#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:38:18 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178788 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/42/4104218.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_4104218
loop_
_publ_author_name
'Rocío Arteaga-Müller'
'Hayato Tsurugi'
'Teruhiko Saito'
'Masao Yanagawa'
'Seiji Oda'
'Kazushi Mashima'
_publ_section_title
;
 New Tantalum Ligand-Free Catalyst System for Highly Selective
 Trimerization of Ethylene Affording 1-Hexene: New Evidence of a
 Metallacycle Mechanism
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5370
_journal_page_last               5371
_journal_paper_doi               10.1021/ja8100837
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C10 H20 Cl3 Nb O2'
_chemical_formula_sum            'C10 H20 Cl3 Nb O2'
_chemical_formula_weight         371.52
_chemical_name_common            Nb-complex
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.058(3)
_cell_angle_beta                 78.262(2)
_cell_angle_gamma                71.287(3)
_cell_formula_units_Z            2
_cell_length_a                   6.9774(5)
_cell_length_b                   7.2895(6)
_cell_length_c                   15.4878(11)
_cell_measurement_reflns_used    11488
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     723.87(10)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 2.0'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  'teXsan Ver. 2.0'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      123(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13618
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.369
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         3299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0210
_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)+(0.0283P)²+0.5037P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0632
_reflns_number_gt                3067
_reflns_number_total             3299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8100837_si_001.cif
_cod_data_source_block           Nb
_cod_original_cell_volume        723.87(9)
_cod_original_sg_symbol_H-M      'P -1         '
_cod_database_code               4104218
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Nb Nb 0.51194(3) 0.21568(3) 0.212538(11) 0.01201(7) Uani 1 1 d
Cl1 Cl 0.18079(8) 0.37733(8) 0.28889(3) 0.02027(12) Uani 1 1 d
Cl2 Cl 0.63623(8) 0.49509(7) 0.17382(3) 0.01896(11) Uani 1 1 d
Cl3 Cl 0.78147(8) 0.04131(7) 0.10605(3) 0.01688(11) Uani 1 1 d
O1 O 0.3332(2) 0.3328(2) 0.09128(10) 0.0167(3) Uani 1 1 d
O2 O 0.3617(2) -0.0037(2) 0.20338(9) 0.0158(3) Uani 1 1 d
C1 C 0.6167(3) 0.1858(3) 0.33088(14) 0.0168(4) Uani 1 1 d
C2 C 0.6510(3) 0.0120(3) 0.31080(14) 0.0147(4) Uani 1 1 d
C3 C 0.7393(4) -0.2015(3) 0.33318(15) 0.0212(5) Uani 1 1 d
C4 C 0.6335(4) 0.3111(3) 0.39240(15) 0.0220(5) Uani 1 1 d
C5 C 0.8299(4) -0.2671(3) 0.41957(16) 0.0225(5) Uani 1 1 d
C6 C 0.7327(4) 0.2050(4) 0.47401(16) 0.0283(5) Uani 1 1 d
C7 C 0.2278(4) -0.0821(3) 0.27461(15) 0.0218(5) Uani 1 1 d
C8 C 0.3084(3) 0.0100(3) 0.11571(14) 0.0174(4) Uani 1 1 d
C9 C 0.2013(3) 0.2193(3) 0.08549(15) 0.0180(4) Uani 1 1 d
C10 C 0.2373(4) 0.5390(3) 0.06557(15) 0.0216(5) Uani 1 1 d
H1 H 0.6323 -0.2642 0.3373 0.027 Uiso 1 1 d
H2 H 0.8498 -0.2482 0.2844 0.027 Uiso 1 1 d
H3 H 0.7133 0.3982 0.3583 0.028 Uiso 1 1 d
H4 H 0.4942 0.3922 0.4130 0.028 Uiso 1 1 d
H5 H 0.7218 -0.2212 0.4685 0.028 Uiso 1 1 d
H6 H 0.8821 -0.4087 0.4285 0.028 Uiso 1 1 d
H7 H 0.9403 -0.2089 0.4152 0.028 Uiso 1 1 d
H8 H 0.6555 0.1181 0.5095 0.033 Uiso 1 1 d
H9 H 0.8744 0.1261 0.4550 0.033 Uiso 1 1 d
H10 H 0.7365 0.2995 0.5107 0.033 Uiso 1 1 d
H11 H 0.0876 0.0027 0.2751 0.027 Uiso 1 1 d
H12 H 0.2368 -0.2136 0.2659 0.027 Uiso 1 1 d
H13 H 0.2725 -0.0869 0.3317 0.027 Uiso 1 1 d
H14 H 0.4334 -0.0354 0.0736 0.021 Uiso 1 1 d
H15 H 0.2182 -0.0705 0.1189 0.021 Uiso 1 1 d
H16 H 0.0690 0.2638 0.1243 0.022 Uiso 1 1 d
H17 H 0.1761 0.2359 0.0241 0.022 Uiso 1 1 d
H18 H 0.3307 0.6123 0.0707 0.026 Uiso 1 1 d
H19 H 0.2119 0.5604 0.0048 0.026 Uiso 1 1 d
H20 H 0.1094 0.5820 0.1061 0.026 Uiso 1 1 d
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'
Cl Cl 0.1484 0.1585 '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'
Nb Nb -2.0727 0.6215 '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
C1 Nb C2 36.66(8)
C1 Nb O2 115.25(7)
C2 Nb O2 85.39(7)
C1 Nb O1 163.81(7)
C2 Nb O1 157.05(7)
O2 Nb O1 72.63(5)
C1 Nb Cl2 84.45(6)
C2 Nb Cl2 113.42(6)
O2 Nb Cl2 160.24(4)
O1 Nb Cl2 87.92(4)
C1 Nb Cl1 86.12(6)
C2 Nb Cl1 103.93(6)
O2 Nb Cl1 83.72(4)
O1 Nb Cl1 80.63(4)
Cl2 Nb Cl1 96.80(2)
C1 Nb Cl3 110.17(6)
C2 Nb Cl3 86.97(6)
O2 Nb Cl3 83.69(4)
O1 Nb Cl3 84.16(4)
Cl2 Nb Cl3 91.058(19)
Cl1 Nb Cl3 162.59(2)
C9 O1 C10 110.50(16)
C9 O1 Nb 113.42(12)
C10 O1 Nb 122.80(12)
C7 O2 C8 113.08(16)
C7 O2 Nb 125.87(12)
C8 O2 Nb 113.57(12)
C2 C1 C4 148.8(2)
C2 C1 Nb 72.16(13)
C4 C1 Nb 139.01(16)
C1 C2 C3 148.0(2)
C1 C2 Nb 71.18(13)
C3 C2 Nb 140.74(15)
C2 C3 C5 115.52(18)
C1 C4 C6 116.2(2)
O2 C8 C9 108.71(16)
O1 C9 C8 107.07(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Nb C1 2.057(2)
Nb C2 2.069(2)
Nb O2 2.2138(14)
Nb O1 2.3393(14)
Nb Cl2 2.3913(6)
Nb Cl1 2.4074(6)
Nb Cl3 2.4233(5)
O1 C9 1.446(2)
O1 C10 1.450(3)
O2 C7 1.449(3)
O2 C8 1.457(2)
C1 C2 1.298(3)
C1 C4 1.483(3)
C2 C3 1.480(3)
C3 C5 1.525(3)
C4 C6 1.522(3)
C8 C9 1.498(3)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C1 Nb O1 C9 -112.6(3)
C2 Nb O1 C9 26.5(2)
O2 Nb O1 C9 9.15(13)
Cl2 Nb O1 C9 -174.38(13)
Cl1 Nb O1 C9 -77.14(13)
Cl3 Nb O1 C9 94.34(13)
C1 Nb O1 C10 24.6(3)
C2 Nb O1 C10 163.68(19)
O2 Nb O1 C10 146.31(16)
Cl2 Nb O1 C10 -37.22(15)
Cl1 Nb O1 C10 60.02(15)
Cl3 Nb O1 C10 -128.50(15)
C1 Nb O2 C7 38.40(18)
C2 Nb O2 C7 60.30(17)
O1 Nb O2 C7 -126.41(17)
Cl2 Nb O2 C7 -136.90(15)
Cl1 Nb O2 C7 -44.29(15)
Cl3 Nb O2 C7 147.76(16)
C1 Nb O2 C8 -174.12(13)
C2 Nb O2 C8 -152.22(14)
O1 Nb O2 C8 21.07(12)
Cl2 Nb O2 C8 10.6(2)
Cl1 Nb O2 C8 103.19(13)
Cl3 Nb O2 C8 -64.77(12)
O2 Nb C1 C2 38.51(15)
O1 Nb C1 C2 154.7(2)
Cl2 Nb C1 C2 -143.08(13)
Cl1 Nb C1 C2 119.69(13)
Cl3 Nb C1 C2 -54.00(13)
C2 Nb C1 C4 178.8(3)
O2 Nb C1 C4 -142.7(2)
O1 Nb C1 C4 -26.5(4)
Cl2 Nb C1 C4 35.7(2)
Cl1 Nb C1 C4 -61.5(2)
Cl3 Nb C1 C4 124.8(2)
C4 C1 C2 C3 -2.0(7)
Nb C1 C2 C3 176.5(4)
C4 C1 C2 Nb -178.5(4)
O2 Nb C2 C1 -145.60(13)
O1 Nb C2 C1 -162.21(16)
Cl2 Nb C2 C1 40.66(14)
Cl1 Nb C2 C1 -63.25(13)
Cl3 Nb C2 C1 130.50(13)
C1 Nb C2 C3 -177.1(3)
O2 Nb C2 C3 37.3(2)
O1 Nb C2 C3 20.7(4)
Cl2 Nb C2 C3 -136.4(2)
Cl1 Nb C2 C3 119.7(2)
Cl3 Nb C2 C3 -46.6(2)
C1 C2 C3 C5 3.5(5)
Nb C2 C3 C5 178.26(18)
C2 C1 C4 C6 -1.2(5)
Nb C1 C4 C6 -178.96(19)
C7 O2 C8 C9 103.6(2)
Nb O2 C8 C9 -48.10(19)
C10 O1 C9 C8 -178.27(17)
Nb O1 C9 C8 -35.87(19)
O2 C8 C9 O1 54.0(2)
