#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:15:41 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178620 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/31/4073145.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_4073145
loop_
_publ_author_name
'Conde, Ana'
'Fandos, Rosa'
'Otero, Antonio'
'Rodríguez, Ana'
_publ_section_title
;
 Water-Soluble Organometallic Complexes of Tantalum:  Can Alkyl and
 Aqua Ligands Coexist in Its Coordination Sphere?
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1568
_journal_paper_doi               10.1021/om0701165
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C19 H22 F6 N O8 S2 Ta'
_chemical_formula_sum            'C19 H22 F6 N O8 S2 Ta'
_chemical_formula_weight         751.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 102.196(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6310(5)
_cell_length_b                   15.2770(6)
_cell_length_c                   13.3770(6)
_cell_measurement_reflns_used    4586
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.95
_cell_measurement_theta_min      2.4
_cell_volume                     2523.02(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SHELXTL'
_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      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi 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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14281
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    4.611
_exptl_absorpt_correction_T_max  0.5010
_exptl_absorpt_correction_T_min  0.2540
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.134
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3139
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0855P)²+3.3150P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1196
_reflns_number_gt                2792
_reflns_number_total             3139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0701165si20070206_050506.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4073145
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
O2 O 0.3473(3) 0.1725(3) 0.7873(3) 0.0471(9) Uani 1 1 d DU . .
S1 S 0.2969(3) 0.1301(3) 0.8555(3) 0.0511(12) Uiso 0.50 1 d PD A 1
C5 C 0.1679(12) 0.0995(9) 0.7688(11) 0.069(4) Uiso 0.50 1 d PD A 1
O3 O 0.3388(7) 0.0459(6) 0.8860(7) 0.0435(18) Uiso 0.50 1 d PD A 1
O4 O 0.2688(16) 0.1815(11) 0.9330(14) 0.113(5) Uiso 0.50 1 d PD A 1
F1 F 0.1011(8) 0.0582(7) 0.8183(8) 0.080(3) Uiso 0.50 1 d PD A 1
F2 F 0.1112(9) 0.1727(8) 0.7266(8) 0.079(2) Uiso 0.50 1 d PD A 1
F3 F 0.1874(11) 0.0483(8) 0.6927(10) 0.101(3) Uiso 0.50 1 d PD A 1
S1A S 0.3001(5) 0.1079(5) 0.8621(5) 0.0326(15) Uiso 0.25 1 d PD A 2
C5A C 0.1600(10) 0.1324(8) 0.8171(9) 0.050(3) Uiso 0.50 1 d PD A 2
O3A O 0.3227(13) 0.0192(11) 0.8529(13) 0.040(3) Uiso 0.25 1 d PD A 2
O4A O 0.3204(19) 0.1415(15) 0.9669(14) 0.070(5) Uiso 0.25 1 d PD A 2
F1A F 0.1024(7) 0.0794(6) 0.8623(7) 0.062(2) Uiso 0.50 1 d PD A 2
F2A F 0.1366(13) 0.1130(10) 0.7133(10) 0.124(5) Uiso 0.50 1 d PD A 2
F3A F 0.1393(15) 0.2108(9) 0.8369(13) 0.130(6) Uiso 0.50 1 d PD A 2
S1B S 0.2831(6) 0.0911(5) 0.8125(6) 0.0550(14) Uiso 0.25 1 d P A 3
O3B O 0.328(2) 0.082(2) 0.928(2) 0.092(7) Uiso 0.25 1 d P A 3
O4B O 0.257(3) 0.029(2) 0.737(3) 0.107(9) Uiso 0.25 1 d P A 3
Ta1 Ta 0.5000 0.198321(16) 0.7500 0.03598(13) Uani 1 2 d SU . .
N1 N 0.5000 0.0567(4) 0.7500 0.0400(14) Uani 1 2 d SU . .
O1 O 0.4304(3) 0.1637(3) 0.6132(3) 0.0453(9) Uani 1 1 d U . .
C1 C 0.4516(5) 0.0153(4) 0.6643(6) 0.0551(16) Uani 1 1 d U A .
C2 C 0.4483(7) -0.0755(4) 0.6630(8) 0.076(2) Uani 1 1 d U . .
H2 H 0.4118 -0.1067 0.6043 0.091 Uiso 1 1 calc R A .
C3 C 0.5000 -0.1186(6) 0.7500 0.100(6) Uani 1 2 d SU . .
H3 H 0.5000 -0.1807 0.7500 0.121 Uiso 1 2 calc SR . .
C4 C 0.4047(5) 0.0768(5) 0.5798(6) 0.0601(18) Uani 1 1 d U A .
H4A H 0.4348 0.0642 0.5188 0.072 Uiso 1 1 calc R . .
H4B H 0.3251 0.0694 0.5609 0.072 Uiso 1 1 calc R . .
C10 C 0.434(3) 0.3461(13) 0.781(3) 0.071(9) Uani 0.50 1 d PU . 1
C11 C 0.529(3) 0.336(2) 0.840(2) 0.054(9) Uani 0.50 1 d PU . 1
C12 C 0.6094(17) 0.3342(11) 0.7866(16) 0.049(4) Uani 0.50 1 d PU . 1
C13 C 0.333(2) 0.3554(12) 0.827(3) 0.138(13) Uani 0.50 1 d PU B 1
H13A H 0.3211 0.4173 0.8408 0.207 Uiso 0.50 1 calc PR B 1
H13B H 0.3438 0.3225 0.8917 0.207 Uiso 0.50 1 calc PR B 1
H13C H 0.2696 0.3322 0.7795 0.207 Uiso 0.50 1 calc PR B 1
C14 C 0.564(3) 0.3401(15) 0.9621(14) 0.119(11) Uani 0.50 1 d PU C 1
H14A H 0.5917 0.3985 0.9834 0.179 Uiso 0.50 1 calc PR C 1
H14B H 0.6202 0.2963 0.9860 0.179 Uiso 0.50 1 calc PR C 1
H14C H 0.5007 0.3276 0.9918 0.179 Uiso 0.50 1 calc PR C 1
C15 C 0.7269(14) 0.3332(14) 0.821(2) 0.108(8) Uani 0.50 1 d PU D 1
H15A H 0.7608 0.3212 0.7634 0.163 Uiso 0.50 1 calc PR D 1
H15B H 0.7474 0.2875 0.8733 0.163 Uiso 0.50 1 calc PR D 1
H15C H 0.7514 0.3902 0.8511 0.163 Uiso 0.50 1 calc PR D 1
C16 C 0.438(2) 0.3334(12) 0.8188(16) 0.045(4) Uani 0.50 1 d PU . 2
C17 C 0.560(4) 0.341(3) 0.825(4) 0.083(17) Uani 0.50 1 d PU . 2
C18 C 0.408(3) 0.3387(13) 0.9168(18) 0.130(12) Uani 0.50 1 d PU E 2
H18A H 0.4637 0.3109 0.9691 0.195 Uiso 0.50 1 calc PR E 2
H18B H 0.3386 0.3085 0.9130 0.195 Uiso 0.50 1 calc PR E 2
H18C H 0.4002 0.4003 0.9347 0.195 Uiso 0.50 1 calc PR E 2
C19 C 0.646(3) 0.3514(14) 0.912(2) 0.140(14) Uani 0.50 1 d PU F 2
H19A H 0.6486 0.4124 0.9348 0.209 Uiso 0.50 1 calc PR F 2
H19B H 0.7147 0.3362 0.8930 0.209 Uiso 0.50 1 calc PR F 2
H19C H 0.6342 0.3129 0.9669 0.209 Uiso 0.50 1 calc PR F 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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
S1 O2 S1B 31.7(3) . .
S1 O2 S1A 10.2(3) . .
S1B O2 S1A 25.6(3) . .
S1 O2 Ta1 144.1(3) . .
S1B O2 Ta1 137.4(4) . .
S1A O2 Ta1 137.2(3) . .
O2 S1 O4 116.7(8) . .
O2 S1 O3 114.9(5) . .
O4 S1 O3 115.6(8) . .
O2 S1 C5 99.9(5) . .
O4 S1 C5 106.1(10) . .
O3 S1 C5 100.2(6) . .
F1 C5 F3 109.6(12) . .
F1 C5 F2 104.9(11) . .
F3 C5 F2 108.8(12) . .
F1 C5 S1 111.9(10) . .
F3 C5 S1 110.1(11) . .
F2 C5 S1 111.3(10) . .
O3A S1A O4A 115.3(11) . .
O3A S1A O2 115.5(8) . .
O4A S1A O2 111.6(10) . .
O3A S1A C5A 112.3(9) . .
O4A S1A C5A 102.2(11) . .
O2 S1A C5A 97.7(5) . .
F3A C5A F1A 109.1(12) . .
F3A C5A F2A 113.6(12) . .
F1A C5A F2A 107.8(10) . .
F3A C5A S1A 111.2(11) . .
F1A C5A S1A 108.7(8) . .
F2A C5A S1A 106.2(10) . .
O4B S1B O3B 131(2) . .
O4B S1B O2 116.4(14) . .
O3B S1B O2 101.2(12) . .
O1 Ta1 O1 148.2(3) . 2_656
O1 Ta1 O2 85.29(18) . .
O1 Ta1 O2 88.89(17) 2_656 .
O1 Ta1 O2 88.89(17) . 2_656
O1 Ta1 O2 85.29(17) 2_656 2_656
O2 Ta1 O2 158.6(2) . 2_656
O1 Ta1 N1 74.10(13) . .
O1 Ta1 N1 74.10(13) 2_656 .
O2 Ta1 N1 79.31(12) . .
O2 Ta1 N1 79.31(12) 2_656 .
O1 Ta1 C11 134.5(9) . .
O1 Ta1 C11 77.1(9) 2_656 .
O2 Ta1 C11 95.4(7) . .
O2 Ta1 C11 103.3(7) 2_656 .
N1 Ta1 C11 150.8(9) . .
O1 Ta1 C11 77.1(9) . 2_656
O1 Ta1 C11 134.5(9) 2_656 2_656
O2 Ta1 C11 103.3(7) . 2_656
O2 Ta1 C11 95.4(7) 2_656 2_656
N1 Ta1 C11 150.8(9) . 2_656
C11 Ta1 C11 58.4(18) . 2_656
O1 Ta1 C17 132.2(11) . .
O1 Ta1 C17 79.4(10) 2_656 .
O2 Ta1 C17 106.5(14) . .
O2 Ta1 C17 92.6(13) 2_656 .
N1 Ta1 C17 152.8(9) . .
C11 Ta1 C17 11.3(15) . .
C11 Ta1 C17 55.1(7) 2_656 .
O1 Ta1 C17 79.4(10) . 2_656
O1 Ta1 C17 132.2(11) 2_656 2_656
O2 Ta1 C17 92.6(13) . 2_656
O2 Ta1 C17 106.5(14) 2_656 2_656
N1 Ta1 C17 152.8(9) . 2_656
C11 Ta1 C17 55.1(7) . 2_656
C11 Ta1 C17 11.3(15) 2_656 2_656
C17 Ta1 C17 54.4(19) . 2_656
O1 Ta1 C16 118.0(6) . .
O1 Ta1 C16 89.5(6) 2_656 .
O2 Ta1 C16 72.1(5) . .
O2 Ta1 C16 128.3(5) 2_656 .
N1 Ta1 C16 147.3(4) . .
C11 Ta1 C16 26.5(10) . .
C11 Ta1 C16 55.0(9) 2_656 .
C17 Ta1 C16 36.1(12) . .
C17 Ta1 C16 46.4(12) 2_656 .
O1 Ta1 C16 89.5(6) . 2_656
O1 Ta1 C16 118.0(6) 2_656 2_656
O2 Ta1 C16 128.3(5) . 2_656
O2 Ta1 C16 72.1(5) 2_656 2_656
N1 Ta1 C16 147.3(4) . 2_656
C11 Ta1 C16 55.0(9) . 2_656
C11 Ta1 C16 26.5(10) 2_656 2_656
C17 Ta1 C16 46.4(12) . 2_656
C17 Ta1 C16 36.1(12) 2_656 2_656
C16 Ta1 C16 65.4(7) . 2_656
O1 Ta1 C10 107.8(10) . .
O1 Ta1 C10 101.2(9) 2_656 .
O2 Ta1 C10 77.2(6) . .
O2 Ta1 C10 124.1(7) 2_656 .
N1 Ta1 C10 156.2(5) . .
C11 Ta1 C10 30.6(12) . .
C11 Ta1 C10 42.6(10) 2_656 .
C17 Ta1 C10 37.2(11) . .
C17 Ta1 C10 33.9(11) 2_656 .
C16 Ta1 C10 12.6(5) . .
C16 Ta1 C10 55.7(6) 2_656 .
C1 N1 C1 123.6(8) . 2_656
C1 N1 Ta1 118.2(4) . .
C1 N1 Ta1 118.2(4) 2_656 .
C4 O1 Ta1 125.7(4) . .
N1 C1 C2 119.3(8) . .
N1 C1 C4 112.8(5) . .
C2 C1 C4 127.9(7) . .
C1 C2 C3 117.4(8) . .
C2 C3 C2 122.9(9) . 2_656
O1 C4 C1 108.9(5) . .
C12 C10 C11 145(3) 2_656 .
C12 C10 C13 92(4) 2_656 .
C11 C10 C13 120(3) . .
C12 C10 C11 49.5(16) 2_656 2_656
C11 C10 C11 99(2) . 2_656
C13 C10 C11 141(4) . 2_656
C12 C10 C10 88.9(19) 2_656 2_656
C11 C10 C10 61(2) . 2_656
C13 C10 C10 174.7(10) . 2_656
C11 C10 C10 39.5(15) 2_656 2_656
C12 C10 Ta1 79.7(15) 2_656 .
C11 C10 Ta1 72.5(16) . .
C13 C10 Ta1 119.1(13) . .
C11 C10 Ta1 67.2(12) 2_656 .
C10 C10 Ta1 66.2(5) 2_656 .
C10 C11 C12 112(3) . .
C10 C11 C14 130(3) . .
C12 C11 C14 117(3) . .
C10 C11 C10 80(2) . 2_656
C12 C11 C10 32.7(18) . 2_656
C14 C11 C10 149(3) . 2_656
C10 C11 Ta1 76.9(15) . .
C12 C11 Ta1 76.7(15) . .
C14 C11 Ta1 121(2) . .
C10 C11 Ta1 70.2(11) 2_656 .
C10 C12 C11 98(3) 2_656 .
C10 C12 C15 130(3) 2_656 .
C11 C12 C15 131(3) . .
C10 C12 Ta1 77.7(16) 2_656 .
C11 C12 Ta1 71.1(15) . .
C15 C12 Ta1 122.7(13) . .
C18 C16 C17 114(3) . .
C18 C16 C17 164(3) . 2_656
C17 C16 C17 80(2) . 2_656
C18 C16 Ta1 123.7(14) . .
C17 C16 Ta1 71.8(17) . .
C17 C16 Ta1 66.7(12) 2_656 .
C19 C17 C16 130(5) . .
C19 C17 C16 130(4) . 2_656
C16 C17 C16 100(2) . 2_656
C19 C17 Ta1 123(2) . .
C16 C17 Ta1 72.1(14) . .
C16 C17 Ta1 66.9(13) 2_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O2 S1 1.379(6) .
O2 S1B 1.560(9) .
O2 S1A 1.607(8) .
O2 Ta1 2.129(4) .
S1 O4 1.405(16) .
S1 O3 1.417(9) .
S1 C5 1.849(17) .
C5 F1 1.336(15) .
C5 F3 1.347(15) .
C5 F2 1.384(15) .
S1A O3A 1.397(17) .
S1A O4A 1.463(19) .
S1A C5A 1.785(14) .
C5A F3A 1.266(14) .
C5A F1A 1.318(13) .
C5A F2A 1.389(15) .
S1B O4B 1.36(4) .
S1B O3B 1.54(3) .
Ta1 O1 1.930(4) .
Ta1 O1 1.930(4) 2_656
Ta1 O2 2.129(4) 2_656
Ta1 N1 2.164(6) .
Ta1 C11 2.42(3) .
Ta1 C11 2.42(3) 2_656
Ta1 C17 2.45(3) .
Ta1 C17 2.45(3) 2_656
Ta1 C16 2.452(19) .
Ta1 C16 2.452(19) 2_656
Ta1 C10 2.47(2) .
N1 C1 1.339(8) .
N1 C1 1.339(8) 2_656
O1 C4 1.416(8) .
C1 C2 1.388(9) .
C1 C4 1.493(11) .
C2 C3 1.376(11) .
C3 C2 1.376(11) 2_656
C10 C12 0.97(4) 2_656
C10 C11 1.29(5) .
C10 C13 1.55(3) .
C10 C11 1.77(4) 2_656
C10 C10 2.00(5) 2_656
C11 C12 1.36(4) .
C11 C14 1.60(4) .
C11 C10 1.77(4) 2_656
C12 C10 0.97(4) 2_656
C12 C15 1.46(3) .
C16 C18 1.45(2) .
C16 C17 1.52(5) .
C16 C17 1.93(5) 2_656
C17 C19 1.42(4) .
C17 C16 1.93(5) 2_656
