#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:15:36 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178642 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/53/4075368.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_4075368
loop_
_publ_author_name
'Bo, Carles'
'Fandos, Rosa'
'Feliz, Marta'
'Hernández, Carolina'
'Otero, Antonio'
'Rodríguez, Ana'
'Ruiz, María José'
'Pastor, César'
_publ_section_title
;
 facversusmerCoordination for a Tridentate Diethylene Glyclolate Ligand in
 Tantalum Complexes:  A Combined Experimental and Theoretical Study
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3336
_journal_paper_doi               10.1021/om060254e
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C14 H23 Cl2 O3 Ta'
_chemical_formula_weight         491.17
_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                90.00
_cell_angle_beta                 105.13(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.060(2)
_cell_length_b                   12.4100(10)
_cell_length_c                   13.713(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     1652.6(7)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XCAD4 (Harms, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       'ω/2θ 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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4101
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         2.25
_diffrn_standards_interval_time  90
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.978
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0233P)²+1.4980P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0564
_reflns_number_gt                2522
_reflns_number_total             3946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060254esi20060321_010937.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4075368
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
Ta1 Ta 0.785464(14) 0.250298(17) 0.491913(11) 0.02872(5) Uani 1 1 d .
Cl1 Cl 0.78406(13) 0.08550(10) 0.59179(10) 0.0469(3) Uani 1 1 d .
Cl2 Cl 0.85670(15) 0.35716(11) 0.36088(10) 0.0526(3) Uani 1 1 d .
O1 O 0.6757(3) 0.1681(3) 0.3796(2) 0.0412(7) Uani 1 1 d .
O2 O 0.9292(3) 0.1406(2) 0.4444(2) 0.0386(7) Uani 1 1 d .
O3 O 0.9655(3) 0.2804(2) 0.5803(2) 0.0400(8) Uani 1 1 d .
C1 C 0.7265(6) 0.0806(5) 0.3347(4) 0.0546(14) Uani 1 1 d .
H1A H 0.6770 0.0752 0.2640 0.066 Uiso 1 1 calc .
H1B H 0.7131 0.0140 0.3680 0.066 Uiso 1 1 calc .
C2 C 0.8787(5) 0.0978(5) 0.3443(4) 0.0507(13) Uani 1 1 d .
H2A H 0.9239 0.0304 0.3370 0.061 Uiso 1 1 calc .
H2B H 0.8927 0.1484 0.2940 0.061 Uiso 1 1 calc .
C3 C 1.0718(5) 0.1733(4) 0.4778(4) 0.0486(12) Uani 1 1 d .
H3A H 1.0928 0.2285 0.4340 0.058 Uiso 1 1 calc .
H3B H 1.1330 0.1125 0.4797 0.058 Uiso 1 1 calc .
C4 C 1.0834(5) 0.2168(4) 0.5824(4) 0.0462(12) Uani 1 1 d .
H4A H 1.0895 0.1577 0.6296 0.055 Uiso 1 1 calc .
H4B H 1.1660 0.2602 0.6043 0.055 Uiso 1 1 calc .
C5 C 0.6498(5) 0.3010(4) 0.6129(3) 0.0424(11) Uani 1 1 d .
C6 C 0.7357(5) 0.3880(4) 0.6107(4) 0.0450(12) Uani 1 1 d .
C7 C 0.6987(5) 0.4320(4) 0.5129(4) 0.0430(11) Uani 1 1 d .
C8 C 0.5857(5) 0.3685(4) 0.4532(3) 0.0401(11) Uani 1 1 d .
C9 C 0.5568(4) 0.2877(4) 0.5159(4) 0.0407(11) Uani 1 1 d .
C10 C 0.6434(7) 0.2437(5) 0.7079(4) 0.0735(19) Uani 1 1 d .
H10A H 0.7346 0.2230 0.7448 0.110 Uiso 1 1 calc R
H10B H 0.5869 0.1807 0.6910 0.110 Uiso 1 1 calc R
H10C H 0.6047 0.2909 0.7487 0.110 Uiso 1 1 calc R
C11 C 0.8455(6) 0.4323(5) 0.6983(4) 0.0718(19) Uani 1 1 d .
H11A H 0.8032 0.4742 0.7409 0.108 Uiso 1 1 calc R
H11B H 0.9070 0.4771 0.6733 0.108 Uiso 1 1 calc R
H11C H 0.8961 0.3738 0.7365 0.108 Uiso 1 1 calc R
C12 C 0.7518(6) 0.5356(4) 0.4820(5) 0.0651(16) Uani 1 1 d .
H12A H 0.7169 0.5948 0.5131 0.098 Uiso 1 1 calc R
H12B H 0.7221 0.5429 0.4099 0.098 Uiso 1 1 calc R
H12C H 0.8506 0.5357 0.5034 0.098 Uiso 1 1 calc R
C13 C 0.5104(6) 0.3904(5) 0.3468(4) 0.0625(16) Uani 1 1 d .
H13A H 0.4710 0.3247 0.3151 0.094 Uiso 1 1 calc R
H13B H 0.5731 0.4191 0.3112 0.094 Uiso 1 1 calc R
H13C H 0.4385 0.4418 0.3452 0.094 Uiso 1 1 calc R
C14 C 0.4474(5) 0.2036(5) 0.4887(5) 0.0612(15) Uani 1 1 d .
H14A H 0.3754 0.2200 0.5205 0.092 Uiso 1 1 calc R
H14B H 0.4861 0.1345 0.5114 0.092 Uiso 1 1 calc R
H14C H 0.4102 0.2022 0.4168 0.092 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O3 Ta1 O1 147.86(13)
O3 Ta1 O2 74.04(12)
O1 Ta1 O2 73.83(12)
O3 Ta1 C8 127.26(15)
O1 Ta1 C8 82.92(15)
O2 Ta1 C8 151.19(14)
O3 Ta1 C9 129.60(15)
O1 Ta1 C9 81.15(15)
O2 Ta1 C9 150.16(14)
C8 Ta1 C9 33.32(15)
O3 Ta1 C7 93.01(14)
O1 Ta1 C7 115.45(15)
O2 Ta1 C7 151.65(14)
C8 Ta1 C7 34.42(15)
C9 Ta1 C7 55.75(16)
O3 Ta1 Cl1 87.28(10)
O1 Ta1 Cl1 85.42(10)
O2 Ta1 Cl1 75.58(9)
C8 Ta1 Cl1 119.86(12)
C9 Ta1 Cl1 86.61(12)
C7 Ta1 Cl1 129.93(12)
O3 Ta1 Cl2 87.14(11)
O1 Ta1 Cl2 85.29(10)
O2 Ta1 Cl2 77.33(9)
C8 Ta1 Cl2 84.14(11)
C9 Ta1 Cl2 116.98(12)
C7 Ta1 Cl2 76.91(12)
Cl1 Ta1 Cl2 152.85(4)
O3 Ta1 C5 96.91(15)
O1 Ta1 C5 111.45(16)
O2 Ta1 C5 150.38(14)
C8 Ta1 C5 55.07(15)
C9 Ta1 C5 33.45(16)
C7 Ta1 C5 54.38(16)
Cl1 Ta1 C5 75.86(12)
Cl2 Ta1 C5 131.22(12)
O3 Ta1 C6 76.93(15)
O1 Ta1 C6 135.17(15)
O2 Ta1 C6 150.80(14)
C8 Ta1 C6 55.64(16)
C9 Ta1 C6 55.16(17)
C7 Ta1 C6 32.91(15)
Cl1 Ta1 C6 100.02(14)
Cl2 Ta1 C6 104.54(14)
C5 Ta1 C6 32.30(17)
C1 O1 Ta1 123.9(3)
C2 O2 C3 118.8(3)
C2 O2 Ta1 114.5(3)
C3 O2 Ta1 114.0(3)
C4 O3 Ta1 123.1(3)
O1 C1 C2 109.0(4)
O2 C2 C1 103.5(4)
O2 C3 C4 103.0(3)
O3 C4 C3 108.8(4)
C6 C5 C9 109.4(4)
C6 C5 C10 123.7(5)
C9 C5 C10 126.2(5)
C6 C5 Ta1 74.3(3)
C9 C5 Ta1 71.9(2)
C10 C5 Ta1 127.9(3)
C5 C6 C7 108.1(4)
C5 C6 C11 126.7(5)
C7 C6 C11 125.1(5)
C5 C6 Ta1 73.4(3)
C7 C6 Ta1 72.1(2)
C11 C6 Ta1 122.6(3)
C6 C7 C8 107.5(4)
C6 C7 C12 125.4(5)
C8 C7 C12 126.4(5)
C6 C7 Ta1 75.0(3)
C8 C7 Ta1 71.6(2)
C12 C7 Ta1 126.2(3)
C9 C8 C7 107.5(4)
C9 C8 C13 126.9(5)
C7 C8 C13 125.4(5)
C9 C8 Ta1 74.1(3)
C7 C8 Ta1 73.9(2)
C13 C8 Ta1 120.4(3)
C8 C9 C5 107.4(4)
C8 C9 C14 127.3(5)
C5 C9 C14 125.3(5)
C8 C9 Ta1 72.6(2)
C5 C9 Ta1 74.7(2)
C14 C9 Ta1 119.4(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ta1 O3 1.935(3)
Ta1 O1 1.934(3)
Ta1 O2 2.205(3)
Ta1 C8 2.432(4)
Ta1 C9 2.452(4)
Ta1 C7 2.462(4)
Ta1 Cl1 2.4635(12)
Ta1 Cl2 2.4846(13)
Ta1 C5 2.488(4)
Ta1 C6 2.500(4)
O1 C1 1.409(6)
O2 C2 1.436(5)
O2 C3 1.445(5)
O3 C4 1.419(5)
C1 C2 1.517(7)
C3 C4 1.508(7)
C5 C6 1.388(7)
C5 C9 1.422(7)
C5 C10 1.500(6)
C6 C7 1.406(7)
C6 C11 1.507(7)
C7 C8 1.448(6)
C7 C12 1.496(7)
C8 C9 1.400(7)
C8 C13 1.483(6)
C9 C14 1.491(7)
