#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:38:18 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178788 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/42/4104265.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_4104265
loop_
_publ_author_name
'Aaron J. Rossini'
'Ryan W. Mills'
'Graham A. Briscoe'
'Erin L. Norton'
'Stephen J. Geier'
'Ivan Hung'
'Shaohui Zheng'
'Jochen Autschbach'
'Robert W. Schurko'
_publ_section_title
;
 Solid-State Chlorine NMR of Group IV Transition Metal Organometallic
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3317
_journal_page_last               3330
_journal_paper_doi               10.1021/ja808390a
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C5 H5 Cl3 Ti'
_chemical_formula_weight         219.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 115.963(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.5890(18)
_cell_length_b                   10.395(3)
_cell_length_c                   6.6896(19)
_cell_measurement_reflns_used    3088
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      3.39
_cell_volume                     411.9(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3897
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.39
_exptl_absorpt_coefficient_mu    1.920
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (SADABS,Bruker,2006)
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             216
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0309
_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)+(0.0420P)²+0.2947P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                699
_reflns_number_total             767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808390a_si_002.cif
_cod_data_source_block           sad
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               4104265
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
_atom_site_refinement_flags
Ti1 Ti 0.53480(10) 0.2500 0.66903(10) 0.0377(2) Uani 1 2 d S
Cl2 Cl 0.6117(2) 0.2500 0.37674(19) 0.0781(4) Uani 1 2 d S
Cl1 Cl 0.73298(14) 0.08398(9) 0.86910(15) 0.0740(3) Uani 1 1 d .
C1 C 0.2408(6) 0.1868(5) 0.7480(8) 0.0910(14) Uani 1 1 d .
H1A H 0.2546 0.1318 0.8723 0.109 Uiso 1 1 calc R
C3 C 0.1618(9) 0.2500 0.4139(9) 0.123(4) Uani 1 2 d S
H2A H 0.1062 0.2500 0.2519 0.148 Uiso 1 2 calc SR
C2 C 0.1934(7) 0.1461(5) 0.5405(12) 0.112(2) Uani 1 1 d .
H3A H 0.1640 0.0570 0.4877 0.134 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0311(4) 0.0418(4) 0.0370(4) 0.000 0.0119(3) 0.000
Cl2 0.0536(6) 0.1363(13) 0.0527(6) 0.000 0.0310(5) 0.000
Cl1 0.0634(5) 0.0610(5) 0.0843(6) 0.0218(4) 0.0201(4) 0.0194(4)
C1 0.0516(19) 0.127(4) 0.104(3) 0.059(3) 0.043(2) 0.011(2)
C3 0.029(2) 0.285(14) 0.045(3) 0.000 0.006(2) 0.000
C2 0.048(2) 0.090(3) 0.202(6) -0.078(4) 0.059(3) -0.033(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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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
Cl1 Ti1 Cl1 101.81(6) 4_565 .
Cl1 Ti1 Cl2 103.26(4) 4_565 .
Cl1 Ti1 Cl2 103.26(4) . .
Cl1 Ti1 C2 144.23(12) 4_565 .
Cl1 Ti1 C2 94.65(17) . .
Cl2 Ti1 C2 103.51(18) . .
Cl1 Ti1 C2 94.65(17) 4_565 4_565
Cl1 Ti1 C2 144.23(12) . 4_565
Cl2 Ti1 C2 103.51(18) . 4_565
C2 Ti1 C2 56.1(3) . 4_565
Cl1 Ti1 C3 127.04(5) 4_565 .
Cl1 Ti1 C3 127.04(5) . .
Cl2 Ti1 C3 85.88(16) . .
C2 Ti1 C3 33.70(18) . .
C2 Ti1 C3 33.70(18) 4_565 .
Cl1 Ti1 C1 88.39(10) 4_565 4_565
Cl1 Ti1 C1 114.36(14) . 4_565
Cl2 Ti1 C1 137.39(13) . 4_565
C2 Ti1 C1 55.85(15) . 4_565
C2 Ti1 C1 34.06(18) 4_565 4_565
C3 Ti1 C1 55.93(17) . 4_565
Cl1 Ti1 C1 114.36(14) 4_565 .
Cl1 Ti1 C1 88.39(10) . .
Cl2 Ti1 C1 137.39(13) . .
C2 Ti1 C1 34.06(18) . .
C2 Ti1 C1 55.85(15) 4_565 .
C3 Ti1 C1 55.93(17) . .
C1 Ti1 C1 33.0(2) 4_565 .
C1 C1 C2 108.3(3) 4_565 .
C1 C1 Ti1 73.51(12) 4_565 .
C2 C1 Ti1 72.2(2) . .
C1 C1 H1A 125.7 4_565 .
C2 C1 H1A 125.7 . .
Ti1 C1 H1A 125.7 . .
C2 C3 C2 108.4(6) . 4_565
C2 C3 Ti1 73.1(3) . .
C2 C3 Ti1 73.1(3) 4_565 .
C2 C3 H2A 125.6 . .
C2 C3 H2A 125.6 4_565 .
Ti1 C3 H2A 125.6 . .
C3 C2 C1 107.5(4) . .
C3 C2 Ti1 73.2(3) . .
C1 C2 Ti1 73.7(2) . .
C3 C2 H3A 125.9 . .
C1 C2 H3A 125.9 . .
Ti1 C2 H3A 125.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 Cl1 2.2236(10) 4_565
Ti1 Cl1 2.2236(10) .
Ti1 Cl2 2.2242(13) .
Ti1 C2 2.296(4) .
Ti1 C2 2.296(4) 4_565
Ti1 C3 2.298(5) .
Ti1 C1 2.315(3) 4_565
Ti1 C1 2.315(3) .
C1 C1 1.314(10) 4_565
C1 C2 1.350(7) .
C1 H1A 0.9800 .
C3 C2 1.332(7) .
C3 C2 1.332(7) 4_565
C3 H2A 0.9800 .
C2 H3A 0.9800 .
