#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:27:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179111 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/73/4307356.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_4307356
loop_
_publ_author_name
'Timothy J. Boyle'
'Robin M. Sewell'
'Leigh Anna M. Ottley'
'Harry D. Pratt'
'Christopher J. Quintana'
'Scott D. Bunge'
_publ_contact_author_address     '1001 University Blvd, Albuquerque, NM 87106'
_publ_contact_author_email       tjboyle@sandia.gov
_publ_contact_author_fax         '(505) 272-7336'
_publ_contact_author_name        'Timothy J. Boyle et.al.'
_publ_section_title
;
Controlled Synthesis of a Structurally Characterized Family of Sterically
Constrained Heterocyclic Alkoxy-Modified Titanium Alkoxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1825
_journal_page_last               1835
_journal_paper_doi               10.1021/ic0618798
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C24 H20 Br2 N2 O4 Ti'
_chemical_formula_sum            'C24 H20 Br2 N2 O4 Ti'
_chemical_formula_weight         608.09
_chemical_name_common            '(16) Ti(OPy)2(2BP)2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                95.62(3)
_cell_angle_beta                 90.64(3)
_cell_angle_gamma                102.69(3)
_cell_formula_units_Z            2
_cell_length_a                   8.995(18)
_cell_length_b                   11.89(2)
_cell_length_c                   12.11(2)
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      25.22
_cell_measurement_theta_min      1.69
_cell_volume                     1257(4)
_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      297(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.906
_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  0.0984
_diffrn_reflns_av_sigmaI/netI    0.2126
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7749
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         25.22
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    3.551
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_correction_T_min  0.129
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       irregular
_exptl_crystal_F_000             604.0
_exptl_crystal_size_max          .554
_exptl_crystal_size_mid          .432
_exptl_crystal_size_min          .095
_refine_diff_density_max         1.542
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.1966
_refine_ls_R_factor_gt           0.0787
_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)+(0.1160P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.2603
_reflns_number_gt                1573
_reflns_number_total             4121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0618798si20061106_104430_12.cif
_cod_data_source_block           6sp131s
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4307356
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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.0906(2) 0.39957(16) 0.74079(15) 0.0476(6) Uani 1 1 d . . .
Br1 Br 0.4477(2) 0.18425(12) 0.65611(11) 0.0861(6) Uani 1 1 d . . .
Br2 Br 0.40753(17) 0.73265(12) 0.61256(11) 0.0812(6) Uani 1 1 d . . .
O1 O 0.0010(8) 0.3898(6) 0.8813(5) 0.0523(19) Uani 1 1 d . . .
O2 O 0.0883(9) 0.3695(7) 0.5833(5) 0.062(2) Uani 1 1 d . . .
O3 O 0.2584(9) 0.3400(7) 0.7832(6) 0.061(2) Uani 1 1 d . . .
O4 O 0.1865(8) 0.5594(6) 0.7444(6) 0.054(2) Uani 1 1 d . . .
N1 N -0.0430(11) 0.2141(8) 0.7021(8) 0.061(3) Uani 1 1 d . . .
N2 N -0.1332(10) 0.4467(7) 0.7161(7) 0.048(2) Uani 1 1 d . . .
C11 C -0.0960(15) 0.1348(11) 0.7745(11) 0.074(4) Uani 1 1 d . . .
H11 H -0.0765 0.1556 0.8501 0.089 Uiso 1 1 calc R . .
C12 C -0.1784(18) 0.0236(13) 0.7383(16) 0.093(5) Uani 1 1 d . . .
H12 H -0.2174 -0.0279 0.7894 0.112 Uiso 1 1 calc R . .
C13 C -0.201(2) -0.0093(13) 0.6267(19) 0.108(6) Uani 1 1 d . . .
H13 H -0.2539 -0.0843 0.6022 0.129 Uiso 1 1 calc R . .
C14 C -0.1485(18) 0.0662(15) 0.5514(14) 0.099(5) Uani 1 1 d . . .
H14 H -0.1668 0.0450 0.4757 0.119 Uiso 1 1 calc R . .
C15 C -0.0637(15) 0.1792(11) 0.5925(11) 0.068(4) Uani 1 1 d . . .
C16 C 0.0059(19) 0.2701(13) 0.5194(10) 0.093(5) Uani 1 1 d . . .
H16A H 0.0733 0.2397 0.4684 0.112 Uiso 1 1 calc R . .
H16B H -0.0739 0.2903 0.4761 0.112 Uiso 1 1 calc R . .
C17 C -0.1540(13) 0.3965(9) 0.9038(8) 0.054(3) Uani 1 1 d . . .
H17A H -0.1561 0.4483 0.9705 0.065 Uiso 1 1 calc R . .
H17B H -0.2136 0.3204 0.9157 0.065 Uiso 1 1 calc R . .
C18 C -0.2196(12) 0.4394(9) 0.8096(9) 0.051(3) Uani 1 1 d . . .
C19 C -0.3630(15) 0.4722(9) 0.8082(11) 0.063(3) Uani 1 1 d . . .
H19 H -0.4226 0.4665 0.8705 0.076 Uiso 1 1 calc R . .
C20 C -0.4129(15) 0.5117(11) 0.7160(12) 0.073(4) Uani 1 1 d . . .
H20 H -0.5064 0.5329 0.7156 0.088 Uiso 1 1 calc R . .
C21 C -0.3233(17) 0.5206(12) 0.6216(11) 0.078(4) Uani 1 1 d . . .
H21 H -0.3571 0.5462 0.5578 0.093 Uiso 1 1 calc R . .
C22 C -0.1804(15) 0.4896(11) 0.6264(10) 0.066(4) Uani 1 1 d . . .
H22 H -0.1174 0.4991 0.5661 0.079 Uiso 1 1 calc R . .
C23 C 0.3218(14) 0.2806(10) 0.8522(9) 0.054(3) Uani 1 1 d . . .
C24 C 0.3032(15) 0.2939(11) 0.9683(10) 0.071(4) Uani 1 1 d . . .
H24 H 0.2402 0.3411 0.9971 0.086 Uiso 1 1 calc R . .
C25 C 0.3740(16) 0.2404(11) 1.0373(10) 0.068(4) Uani 1 1 d . . .
H25 H 0.3609 0.2522 1.1133 0.081 Uiso 1 1 calc R . .
C26 C 0.4691(16) 0.1657(11) 0.9967(11) 0.075(4) Uani 1 1 d . . .
H26 H 0.5176 0.1285 1.0455 0.090 Uiso 1 1 calc R . .
C27 C 0.4889(13) 0.1488(9) 0.8822(11) 0.061(3) Uani 1 1 d . . .
H27 H 0.5509 0.1007 0.8535 0.074 Uiso 1 1 calc R . .
C28 C 0.4134(15) 0.2061(11) 0.8125(8) 0.063(4) Uani 1 1 d . . .
C29 C 0.1765(13) 0.6715(9) 0.7733(8) 0.050(3) Uani 1 1 d . . .
C30 C 0.0751(13) 0.6995(10) 0.8511(9) 0.059(3) Uani 1 1 d . . .
H30 H 0.0112 0.6401 0.8836 0.070 Uiso 1 1 calc R . .
C31 C 0.0655(17) 0.8142(12) 0.8825(11) 0.084(4) Uani 1 1 d . . .
H31 H -0.0021 0.8307 0.9359 0.101 Uiso 1 1 calc R . .
C32 C 0.1591(17) 0.9033(11) 0.8323(12) 0.081(4) Uani 1 1 d . . .
H32 H 0.1519 0.9798 0.8502 0.097 Uiso 1 1 calc R . .
C33 C 0.2628(14) 0.8771(11) 0.7557(10) 0.067(4) Uani 1 1 d . . .
H33 H 0.3297 0.9367 0.7256 0.081 Uiso 1 1 calc R . .
C34 C 0.2676(13) 0.7640(10) 0.7237(9) 0.056(3) Uani 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'
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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
_geom_angle_publ_flag
O3 Ti1 O1 93.9(3) . . ?
O3 Ti1 O4 99.8(4) . . ?
O1 Ti1 O4 103.1(3) . . ?
O3 Ti1 O2 101.6(3) . . ?
O1 Ti1 O2 153.6(3) . . ?
O4 Ti1 O2 95.2(3) . . ?
O3 Ti1 N2 168.1(3) . . ?
O1 Ti1 N2 75.8(3) . . ?
O4 Ti1 N2 88.6(3) . . ?
O2 Ti1 N2 85.9(3) . . ?
O3 Ti1 N1 88.1(4) . . ?
O1 Ti1 N1 84.8(3) . . ?
O4 Ti1 N1 168.3(3) . . ?
O2 Ti1 N1 74.6(3) . . ?
N2 Ti1 N1 85.0(4) . . ?
C17 O1 Ti1 125.2(6) . . ?
C16 O2 Ti1 126.4(7) . . ?
C23 O3 Ti1 149.6(7) . . ?
C29 O4 Ti1 147.0(7) . . ?
C15 N1 C11 117.8(11) . . ?
C15 N1 Ti1 113.8(8) . . ?
C11 N1 Ti1 128.3(9) . . ?
C22 N2 C18 120.2(10) . . ?
C22 N2 Ti1 126.6(7) . . ?
C18 N2 Ti1 112.8(7) . . ?
N1 C11 C12 121.9(13) . . ?
N1 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C13 C12 C11 119.3(14) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C14 C13 C12 120.8(15) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C15 117.8(15) . . ?
C13 C14 H14 121.1 . . ?
C15 C14 H14 121.1 . . ?
N1 C15 C14 122.2(13) . . ?
N1 C15 C16 114.0(11) . . ?
C14 C15 C16 123.8(13) . . ?
O2 C16 C15 110.6(10) . . ?
O2 C16 H16A 109.5 . . ?
C15 C16 H16A 109.5 . . ?
O2 C16 H16B 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
O1 C17 C18 109.3(8) . . ?
O1 C17 H17A 109.8 . . ?
C18 C17 H17A 109.8 . . ?
O1 C17 H17B 109.8 . . ?
C18 C17 H17B 109.8 . . ?
H17A C17 H17B 108.3 . . ?
N2 C18 C19 119.3(11) . . ?
N2 C18 C17 115.6(10) . . ?
C19 C18 C17 125.1(10) . . ?
C20 C19 C18 120.3(11) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C21 120.2(13) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
C20 C21 C22 118.2(13) . . ?
C20 C21 H21 120.9 . . ?
C22 C21 H21 120.9 . . ?
N2 C22 C21 121.7(11) . . ?
N2 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
O3 C23 C28 121.1(10) . . ?
O3 C23 C24 121.7(11) . . ?
C28 C23 C24 117.2(12) . . ?
C25 C24 C23 121.6(13) . . ?
C25 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
C24 C25 C26 121.1(12) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C27 C26 C25 119.1(12) . . ?
C27 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
C28 C27 C26 118.3(12) . . ?
C28 C27 H27 120.9 . . ?
C26 C27 H27 120.9 . . ?
C23 C28 C27 122.7(11) . . ?
C23 C28 Br1 120.1(9) . . ?
C27 C28 Br1 117.1(10) . . ?
O4 C29 C30 121.8(9) . . ?
O4 C29 C34 121.3(9) . . ?
C30 C29 C34 116.9(10) . . ?
C29 C30 C31 122.2(10) . . ?
C29 C30 H30 118.9 . . ?
C31 C30 H30 118.9 . . ?
C32 C31 C30 119.0(12) . . ?
C32 C31 H31 120.5 . . ?
C30 C31 H31 120.5 . . ?
C33 C32 C31 119.5(12) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C34 C33 C32 120.6(11) . . ?
C34 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
C33 C34 C29 121.5(10) . . ?
C33 C34 Br2 118.8(9) . . ?
C29 C34 Br2 119.7(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O3 1.889(9) . ?
Ti1 O1 1.894(7) . ?
Ti1 O4 1.902(8) . ?
Ti1 O2 1.906(8) . ?
Ti1 N2 2.229(10) . ?
Ti1 N1 2.269(10) . ?
Br1 C28 1.925(11) . ?
Br2 C34 1.919(11) . ?
O1 C17 1.442(13) . ?
O2 C16 1.403(14) . ?
O3 C23 1.344(14) . ?
O4 C29 1.367(12) . ?
N1 C15 1.351(15) . ?
N1 C11 1.362(14) . ?
N2 C22 1.348(14) . ?
N2 C18 1.380(12) . ?
C11 C12 1.393(18) . ?
C11 H11 0.9300 . ?
C12 C13 1.37(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.36(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.430(18) . ?
C14 H14 0.9300 . ?
C15 C16 1.498(18) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.464(15) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.428(16) . ?
C19 C20 1.361(18) . ?
C19 H19 0.9300 . ?
C20 C21 1.405(17) . ?
C20 H20 0.9300 . ?
C21 C22 1.416(18) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C28 1.393(17) . ?
C23 C24 1.415(15) . ?
C24 C25 1.334(17) . ?
C24 H24 0.9300 . ?
C25 C26 1.421(17) . ?
C25 H25 0.9300 . ?
C26 C27 1.401(16) . ?
C26 H26 0.9300 . ?
C27 C28 1.393(17) . ?
C27 H27 0.9300 . ?
C29 C30 1.387(14) . ?
C29 C34 1.409(14) . ?
C30 C31 1.400(16) . ?
C30 H30 0.9300 . ?
C31 C32 1.395(17) . ?
C31 H31 0.9300 . ?
C32 C33 1.385(17) . ?
C32 H32 0.9300 . ?
C33 C34 1.372(17) . ?
C33 H33 0.9300 . ?
