#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:27:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179111 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/73/4307346.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_4307346
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         'C18 H26 N2 O4 Ti'
_chemical_formula_sum            'C18 H26 N2 O4 Ti'
_chemical_formula_weight         382.31
_chemical_name_common            '(4) Ti(OPy)2(OPri)2'
_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                 92.635(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.268(2)
_cell_length_b                   14.820(3)
_cell_length_c                   12.104(2)
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.17
_cell_volume                     2019.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14679
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       irregular
_exptl_crystal_F_000             808
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0592
_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)+(0.0564P)²+2.2950P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1411
_reflns_number_gt                2892
_reflns_number_total             3697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0618798si20061106_104430_02.cif
_cod_data_source_block           em01s
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_cell_volume        2019.1(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4307346
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.07431(5) 0.22784(4) 0.72318(5) 0.02650(19) Uani 1 1 d . . .
N1 N 0.1085(2) 0.26109(18) 0.9028(2) 0.0303(6) Uani 1 1 d . . .
N2 N 0.1095(2) 0.08844(18) 0.7893(2) 0.0289(6) Uani 1 1 d . . .
O1 O 0.24195(19) 0.24426(15) 0.7397(2) 0.0338(6) Uani 1 1 d . . .
O2 O -0.07582(18) 0.18518(15) 0.76676(18) 0.0275(5) Uani 1 1 d . . .
O3 O 0.0813(2) 0.18410(18) 0.5832(2) 0.0399(6) Uani 1 1 d . . .
O4 O 0.01996(19) 0.34244(15) 0.6989(2) 0.0361(6) Uani 1 1 d . . .
C1 C 0.3051(3) 0.2626(3) 0.8383(3) 0.0435(9) Uani 1 1 d . . .
H1A H 0.3528 0.3180 0.8297 0.052 Uiso 1 1 calc R . .
H1B H 0.3604 0.2122 0.8560 0.052 Uiso 1 1 calc R . .
C2 C 0.2229(3) 0.2751(2) 0.9321(3) 0.0371(8) Uani 1 1 d . . .
C3 C 0.2604(4) 0.2966(3) 1.0388(4) 0.0501(11) Uani 1 1 d . . .
H3 H 0.3423 0.3060 1.0576 0.060 Uiso 1 1 calc R . .
C4 C 0.1773(4) 0.3041(3) 1.1172(4) 0.0534(11) Uani 1 1 d . . .
H4 H 0.2011 0.3180 1.1916 0.064 Uiso 1 1 calc R . .
C5 C 0.0579(4) 0.2914(3) 1.0876(3) 0.0469(10) Uani 1 1 d . . .
H5 H -0.0011 0.2969 1.1408 0.056 Uiso 1 1 calc R . .
C6 C 0.0276(3) 0.2706(2) 0.9800(3) 0.0377(8) Uani 1 1 d . . .
H6 H -0.0540 0.2626 0.9589 0.045 Uiso 1 1 calc R . .
C7 C -0.0980(3) 0.1007(2) 0.8099(3) 0.0338(8) Uani 1 1 d . . .
H7A H -0.1563 0.0687 0.7603 0.041 Uiso 1 1 calc R . .
H7B H -0.1331 0.1075 0.8829 0.041 Uiso 1 1 calc R . .
C8 C 0.0136(3) 0.0454(2) 0.8226(3) 0.0287(7) Uani 1 1 d . . .
C9 C 0.0191(3) -0.0419(2) 0.8624(3) 0.0382(9) Uani 1 1 d . . .
H9 H -0.0503 -0.0710 0.8863 0.046 Uiso 1 1 calc R . .
C10 C 0.1268(3) -0.0862(2) 0.8671(3) 0.0422(9) Uani 1 1 d . . .
H10 H 0.1323 -0.1463 0.8943 0.051 Uiso 1 1 calc R . .
C11 C 0.2267(3) -0.0424(2) 0.8317(3) 0.0441(10) Uani 1 1 d . . .
H11 H 0.3018 -0.0717 0.8336 0.053 Uiso 1 1 calc R . .
C12 C 0.2142(3) 0.0442(2) 0.7939(3) 0.0402(9) Uani 1 1 d . . .
H12 H 0.2825 0.0746 0.7697 0.048 Uiso 1 1 calc R . .
C13 C 0.1682(4) 0.1653(3) 0.5065(4) 0.0611(13) Uani 1 1 d . . .
H13 H 0.2485 0.1666 0.5453 0.073 Uiso 1 1 calc R . .
C14 C 0.1457(7) 0.0726(6) 0.4593(7) 0.163(4) Uani 1 1 d . . .
H14A H 0.1490 0.0281 0.5193 0.244 Uiso 1 1 calc R . .
H14B H 0.2065 0.0584 0.4066 0.244 Uiso 1 1 calc R . .
H14C H 0.0670 0.0710 0.4213 0.244 Uiso 1 1 calc R . .
C15 C 0.1632(5) 0.2355(5) 0.4177(5) 0.109(3) Uani 1 1 d . . .
H15A H 0.0939 0.2246 0.3676 0.164 Uiso 1 1 calc R . .
H15B H 0.2357 0.2324 0.3760 0.164 Uiso 1 1 calc R . .
H15C H 0.1569 0.2954 0.4512 0.164 Uiso 1 1 calc R . .
C16 C -0.0779(4) 0.3971(3) 0.7193(4) 0.0630(14) Uani 1 1 d . . .
H16 H -0.1409 0.3604 0.7537 0.076 Uiso 1 1 calc R . .
C17 C -0.1277(6) 0.4372(5) 0.6037(6) 0.117(2) Uani 1 1 d . . .
H17A H -0.0868 0.4939 0.5886 0.175 Uiso 1 1 calc R . .
H17B H -0.2131 0.4485 0.6070 0.175 Uiso 1 1 calc R . .
H17C H -0.1136 0.3938 0.5446 0.175 Uiso 1 1 calc R . .
C18 C -0.0450(6) 0.4717(4) 0.7901(7) 0.123(3) Uani 1 1 d . . .
H18A H 0.0034 0.4498 0.8538 0.184 Uiso 1 1 calc R . .
H18B H -0.1169 0.5007 0.8159 0.184 Uiso 1 1 calc R . .
H18C H 0.0007 0.5155 0.7489 0.184 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'
Ti Ti 0.2776 0.4457 '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'
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 O4 102.13(12) . . ?
O3 Ti1 O2 102.54(10) . . ?
O4 Ti1 O2 93.32(10) . . ?
O3 Ti1 O1 93.31(10) . . ?
O4 Ti1 O1 102.81(10) . . ?
O2 Ti1 O1 154.51(10) . . ?
O3 Ti1 N2 89.42(11) . . ?
O4 Ti1 N2 165.19(10) . . ?
O2 Ti1 N2 74.94(9) . . ?
O1 Ti1 N2 85.53(10) . . ?
O3 Ti1 N1 165.29(10) . . ?
O4 Ti1 N1 89.62(11) . . ?
O2 Ti1 N1 85.38(10) . . ?
O1 Ti1 N1 75.25(10) . . ?
N2 Ti1 N1 80.61(10) . . ?
C2 N1 C6 118.5(3) . . ?
C2 N1 Ti1 114.2(2) . . ?
C6 N1 Ti1 127.2(2) . . ?
C8 N2 C12 118.3(3) . . ?
C8 N2 Ti1 114.6(2) . . ?
C12 N2 Ti1 127.0(2) . . ?
C1 O1 Ti1 125.6(2) . . ?
C7 O2 Ti1 125.68(19) . . ?
C13 O3 Ti1 138.2(2) . . ?
C16 O4 Ti1 140.5(2) . . ?
O1 C1 C2 111.3(3) . . ?
O1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
O1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N1 C2 C3 122.3(4) . . ?
N1 C2 C1 113.5(3) . . ?
C3 C2 C1 124.1(3) . . ?
C4 C3 C2 118.6(4) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C3 C4 C5 119.7(4) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 118.3(4) . . ?
C6 C5 H5 120.9 . . ?
C4 C5 H5 120.9 . . ?
N1 C6 C5 122.6(3) . . ?
N1 C6 H6 118.7 . . ?
C5 C6 H6 118.7 . . ?
O2 C7 C8 111.5(3) . . ?
O2 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
O2 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
N2 C8 C9 122.0(3) . . ?
N2 C8 C7 113.2(3) . . ?
C9 C8 C7 124.8(3) . . ?
C10 C9 C8 119.1(3) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
C9 C10 C11 119.4(3) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C12 C11 C10 118.0(3) . . ?
C12 C11 H11 121.0 . . ?
C10 C11 H11 121.0 . . ?
N2 C12 C11 123.1(3) . . ?
N2 C12 H12 118.4 . . ?
C11 C12 H12 118.4 . . ?
O3 C13 C15 109.4(4) . . ?
O3 C13 C14 108.7(4) . . ?
C15 C13 C14 111.2(6) . . ?
O3 C13 H13 109.2 . . ?
C15 C13 H13 109.2 . . ?
C14 C13 H13 109.2 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O4 C16 C18 111.6(4) . . ?
O4 C16 C17 107.9(4) . . ?
C18 C16 C17 107.8(5) . . ?
O4 C16 H16 109.8 . . ?
C18 C16 H16 109.8 . . ?
C17 C16 H16 109.8 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
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 1.819(2) . ?
Ti1 O4 1.825(2) . ?
Ti1 O2 1.903(2) . ?
Ti1 O1 1.906(2) . ?
Ti1 N2 2.244(3) . ?
Ti1 N1 2.246(3) . ?
N1 C2 1.337(4) . ?
N1 C6 1.342(4) . ?
N2 C8 1.333(4) . ?
N2 C12 1.348(4) . ?
O1 C1 1.388(4) . ?
O2 C7 1.384(4) . ?
O3 C13 1.407(4) . ?
O4 C16 1.400(4) . ?
C1 C2 1.510(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.378(5) . ?
C3 C4 1.368(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.367(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.503(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.382(5) . ?
C9 C10 1.378(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.368(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C15 1.495(7) . ?
C13 C14 1.505(8) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C18 1.437(7) . ?
C16 C17 1.598(8) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
