#------------------------------------------------------------------------------
#$Date: 2019-11-05 12:41:35 +0200 (Tue, 05 Nov 2019) $
#$Revision: 223329 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/16/7701662.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_7701662
loop_
_publ_author_name
'Perry, Mitchell R.'
'Gilmour, Damon J.'
'Schafer, Laurel L.'
_publ_section_title
;
 Mono, bis, and tris(phosphoramidate) titanium complexes: synthesis,
 structure, and reactivity investigations.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9782
_journal_page_last               9790
_journal_paper_doi               10.1039/c9dt00911f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C28 H50 N4 O6 P2 Ti'
_chemical_formula_sum            'C28 H50 N4 O6 P2 Ti'
_chemical_formula_weight         648.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2019-03-25 deposited with the CCDC.	2019-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.550(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.113(3)
_cell_length_b                   10.978(2)
_cell_length_c                   11.644(2)
_cell_measurement_reflns_used    5575
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.68
_cell_volume                     1666.1(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9380
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.394
_diffrn_reflns_theta_max         25.394
_diffrn_reflns_theta_min         1.894
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0561 before and 0.0455 after correction. The Ratio of minimum to maximum transmission is 0.8713. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       prism
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.604
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.14(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         2916
_refine_ls_number_restraints     592
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+20.2496P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1608
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                2706
_reflns_number_total             2916
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00911f2.cif
_cod_data_source_block           ls627_1
_cod_original_cell_volume        1666.2(6)
_cod_database_code               7701662
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.907
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.86(11)
 0.14(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C9-C10
 1.4 with sigma of 0.02
 C9-C10 \\sim C12-C11 \\sim C9A-C10A \\sim C12A-C11A
 with sigma of 0.01
 O2A-C11A \\sim O1A-C9A \\sim O2-C11 \\sim O1-C9
 with sigma of 0.01
 N2-C13 \\sim N2-C14 \\sim N2A-C13A \\sim N2A-C14A
 with sigma of 0.01
 P1-O2 \\sim P1-O1 \\sim P1A-O1A \\sim P1A-O2A
 with sigma of 0.01
 P1A-O3A \\sim P1-O3
 with sigma of 0.01
 P1A-N1A \\sim P1-N1
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C9A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) = Uanis(O3A)
Uanis(C1A) = Uanis(C1)
Uanis(C8) = Uanis(C8A)
Uanis(C2) = Uanis(C2A)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=
 Sof(C6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 Sof(H8AC)=Sof(P1A)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(O1A)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(O2A)=Sof(C12A)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=Sof(N1A)=Sof(O3A)=1-FVAR(1)
 Sof(P1)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(N1)=Sof(C1)=Sof(C2)=Sof(C3)=Sof(H3)=
 Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: N2(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C14(0.5) H14A(0.5)
 H14B(0.5) H14C(0.5) N2A(0.5) C14A(0.5) H14D(0.5) H14E(0.5) H14F(0.5) C13A(0.5)
 H13D(0.5) H13E(0.5) H13F(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C9A(H9AA,H9AB), C11A(H11C,H11D)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C3A(H3A), C4A(H4A), C5A(H5A)
7.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C1A(C2A,C3A,C4A,C5A,C6A)
7.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,
 H8AC), C10A(H10D,H10E,H10F), C12A(H12D,H12E,H12F), C14A(H14D,H14E,H14F),
 C13A(H13D,H13E,H13F)
;
_olex2_exptl_crystal_mounting_method goniometer
_olex2_submission_original_sample_id vc-7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.5004(4) 0.4781(5) 0.3012(6) 0.0217(13) Uani 0.691(14) 1 d D U . A 1
O1 O 0.4622(9) 0.3454(8) 0.2511(10) 0.028(3) Uani 0.691(14) 1 d D U . A 1
O2 O 0.5475(9) 0.5204(11) 0.2051(10) 0.039(3) Uani 0.691(14) 1 d D U . A 1
O3 O 0.5743(10) 0.4783(13) 0.4352(10) 0.029(2) Uani 0.691(14) 1 d D U . A 1
N1 N 0.4177(16) 0.572(2) 0.306(2) 0.031(3) Uani 0.691(14) 1 d D U . A 1
N2 N 0.5904(18) 0.7404(19) 0.513(3) 0.044(5) Uani 0.5 1 d D U . A 1
C1 C 0.3235(8) 0.6041(12) 0.2055(11) 0.039(3) Uani 0.691(14) 1 d . U . A 1
C2 C 0.3234(9) 0.7011(11) 0.1289(12) 0.043(3) Uani 0.691(14) 1 d G U . A 1
C3 C 0.2324(10) 0.7378(11) 0.0349(10) 0.046(4) Uani 0.691(14) 1 d G U . A 1
H3 H 0.2323 0.8041 -0.0175 0.055 Uiso 0.691(14) 1 calc R . . A 1
C4 C 0.1414(9) 0.6773(13) 0.0176(10) 0.046(4) Uani 0.691(14) 1 d G U . A 1
H4 H 0.0791 0.7024 -0.0466 0.055 Uiso 0.691(14) 1 calc R . . A 1
C5 C 0.1414(8) 0.5802(13) 0.0943(12) 0.044(4) Uani 0.691(14) 1 d G U . A 1
H5 H 0.0792 0.5389 0.0825 0.053 Uiso 0.691(14) 1 calc R . . A 1
C6 C 0.2325(9) 0.5436(11) 0.1883(12) 0.037(4) Uani 0.691(14) 1 d G U . A 1
C7 C 0.4188(16) 0.7709(18) 0.1482(17) 0.051(4) Uani 0.691(14) 1 d . U . A 1
H7A H 0.4444 0.8080 0.2311 0.076 Uiso 0.691(14) 1 calc GR . . A 1
H7B H 0.4038 0.8349 0.0850 0.076 Uiso 0.691(14) 1 calc GR . . A 1
H7C H 0.4709 0.7158 0.1413 0.076 Uiso 0.691(14) 1 calc GR . . A 1
C8 C 0.2327(17) 0.442(2) 0.2746(18) 0.046(4) Uani 0.691(14) 1 d . U . A 1
H8A H 0.2505 0.3656 0.2447 0.070 Uiso 0.691(14) 1 calc GR . . A 1
H8B H 0.1644 0.4350 0.2774 0.070 Uiso 0.691(14) 1 calc GR . . A 1
H8C H 0.2832 0.4597 0.3582 0.070 Uiso 0.691(14) 1 calc GR . . A 1
C9 C 0.4463(14) 0.2502(13) 0.3260(15) 0.046(4) Uani 0.691(14) 1 d D U . A 1
H9A H 0.4536 0.2842 0.4077 0.055 Uiso 0.691(14) 1 calc R . . A 1
H9B H 0.3754 0.2188 0.2852 0.055 Uiso 0.691(14) 1 calc R . . A 1
C10 C 0.5169(18) 0.1517(18) 0.345(2) 0.083(8) Uani 0.691(14) 1 d D U . A 1
H10A H 0.5326 0.1411 0.2705 0.125 Uiso 0.691(14) 1 calc GR . . A 1
H10B H 0.4863 0.0766 0.3609 0.125 Uiso 0.691(14) 1 calc GR . . A 1
H10C H 0.5803 0.1697 0.4164 0.125 Uiso 0.691(14) 1 calc GR . . A 1
C11 C 0.6315(15) 0.4550(17) 0.195(2) 0.073(6) Uani 0.691(14) 1 d D U . A 1
H11A H 0.6046 0.3914 0.1303 0.088 Uiso 0.691(14) 1 calc R . . A 1
H11B H 0.6703 0.4139 0.2751 0.088 Uiso 0.691(14) 1 calc R . . A 1
C12 C 0.6990(17) 0.5334(18) 0.164(2) 0.069(6) Uani 0.691(14) 1 d D U . A 1
H12A H 0.6595 0.5805 0.0893 0.103 Uiso 0.691(14) 1 calc GR . . A 1
H12B H 0.7506 0.4843 0.1478 0.103 Uiso 0.691(14) 1 calc GR . . A 1
H12C H 0.7333 0.5892 0.2332 0.103 Uiso 0.691(14) 1 calc GR . . A 1
C13 C 0.6926(19) 0.716(2) 0.513(3) 0.066(7) Uani 0.5 1 d D U . A 1
H13A H 0.7073 0.7748 0.4585 0.099 Uiso 0.5 1 calc GR . . A 1
H13B H 0.6950 0.6335 0.4835 0.099 Uiso 0.5 1 calc GR . . A 1
H13C H 0.7439 0.7251 0.5980 0.099 Uiso 0.5 1 calc GR . . A 1
C14 C 0.588(3) 0.8619(19) 0.563(3) 0.069(8) Uani 0.5 1 d D U . A 1
H14A H 0.6436 0.8691 0.6452 0.103 Uiso 0.5 1 calc GR . . A 1
H14B H 0.5220 0.8747 0.5703 0.103 Uiso 0.5 1 calc GR . . A 1
H14C H 0.5974 0.9234 0.5071 0.103 Uiso 0.5 1 calc GR . . A 1
Ti1 Ti 0.5000 0.6178(2) 0.5000 0.0299(6) Uani 1 2 d S TU P . .
C1A C 0.651(2) 0.617(3) 0.788(3) 0.039(3) Uani 0.309(14) 1 d . U . A 2
C2A C 0.6344(18) 0.714(3) 0.855(3) 0.043(3) Uani 0.309(14) 1 d G U . A 2
C3A C 0.717(2) 0.766(2) 0.951(2) 0.040(7) Uani 0.309(14) 1 d G U . A 2
H3A H 0.7056 0.8326 0.9966 0.048 Uiso 0.309(14) 1 calc R . . A 2
C4A C 0.8150(19) 0.720(3) 0.982(2) 0.044(9) Uani 0.309(14) 1 d G U . A 2
H4A H 0.8712 0.7550 1.0478 0.053 Uiso 0.309(14) 1 calc R . . A 2
C5A C 0.8312(19) 0.622(3) 0.915(3) 0.045(8) Uani 0.309(14) 1 d G U . A 2
H5A H 0.8984 0.5907 0.9360 0.054 Uiso 0.309(14) 1 calc R . . A 2
C6A C 0.749(3) 0.571(3) 0.819(3) 0.050(9) Uani 0.309(14) 1 d G U . A 2
C7A C 0.526(3) 0.766(3) 0.827(4) 0.040(8) Uani 0.309(14) 1 d . U . A 2
H7AA H 0.4776 0.7315 0.7486 0.060 Uiso 0.309(14) 1 calc GR . . A 2
H7AB H 0.5271 0.8548 0.8197 0.060 Uiso 0.309(14) 1 calc GR . . A 2
H7AC H 0.5041 0.7440 0.8945 0.060 Uiso 0.309(14) 1 calc GR . . A 2
C8A C 0.780(4) 0.469(5) 0.755(5) 0.046(4) Uani 0.309(14) 1 d . U . A 2
H8AA H 0.7284 0.4038 0.7345 0.070 Uiso 0.309(14) 1 calc GR . . A 2
H8AB H 0.8465 0.4361 0.8110 0.070 Uiso 0.309(14) 1 calc GR . . A 2
H8AC H 0.7857 0.4988 0.6790 0.070 Uiso 0.309(14) 1 calc GR . . A 2
P1A P 0.4896(16) 0.4523(16) 0.6691(16) 0.041(4) Uani 0.309(14) 1 d D U . A 2
C10A C 0.562(3) 0.119(3) 0.699(3) 0.051(9) Uani 0.309(14) 1 d D U . A 2
H10D H 0.6084 0.1124 0.7866 0.077 Uiso 0.309(14) 1 calc GR . . A 2
H10E H 0.6025 0.1335 0.6481 0.077 Uiso 0.309(14) 1 calc GR . . A 2
H10F H 0.5238 0.0425 0.6727 0.077 Uiso 0.309(14) 1 calc GR . . A 2
C9A C 0.492(2) 0.217(2) 0.684(3) 0.032(6) Uani 0.309(14) 1 d D U . A 2
H9AA H 0.4388 0.2175 0.5984 0.038 Uiso 0.309(14) 1 calc R . . A 2
H9AB H 0.4576 0.2092 0.7432 0.038 Uiso 0.309(14) 1 calc R . . A 2
O1A O 0.550(2) 0.3279(18) 0.707(2) 0.034(6) Uani 0.309(14) 1 d D U . A 2
C11A C 0.435(3) 0.445(3) 0.880(2) 0.048(8) Uani 0.309(14) 1 d D U . A 2
H11C H 0.5053 0.4655 0.9386 0.058 Uiso 0.309(14) 1 calc R . . A 2
H11D H 0.4221 0.3585 0.8936 0.058 Uiso 0.309(14) 1 calc R . . A 2
O2A O 0.428(2) 0.460(3) 0.757(2) 0.065(7) Uani 0.309(14) 1 d D U . A 2
C12A C 0.363(4) 0.520(5) 0.906(4) 0.084(16) Uani 0.309(14) 1 d D U . A 2
H12D H 0.3955 0.5556 0.9893 0.126 Uiso 0.309(14) 1 calc GR . . A 2
H12E H 0.3038 0.4707 0.9024 0.126 Uiso 0.309(14) 1 calc GR . . A 2
H12F H 0.3395 0.5855 0.8443 0.126 Uiso 0.309(14) 1 calc GR . . A 2
N2A N 0.377(2) 0.722(2) 0.496(3) 0.054(7) Uani 0.5 1 d D U . A 2
C14A C 0.341(2) 0.824(2) 0.410(2) 0.063(7) Uani 0.5 1 d D U . A 2
H14D H 0.3917 0.8431 0.3739 0.094 Uiso 0.5 1 calc GR . . A 2
H14E H 0.3315 0.8956 0.4550 0.094 Uiso 0.5 1 calc GR . . A 2
H14F H 0.2756 0.8030 0.3432 0.094 Uiso 0.5 1 calc GR . . A 2
C13A C 0.302(2) 0.690(3) 0.549(3) 0.090(12) Uani 0.5 1 d D U . A 2
H13D H 0.2831 0.6045 0.5330 0.135 Uiso 0.5 1 calc GR . . A 2
H13E H 0.2411 0.7415 0.5118 0.135 Uiso 0.5 1 calc GR . . A 2
H13F H 0.3323 0.7045 0.6393 0.135 Uiso 0.5 1 calc GR . . A 2
N1A N 0.563(4) 0.565(4) 0.690(6) 0.039(7) Uani 0.309(14) 1 d D U . A 2
O3A O 0.413(2) 0.456(3) 0.537(2) 0.029(2) Uani 0.309(14) 1 d D U . A 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'
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'
P P 0.1023 0.0942 '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
O1 P1 Ti1 134.9(5) . .
O2 P1 O1 100.7(6) . .
O2 P1 Ti1 124.4(5) . .
O3 P1 O1 112.6(7) . .
O3 P1 O2 114.9(7) . .
O3 P1 N1 100.9(11) . .
O3 P1 Ti1 50.1(6) . .
N1 P1 O1 117.7(11) . .
N1 P1 O2 110.7(12) . .
N1 P1 Ti1 50.9(9) . .
C9 O1 P1 123.8(10) . .
C11 O2 P1 120.0(12) . .
P1 O3 Ti1 97.3(7) . .
P1 N1 Ti1 94.7(10) . .
C1 N1 P1 126.4(18) . .
C1 N1 Ti1 138.9(12) . .
C13 N2 Ti1 121.8(16) . .
C14 N2 C13 110(2) . .
C14 N2 Ti1 126(2) . .
C2 C1 N1 118.9(13) . .
C2 C1 C6 120.0 . .
C6 C1 N1 121.0(13) . .
C1 C2 C3 120.0 . .
C1 C2 C7 121.3(9) . .
C3 C2 C7 118.7(9) . .
C2 C3 H3 120.0 . .
C4 C3 C2 120.0 . .
C4 C3 H3 120.0 . .
C3 C4 H4 120.0 . .
C5 C4 C3 120.0 . .
C5 C4 H4 120.0 . .
C4 C5 H5 120.0 . .
C6 C5 C4 120.0 . .
C6 C5 H5 120.0 . .
C1 C6 C8 119.6(11) . .
C5 C6 C1 120.0 . .
C5 C6 C8 120.4(11) . .
C2 C7 H7A 109.5 . .
C2 C7 H7B 109.5 . .
C2 C7 H7C 109.5 . .
H7A C7 H7B 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O1 C9 H9A 109.1 . .
O1 C9 H9B 109.1 . .
H9A C9 H9B 107.8 . .
C10 C9 O1 112.5(15) . .
C10 C9 H9A 109.1 . .
C10 C9 H9B 109.1 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10B 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O2 C11 H11A 109.2 . .
O2 C11 H11B 109.2 . .
O2 C11 C12 111.8(16) . .
H11A C11 H11B 107.9 . .
C12 C11 H11A 109.2 . .
C12 C11 H11B 109.2 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12B 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N2 C13 H13A 109.5 . .
N2 C13 H13B 109.5 . .
N2 C13 H13C 109.5 . .
H13A C13 H13B 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
N2 C14 H14A 109.5 . .
N2 C14 H14B 109.5 . .
N2 C14 H14C 109.5 . .
H14A C14 H14B 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
O3 Ti1 O3 89.2(7) 2_656 .
O3 Ti1 N1 67.0(4) . .
O3 Ti1 N1 67.0(4) 2_656 2_656
O3 Ti1 N1 93.5(8) 2_656 .
O3 Ti1 N1 93.5(8) . 2_656
N1 Ti1 N1 153.2(11) 2_656 .
N2 Ti1 O3 97.7(8) 2_656 2_656
N2 Ti1 O3 156.8(10) . 2_656
N2 Ti1 O3 156.8(10) 2_656 .
N2 Ti1 O3 97.7(8) . .
N2 Ti1 N1 90.4(10) . 2_656
N2 Ti1 N1 90.4(10) 2_656 .
N2 Ti1 N1 109.5(12) 2_656 2_656
N2 Ti1 N1 109.5(12) . .
N2 Ti1 N2 84.7(14) 2_656 .
N2A Ti1 N2A 112.7(16) . 2_656
N2A Ti1 N1A 101(2) . .
N2A Ti1 N1A 101(2) 2_656 2_656
N2A Ti1 N1A 96.4(12) 2_656 .
N2A Ti1 N1A 96.4(12) . 2_656
N2A Ti1 O3A 158.4(13) . 2_656
N2A Ti1 O3A 158.4(12) 2_656 .
N2A Ti1 O3A 85.9(11) 2_656 2_656
N2A Ti1 O3A 85.9(11) . .
N1A Ti1 N1A 148(3) 2_656 .
N1A Ti1 O3A 87(2) 2_656 .
N1A Ti1 O3A 68.4(8) . .
N1A Ti1 O3A 87(2) . 2_656
N1A Ti1 O3A 68.4(8) 2_656 2_656
O3A Ti1 O3A 78.3(18) 2_656 .
C2A C1A C6A 120.0 . .
C2A C1A N1A 118(3) . .
C6A C1A N1A 122(3) . .
C1A C2A C3A 120.0 . .
C1A C2A C7A 122(2) . .
C3A C2A C7A 118(2) . .
C2A C3A H3A 120.0 . .
C2A C3A C4A 120.0 . .
C4A C3A H3A 120.0 . .
C3A C4A H4A 120.0 . .
C5A C4A C3A 120.0 . .
C5A C4A H4A 120.0 . .
C4A C5A H5A 120.0 . .
C6A C5A C4A 120.0 . .
C6A C5A H5A 120.0 . .
C1A C6A C8A 127(3) . .
C5A C6A C1A 120.0 . .
C5A C6A C8A 113(3) . .
C2A C7A H7AA 109.5 . .
C2A C7A H7AB 109.5 . .
C2A C7A H7AC 109.5 . .
H7AA C7A H7AB 109.5 . .
H7AA C7A H7AC 109.5 . .
H7AB C7A H7AC 109.5 . .
C6A C8A H8AA 109.5 . .
C6A C8A H8AB 109.5 . .
C6A C8A H8AC 109.5 . .
H8AA C8A H8AB 109.5 . .
H8AA C8A H8AC 109.5 . .
H8AB C8A H8AC 109.5 . .
O1A P1A Ti1 127.2(14) . .
O2A P1A Ti1 128.9(15) . .
O2A P1A O1A 103.9(19) . .
N1A P1A Ti1 51(2) . .
N1A P1A O1A 113(3) . .
N1A P1A O2A 111(3) . .
O3A P1A Ti1 57.3(15) . .
O3A P1A O1A 113.9(18) . .
O3A P1A O2A 108(2) . .
O3A P1A N1A 108(3) . .
H10D C10A H10E 109.5 . .
H10D C10A H10F 109.5 . .
H10E C10A H10F 109.5 . .
C9A C10A H10D 109.5 . .
C9A C10A H10E 109.5 . .
C9A C10A H10F 109.5 . .
C10A C9A H9AA 110.2 . .
C10A C9A H9AB 110.2 . .
H9AA C9A H9AB 108.5 . .
O1A C9A C10A 108(3) . .
O1A C9A H9AA 110.2 . .
O1A C9A H9AB 110.2 . .
C9A O1A P1A 118(2) . .
H11C C11A H11D 107.9 . .
O2A C11A H11C 109.3 . .
O2A C11A H11D 109.2 . .
O2A C11A C12A 112(3) . .
C12A C11A H11C 109.3 . .
C12A C11A H11D 109.3 . .
C11A O2A P1A 145(3) . .
C11A C12A H12D 109.5 . .
C11A C12A H12E 109.5 . .
C11A C12A H12F 109.5 . .
H12D C12A H12E 109.5 . .
H12D C12A H12F 109.5 . .
H12E C12A H12F 109.5 . .
C14A N2A Ti1 121.0(18) . .
C14A N2A C13A 111(2) . .
C13A N2A Ti1 126.9(16) . .
N2A C14A H14D 109.5 . .
N2A C14A H14E 109.5 . .
N2A C14A H14F 109.5 . .
H14D C14A H14E 109.5 . .
H14D C14A H14F 109.5 . .
H14E C14A H14F 109.5 . .
N2A C13A H13D 109.5 . .
N2A C13A H13E 109.5 . .
N2A C13A H13F 109.5 . .
H13D C13A H13E 109.5 . .
H13D C13A H13F 109.5 . .
H13E C13A H13F 109.5 . .
C1A N1A Ti1 128(3) . .
C1A N1A P1A 138(4) . .
P1A N1A Ti1 94(3) . .
P1A O3A Ti1 89.3(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 O1 1.585(8) .
P1 O2 1.576(9) .
P1 O3 1.508(8) .
P1 N1 1.577(12) .
O1 C9 1.433(13) .
O2 C11 1.428(14) .
O3 Ti1 2.150(15) .
N1 C1 1.44(2) .
N1 Ti1 2.16(3) .
N2 C13 1.464(16) .
N2 C14 1.462(15) .
N2 Ti1 1.82(2) .
C1 C2 1.3900 .
C1 C6 1.3900 .
C2 C3 1.3900 .
C2 C7 1.49(2) .
C3 H3 0.9500 .
C3 C4 1.3900 .
C4 H4 0.9500 .
C4 C5 1.3900 .
C5 H5 0.9500 .
C5 C6 1.3900 .
C6 C8 1.500(19) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C9 C10 1.430(15) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C11 C12 1.432(16) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
Ti1 O3 2.150(16) 2_656
Ti1 N1 2.16(3) 2_656
Ti1 N2 1.82(2) 2_656
Ti1 N2A 2.06(3) .
Ti1 N2A 2.06(3) 2_656
Ti1 N1A 2.12(6) .
Ti1 N1A 2.12(6) 2_656
Ti1 O3A 2.29(4) 2_656
Ti1 O3A 2.29(4) .
C1A C2A 1.3900 .
C1A C6A 1.3900 .
C1A N1A 1.44(5) .
C2A C3A 1.3900 .
C2A C7A 1.55(4) .
C3A H3A 0.9500 .
C3A C4A 1.3900 .
C4A H4A 0.9500 .
C4A C5A 1.3900 .
C5A H5A 0.9500 .
C5A C6A 1.3900 .
C6A C8A 1.50(5) .
C7A H7AA 0.9800 .
C7A H7AB 0.9800 .
C7A H7AC 0.9800 .
C8A H8AA 0.9800 .
C8A H8AB 0.9800 .
C8A H8AC 0.9800 .
P1A O1A 1.578(13) .
P1A O2A 1.569(13) .
P1A N1A 1.575(16) .
P1A O3A 1.498(14) .
C10A H10D 0.9800 .
C10A H10E 0.9800 .
C10A H10F 0.9800 .
C10A C9A 1.434(18) .
C9A H9AA 0.9900 .
C9A H9AB 0.9900 .
C9A O1A 1.428(16) .
C11A H11C 0.9900 .
C11A H11D 0.9900 .
C11A O2A 1.416(16) .
C11A C12A 1.432(18) .
C12A H12D 0.9800 .
C12A H12E 0.9800 .
C12A H12F 0.9800 .
N2A C14A 1.461(15) .
N2A C13A 1.461(16) .
C14A H14D 0.9800 .
C14A H14E 0.9800 .
C14A H14F 0.9800 .
C13A H13D 0.9800 .
C13A H13E 0.9800 .
C13A H13F 0.9800 .
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
_geom_torsion_site_symmetry_4
P1 O1 C9 C10 -113.7(18) .
P1 O2 C11 C12 -147.2(16) .
P1 N1 C1 C2 -91(2) .
P1 N1 C1 C6 93(2) .
O1 P1 O2 C11 -61.2(15) .
O1 P1 O3 Ti1 -130.4(6) .
O1 P1 N1 C1 -53(3) .
O1 P1 N1 Ti1 126.9(8) .
O2 P1 O1 C9 157.1(13) .
O2 P1 O3 Ti1 115.1(7) .
O2 P1 N1 C1 62(2) .
O2 P1 N1 Ti1 -118.1(9) .
O3 P1 O1 C9 34.2(15) .
O3 P1 O2 C11 60.1(16) .
O3 P1 N1 C1 -176(2) .
O3 P1 N1 Ti1 4.0(12) .
N1 P1 O1 C9 -82.5(18) .
N1 P1 O2 C11 173.6(16) .
N1 P1 O3 Ti1 -4.0(12) .
N1 C1 C2 C3 -176.6(15) .
N1 C1 C2 C7 0.9(16) .
N1 C1 C6 C5 176.5(15) .
N1 C1 C6 C8 -1.1(17) .
C1 C2 C3 C4 0.0 .
C2 C1 C6 C5 0.0 .
C2 C1 C6 C8 -177.6(15) .
C2 C3 C4 C5 0.0 .
C3 C4 C5 C6 0.0 .
C4 C5 C6 C1 0.0 .
C4 C5 C6 C8 177.6(15) .
C6 C1 C2 C3 0.0 .
C6 C1 C2 C7 177.5(13) .
C7 C2 C3 C4 -177.6(13) .
C13 N2 Ti1 O3 -16(3) .
C13 N2 Ti1 O3 90(3) 2_656
C13 N2 Ti1 N1 -84(3) .
C13 N2 Ti1 N1 77(3) 2_656
C13 N2 Ti1 N2 -173(3) 2_656
C14 N2 Ti1 O3 -175(2) .
C14 N2 Ti1 O3 -69(4) 2_656
C14 N2 Ti1 N1 -81(3) 2_656
C14 N2 Ti1 N1 117(2) .
C14 N2 Ti1 N2 28.5(19) 2_656
Ti1 P1 O1 C9 -21.4(16) .
Ti1 P1 O2 C11 117.5(14) .
Ti1 P1 N1 C1 -180(3) .
Ti1 N1 C1 C2 90(3) .
Ti1 N1 C1 C6 -87(3) .
Ti1 P1A O1A C9A -118(2) .
Ti1 P1A O2A C11A -132(5) .
Ti1 P1A N1A C1A -173(9) .
C1A C2A C3A C4A 0.0 .
C2A C1A C6A C5A 0.0 .
C2A C1A C6A C8A -179(4) .
C2A C1A N1A Ti1 89(5) .
C2A C1A N1A P1A -100(7) .
C2A C3A C4A C5A 0.0 .
C3A C4A C5A C6A 0.0 .
C4A C5A C6A C1A 0.0 .
C4A C5A C6A C8A 179(3) .
C6A C1A C2A C3A 0.0 .
C6A C1A C2A C7A -178(3) .
C6A C1A N1A Ti1 -92(5) .
C6A C1A N1A P1A 79(8) .
C7A C2A C3A C4A 178(3) .
C10A C9A O1A P1A 167(2) .
O1A P1A O2A C11A 45(6) .
O1A P1A N1A Ti1 120(2) .
O1A P1A N1A C1A -53(8) .
O1A P1A O3A Ti1 -120.1(18) .
O2A P1A O1A C9A 65(3) .
O2A P1A N1A Ti1 -124(2) .
O2A P1A N1A C1A 63(8) .
O2A P1A O3A Ti1 125.3(18) .
C12A C11A O2A P1A 153(5) .
N1A C1A C2A C3A 179(4) .
N1A C1A C2A C7A 1(4) .
N1A C1A C6A C5A -179(4) .
N1A C1A C6A C8A 2(4) .
N1A P1A O1A C9A -175(4) .
N1A P1A O2A C11A -76(6) .
N1A P1A O3A Ti1 6(3) .
O3A P1A O1A C9A -52(3) .
O3A P1A O2A C11A 166(5) .
O3A P1A N1A Ti1 -6(3) .
O3A P1A N1A C1A -179(7) .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.86(11)
2 0.14(11)
