Si2 Tc'
_chemical_formula_weight         580.80
_chemical_name_systematic
;
Bis{(1,3-Diethyl-4,5-dimethyl)imidazolylyliden}-
(1,1,3,3-tetramethyldisiloxane-1,3-diolato)nitridotechnetium(V)

;
_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                 95.44(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.057(2)
_cell_length_b                   18.112(3)
_cell_length_c                   15.597(3)
_cell_measurement_reflns_used    984
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.421
_cell_measurement_theta_min      3.359
_cell_volume                     2828.2(9)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        SAINT
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart'
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34332
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '10 sec / frame'
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  none
_exptl_absorpt_correction_T_min  none
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          .58
_exptl_crystal_size_mid          .43
_exptl_crystal_size_min          .43
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         8631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0296
_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)+(0.0338P)²+4.2741P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                7632
_reflns_number_total             8631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050245qsi20050401_053408.cif
_cod_data_source_block           tcnc2si
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4075888
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
Tc Tc 0.484801(14) 0.067047(7) 0.700271(9) 0.01339(4) Uani 1 1 d .
N1 N 0.35201(16) 0.03331(9) 0.64757(10) 0.0191(3) Uani 1 1 d .
C1 C 0.50308(17) -0.01013(9) 0.80348(11) 0.0148(3) Uani 1 1 d .
N2 N 0.42434(16) -0.06785(8) 0.82235(10) 0.0165(3) Uani 1 1 d .
C3 C 0.47023(19) -0.10084(10) 0.90127(12) 0.0183(3) Uani 1 1 d .
C4 C 0.57987(19) -0.06282(10) 0.93222(12) 0.0184(3) Uani 1 1 d .
N5 N 0.59881(15) -0.00757(8) 0.87157(10) 0.0162(3) Uani 1 1 d .
C6 C 0.29752(19) -0.08934(10) 0.77554(12) 0.0199(3) Uani 1 1 d .
H6A H 0.2878 -0.1426 0.7782 0.024 Uiso 1 1 calc R
H6B H 0.2980 -0.0755 0.7155 0.024 Uiso 1 1 calc R
C7 C 0.1791(2) -0.05286(12) 0.81257(14) 0.0260(4) Uani 1 1 d .
H7A H 0.0978 -0.0682 0.7803 0.039 Uiso 1 1 calc R
H7B H 0.1875 -0.0002 0.8091 0.039 Uiso 1 1 calc R
H7C H 0.1773 -0.0672 0.8717 0.039 Uiso 1 1 calc R
C8 C 0.70785(19) 0.04591(11) 0.88111(13) 0.0209(3) Uani 1 1 d .
H8A H 0.7133 0.0665 0.9387 0.025 Uiso 1 1 calc R
H8B H 0.6883 0.0860 0.8406 0.025 Uiso 1 1 calc R
C9 C 0.8422(2) 0.01232(14) 0.86581(16) 0.0308(5) Uani 1 1 d .
H9A H 0.9101 0.0496 0.8729 0.046 Uiso 1 1 calc R
H9B H 0.8381 -0.0072 0.8084 0.046 Uiso 1 1 calc R
H9C H 0.8631 -0.0267 0.9065 0.046 Uiso 1 1 calc R
C10 C 0.4059(2) -0.16709(11) 0.93639(13) 0.0247(4) Uani 1 1 d .
H10A H 0.3288 -0.1806 0.8986 0.037 Uiso 1 1 calc R
H10B H 0.3792 -0.1559 0.9924 0.037 Uiso 1 1 calc R
H10C H 0.4682 -0.2074 0.9407 0.037 Uiso 1 1 calc R
C11 C 0.6671(2) -0.07216(12) 1.01435(13) 0.0251(4) Uani 1 1 d .
H11A H 0.7374 -0.0361 1.0172 0.038 Uiso 1 1 calc R
H11B H 0.7051 -0.1208 1.0165 0.038 Uiso 1 1 calc R
H11C H 0.6150 -0.0655 1.0622 0.038 Uiso 1 1 calc R
C21 C 0.63755(17) 0.01302(10) 0.63768(11) 0.0158(3) Uani 1 1 d .
N22 N 0.76838(15) 0.03450(9) 0.64246(10) 0.0175(3) Uani 1 1 d .
C23 C 0.84681(19) -0.01719(11) 0.60339(12) 0.0196(3) Uani 1 1 d .
C24 C 0.76259(19) -0.07074(10) 0.57112(12) 0.0189(3) Uani 1 1 d .
N25 N 0.63506(16) -0.05157(8) 0.59268(10) 0.0168(3) Uani 1 1 d .
C26 C 0.8213(2) 0.10617(11) 0.67268(13) 0.0218(3) Uani 1 1 d .
H26A H 0.9059 0.0989 0.7069 0.026 Uiso 1 1 calc R
H26B H 0.7598 0.1288 0.7092 0.026 Uiso 1 1 calc R
C27 C 0.8416(2) 0.15751(12) 0.59799(15) 0.0287(4) Uani 1 1 d .
H27A H 0.8764 0.2039 0.6199 0.043 Uiso 1 1 calc R
H27B H 0.7576 0.1655 0.5646 0.043 Uiso 1 1 calc R
H27C H 0.9035 0.1356 0.5623 0.043 Uiso 1 1 calc R
C28 C 0.51772(19) -0.09856(10) 0.57156(12) 0.0197(3) Uani 1 1 d .
H28A H 0.5189 -0.1172 0.5133 0.024 Uiso 1 1 calc R
H28B H 0.4373 -0.0693 0.5738 0.024 Uiso 1 1 calc R
C29 C 0.5147(2) -0.16339(11) 0.63367(14) 0.0254(4) Uani 1 1 d .
H29A H 0.4368 -0.1929 0.6181 0.038 Uiso 1 1 calc R
H29B H 0.5120 -0.1451 0.6913 0.038 Uiso 1 1 calc R
H29C H 0.5933 -0.1930 0.6307 0.038 Uiso 1 1 calc R
C30 C 0.9956(2) -0.01105(13) 0.60674(14) 0.0267(4) Uani 1 1 d .
H30A H 1.0240 0.0345 0.6342 0.040 Uiso 1 1 calc R
H30B H 1.0223 -0.0120 0.5493 0.040 Uiso 1 1 calc R
H30C H 1.0360 -0.0517 0.6389 0.040 Uiso 1 1 calc R
C31 C 0.7886(2) -0.13854(11) 0.52072(13) 0.0240(4) Uani 1 1 d .
H31A H 0.7066 -0.1652 0.5078 0.036 Uiso 1 1 calc R
H31B H 0.8518 -0.1693 0.5540 0.036 Uiso 1 1 calc R
H31C H 0.8240 -0.1247 0.4680 0.036 Uiso 1 1 calc R
O1 O 0.53870(14) 0.16055(7) 0.63680(9) 0.0192(2) Uani 1 1 d .
Si1 Si 0.51214(5) 0.24650(3) 0.65347(3) 0.01809(10) Uani 1 1 d .
O3 O 0.37376(14) 0.25844(7) 0.70126(9) 0.0205(3) Uani 1 1 d .
Si2 Si 0.34082(5) 0.20745(3) 0.78471(3) 0.01605(9) Uani 1 1 d .
O2 O 0.44288(14) 0.13908(7) 0.79657(8) 0.0181(2) Uani 1 1 d .
C46 C 0.6518(2) 0.28996(13) 0.72394(17) 0.0335(5) Uani 1 1 d .
H46A H 0.6322 0.3412 0.7323 0.050 Uiso 1 1 calc R
H46B H 0.7334 0.2857 0.6970 0.050 Uiso 1 1 calc R
H46C H 0.6615 0.2653 0.7787 0.050 Uiso 1 1 calc R
C47 C 0.4913(2) 0.29822(11) 0.54910(14) 0.0273(4) Uani 1 1 d .
H47A H 0.4755 0.3495 0.5602 0.041 Uiso 1 1 calc R
H47B H 0.4167 0.2784 0.5134 0.041 Uiso 1 1 calc R
H47C H 0.5709 0.2934 0.5201 0.041 Uiso 1 1 calc R
C48 C 0.3616(2) 0.26781(11) 0.88223(13) 0.0234(4) Uani 1 1 d .
H48A H 0.3006 0.3086 0.8750 0.035 Uiso 1 1 calc R
H48B H 0.4515 0.2861 0.8899 0.035 Uiso 1 1 calc R
H48C H 0.3432 0.2398 0.9320 0.035 Uiso 1 1 calc R
C49 C 0.1633(2) 0.17672(12) 0.76412(14) 0.0256(4) Uani 1 1 d .
H49A H 0.1061 0.2192 0.7574 0.038 Uiso 1 1 calc R
H49B H 0.1396 0.1477 0.8119 0.038 Uiso 1 1 calc R
H49C H 0.1530 0.1475 0.7125 0.038 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'
Tc Tc -1.4390 0.7593 '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'
Si Si 0.0817 0.0704 '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
N1 Tc O1 107.94(7)
N1 Tc O2 113.10(7)
O1 Tc O2 84.91(5)
N1 Tc C1 98.28(7)
O1 Tc C1 153.67(6)
O2 Tc C1 82.74(6)
N1 Tc C21 100.92(8)
O1 Tc C21 85.61(6)
O2 Tc C21 145.96(6)
C1 Tc C21 91.75(6)
N2 C1 N5 103.88(14)
N2 C1 Tc 131.19(13)
N5 C1 Tc 124.79(12)
C1 N2 C3 111.50(15)
C1 N2 C6 126.52(15)
C3 N2 C6 121.51(15)
C4 C3 N2 106.58(15)
C4 C3 C10 130.33(17)
N2 C3 C10 123.04(17)
C3 C4 N5 106.34(16)
C3 C4 C11 130.02(17)
N5 C4 C11 123.62(17)
C1 N5 C4 111.70(15)
C1 N5 C8 124.71(15)
C4 N5 C8 123.59(15)
N2 C6 C7 111.84(16)
N5 C8 C9 112.85(17)
N25 C21 N22 104.05(15)
N25 C21 Tc 130.55(13)
N22 C21 Tc 125.12(13)
C21 N22 C23 111.40(15)
C21 N22 C26 126.05(16)
C23 N22 C26 122.02(16)
C24 C23 N22 106.41(16)
C24 C23 C30 130.92(18)
N22 C23 C30 122.53(18)
C23 C24 N25 106.76(16)
C23 C24 C31 130.56(18)
N25 C24 C31 122.68(17)
C21 N25 C24 111.34(15)
C21 N25 C28 126.06(15)
C24 N25 C28 122.55(15)
N22 C26 C27 111.53(17)
N25 C28 C29 111.61(16)
Si1 O1 Tc 131.62(8)
O1 Si1 O3 111.09(7)
O1 Si1 C47 110.55(9)
O3 Si1 C47 107.25(9)
O1 Si1 C46 112.07(10)
O3 Si1 C46 107.27(10)
C47 Si1 C46 108.42(11)
Si1 O3 Si2 121.41(8)
O2 Si2 O3 110.31(7)
O2 Si2 C49 112.30(9)
O3 Si2 C49 106.88(9)
O2 Si2 C48 109.65(8)
O3 Si2 C48 107.37(9)
C49 Si2 C48 110.20(10)
Si2 O2 Tc 125.15(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Tc N1 1.6199(16)
Tc O1 2.0600(13)
Tc O2 2.0629(13)
Tc C1 2.1268(17)
Tc C21 2.1342(18)
C1 N2 1.360(2)
C1 N5 1.365(2)
N2 C3 1.406(2)
N2 C6 1.461(2)
C3 C4 1.350(3)
C3 C10 1.492(3)
C4 N5 1.402(2)
C4 C11 1.492(3)
N5 C8 1.460(2)
C6 C7 1.523(3)
C8 C9 1.521(3)
C21 N25 1.363(2)
C21 N22 1.367(2)
N22 C23 1.400(2)
N22 C26 1.464(2)
C23 C24 1.353(3)
C23 C30 1.497(3)
C24 N25 1.400(2)
C24 C31 1.494(3)
N25 C28 1.467(2)
C26 C27 1.519(3)
C28 C29 1.524(3)
O1 Si1 1.6049(14)
Si1 O3 1.6540(15)
Si1 C47 1.873(2)
Si1 C46 1.873(2)
O3 Si2 1.6549(14)
Si2 O2 1.6078(14)
Si2 C49 1.868(2)
Si2 C48 1.869(2)
