# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_9143
_database_code_depnum_ccdc_archive 'CCDC 1490138'
_audit_update_record             
;
2016-07-04 deposited with the CCDC.
2016-09-22 downloaded from the CCDC.
;

# Crystallographer: Patrick J. Carroll

# Compound 2

_audit_creation_date             2016-06-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_formula_moiety         'C88 H124 N6 P4 Ti2, 2(C6 H6)'
_chemical_formula_sum            'C100 H136 N6 P4 Ti2'
_chemical_formula_weight         1641.82

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   30.5846(16)
_cell_length_b                   15.6055(8)
_cell_length_c                   25.1965(13)
_cell_angle_alpha                90
_cell_angle_beta                 129.980(2)
_cell_angle_gamma                90
_cell_volume                     9215.1(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.43
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/4'
_exptl_crystal_color             orange
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       plank
_exptl_crystal_F_000             3528
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            118816
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.645
_diffrn_reflns_theta_min         1.547
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_number_gt                7336
_reflns_number_total             10690
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        'Bruker SAINT v8.34A'
_computing_molecular_graphics    'Mercury v3.6'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         10690
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0646
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0429P)²+40.8513P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1563
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct

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
Ti1 Ti 0.5000 0.75950(5) 0.7500 0.01996(18) Uani 1 2 d S T P . .
Ti2 Ti 0.5000 0.44454(5) 0.7500 0.01926(18) Uani 1 2 d S T P . .
P1 P 0.61044(3) 0.78134(5) 0.85951(4) 0.02216(18) Uani 1 1 d . . . . .
P2 P 0.57188(3) 0.42326(5) 0.72179(4) 0.02292(18) Uani 1 1 d . . . . .
N1 N 0.53329(10) 0.82051(15) 0.70808(14) 0.0233(6) Uani 1 1 d . . . . .
N2 N 0.57275(10) 0.38662(15) 0.83874(14) 0.0231(6) Uani 1 1 d . . . . .
N3 N 0.5000 0.5620(2) 0.7500 0.0182(7) Uani 1 2 d S T P . .
N4 N 0.5000 0.6421(2) 0.7500 0.0198(7) Uani 1 2 d S T P . .
C1 C 0.59129(12) 0.81555(18) 0.73851(17) 0.0239(7) Uani 1 1 d . . . . .
C2 C 0.61006(12) 0.83171(19) 0.70085(18) 0.0262(7) Uani 1 1 d . . . . .
H2 H 0.5834 0.8506 0.6542 0.035 Uiso 1 1 calc R . . . .
C3 C 0.66672(13) 0.8205(2) 0.73072(19) 0.0306(8) Uani 1 1 d . . . . .
H3 H 0.6778 0.8316 0.7037 0.041 Uiso 1 1 calc R . . . .
C4 C 0.70780(13) 0.7937(2) 0.79882(18) 0.0310(8) Uani 1 1 d . . . . .
C5 C 0.69029(12) 0.7813(2) 0.83724(17) 0.0267(7) Uani 1 1 d . . . . .
H5 H 0.7178 0.7644 0.8843 0.036 Uiso 1 1 calc R . . . .
C6 C 0.63353(12) 0.79271(19) 0.80898(17) 0.0243(7) Uani 1 1 d . . . . .
C7 C 0.76956(14) 0.7805(3) 0.8303(2) 0.0468(10) Uani 1 1 d . . . . .
H7a H 0.7917 0.8322 0.8557 0.070 Uiso 1 1 calc GR . . . .
H7b H 0.7712 0.7692 0.7933 0.070 Uiso 1 1 calc GR . . . .
H7c H 0.7856 0.7317 0.8621 0.070 Uiso 1 1 calc GR . . . .
C8 C 0.66111(12) 0.70146(19) 0.92622(16) 0.0233(7) Uani 1 1 d . . . . .
H8 H 0.7003 0.7225 0.9482 0.031 Uiso 1 1 calc R . . . .
C9 C 0.65404(13) 0.61547(19) 0.89268(18) 0.0283(7) Uani 1 1 d . . . . .
H9a H 0.6781 0.5725 0.9288 0.042 Uiso 1 1 calc GR . . . .
H9b H 0.6654 0.6212 0.8643 0.042 Uiso 1 1 calc GR . . . .
H9c H 0.6140 0.5975 0.8634 0.042 Uiso 1 1 calc GR . . . .
C10 C 0.65783(13) 0.6934(2) 0.98403(17) 0.0300(7) Uani 1 1 d . . . . .
H10a H 0.6206 0.6700 0.9650 0.045 Uiso 1 1 calc GR . . . .
H10b H 0.6628 0.7501 1.0040 0.045 Uiso 1 1 calc GR . . . .
H10c H 0.6881 0.6550 1.0201 0.045 Uiso 1 1 calc GR . . . .
C11 C 0.63348(12) 0.88280(19) 0.90981(18) 0.0296(8) Uani 1 1 d . . . . .
H11 H 0.6185 0.8822 0.9353 0.039 Uiso 1 1 calc R . . . .
C12 C 0.60627(14) 0.9581(2) 0.8602(2) 0.0407(9) Uani 1 1 d . . . . .
H12a H 0.6127 1.0106 0.8858 0.061 Uiso 1 1 calc GR . . . .
H12b H 0.5652 0.9481 0.8246 0.061 Uiso 1 1 calc GR . . . .
H12c H 0.6233 0.9644 0.8383 0.061 Uiso 1 1 calc GR . . . .
C13 C 0.69837(13) 0.8963(2) 0.9635(2) 0.0374(9) Uani 1 1 d . . . . .
H13a H 0.7146 0.8943 0.9404 0.056 Uiso 1 1 calc GR . . . .
H13b H 0.7154 0.8509 0.9986 0.056 Uiso 1 1 calc GR . . . .
H13c H 0.7064 0.9521 0.9859 0.056 Uiso 1 1 calc GR . . . .
C14 C 0.49795(12) 0.85207(19) 0.63791(18) 0.0266(7) Uani 1 1 d . . . . .
C15 C 0.47154(12) 0.7943(2) 0.58207(18) 0.0267(7) Uani 1 1 d . . . . .
C16 C 0.43888(13) 0.8250(2) 0.51446(19) 0.0323(8) Uani 1 1 d . . . . .
H16 H 0.4200 0.7850 0.4774 0.043 Uiso 1 1 calc R . . . .
C17 C 0.43303(14) 0.9118(2) 0.4994(2) 0.0371(9) Uani 1 1 d . . . . .
C18 C 0.46130(14) 0.9676(2) 0.5550(2) 0.0391(9) Uani 1 1 d . . . . .
H18 H 0.4585 1.0273 0.5459 0.052 Uiso 1 1 calc R . . . .
C19 C 0.49399(13) 0.9406(2) 0.6240(2) 0.0341(8) Uani 1 1 d . . . . .
C20 C 0.48382(13) 0.70071(19) 0.59597(17) 0.0279(7) Uani 1 1 d . . . . .
H20a H 0.4628 0.6698 0.5519 0.042 Uiso 1 1 calc GR . . . .
H20b H 0.4719 0.6800 0.6217 0.042 Uiso 1 1 calc GR . . . .
H20c H 0.5248 0.6909 0.6234 0.042 Uiso 1 1 calc GR . . . .
C21 C 0.40001(18) 0.9439(3) 0.4261(2) 0.0517(11) Uani 1 1 d . . . . .
H21a H 0.3994 1.0067 0.4258 0.078 Uiso 1 1 calc GR . . . .
H21b H 0.3608 0.9220 0.3971 0.078 Uiso 1 1 calc GR . . . .
H21c H 0.4184 0.9237 0.4078 0.078 Uiso 1 1 calc GR . . . .
C22 C 0.52709(14) 1.0046(2) 0.6817(2) 0.0421(10) Uani 1 1 d . . . . .
H22a H 0.5678 0.9988 0.7055 0.063 Uiso 1 1 calc GR . . . .
H22b H 0.5207 0.9942 0.7146 0.063 Uiso 1 1 calc GR . . . .
H22c H 0.5144 1.0626 0.6627 0.063 Uiso 1 1 calc GR . . . .
C23 C 0.62793(12) 0.38915(18) 0.85933(17) 0.0235(7) Uani 1 1 d . . . . .
C24 C 0.67737(13) 0.3710(2) 0.92814(18) 0.0285(7) Uani 1 1 d . . . . .
H24 H 0.6736 0.3544 0.9613 0.038 Uiso 1 1 calc R . . . .
C25 C 0.73137(13) 0.3771(2) 0.94774(18) 0.0306(8) Uani 1 1 d . . . . .
H25 H 0.7638 0.3642 0.9942 0.041 Uiso 1 1 calc R . . . .
C26 C 0.73954(13) 0.4014(2) 0.90172(18) 0.0296(7) Uani 1 1 d . . . . .
C27 C 0.69118(13) 0.41757(19) 0.83424(18) 0.0268(7) Uani 1 1 d . . . . .
H27 H 0.6956 0.4337 0.8016 0.036 Uiso 1 1 calc R . . . .
C28 C 0.63588(12) 0.41114(18) 0.81191(17) 0.0233(7) Uani 1 1 d . . . . .
C29 C 0.79895(14) 0.4089(3) 0.9246(2) 0.0416(9) Uani 1 1 d . . . . .
H29a H 0.8177 0.4603 0.9532 0.062 Uiso 1 1 calc GR . . . .
H29b H 0.7963 0.4130 0.8838 0.062 Uiso 1 1 calc GR . . . .
H29c H 0.8213 0.3581 0.9517 0.062 Uiso 1 1 calc GR . . . .
C30 C 0.59128(16) 0.5050(3) 0.68699(19) 0.0429(9) Uani 1 1 d . . . . .
H30 H 0.6262 0.4820 0.6963 0.057 Uiso 1 1 calc R . . . .
C31 C 0.60918(17) 0.5865(2) 0.7246(2) 0.0463(10) Uani 1 1 d . . . . .
H31a H 0.6173 0.6280 0.7027 0.069 Uiso 1 1 calc GR . . . .
H31b H 0.6436 0.5775 0.7728 0.069 Uiso 1 1 calc GR . . . .
H31c H 0.5786 0.6087 0.7234 0.069 Uiso 1 1 calc GR . . . .
C32 C 0.54660(14) 0.5115(2) 0.60844(18) 0.0321(8) Uani 1 1 d . . . . .
H32a H 0.5100 0.5290 0.5953 0.048 Uiso 1 1 calc GR . . . .
H32b H 0.5422 0.4556 0.5878 0.048 Uiso 1 1 calc GR . . . .
H32c H 0.5588 0.5540 0.5916 0.048 Uiso 1 1 calc GR . . . .
C33 C 0.57051(14) 0.3247(2) 0.6790(2) 0.0354(8) Uani 1 1 d . . . . .
H33 H 0.5333 0.3245 0.6306 0.047 Uiso 1 1 calc R . . . .
C34 C 0.57163(15) 0.2456(2) 0.7146(2) 0.0435(10) Uani 1 1 d . . . . .
H34a H 0.5675 0.1944 0.6891 0.065 Uiso 1 1 calc GR . . . .
H34b H 0.5402 0.2481 0.7156 0.065 Uiso 1 1 calc GR . . . .
H34c H 0.6080 0.2429 0.7621 0.065 Uiso 1 1 calc GR . . . .
C35 C 0.61812(16) 0.3162(3) 0.6742(2) 0.0479(10) Uani 1 1 d . . . . .
H35a H 0.6554 0.3160 0.7209 0.072 Uiso 1 1 calc GR . . . .
H35b H 0.6161 0.3646 0.6480 0.072 Uiso 1 1 calc GR . . . .
H35c H 0.6131 0.2625 0.6507 0.072 Uiso 1 1 calc GR . . . .
C36 C 0.57251(12) 0.34978(19) 0.89082(17) 0.0251(7) Uani 1 1 d . . . . .
C37 C 0.57841(13) 0.4012(2) 0.94057(17) 0.0268(7) Uani 1 1 d . . . . .
C38 C 0.57855(14) 0.3637(2) 0.99075(19) 0.0345(8) Uani 1 1 d . . . . .
H38 H 0.5820 0.3994 1.0238 0.046 Uiso 1 1 calc R . . . .
C39 C 0.57380(14) 0.2761(2) 0.9939(2) 0.0393(9) Uani 1 1 d . . . . .
C40 C 0.57113(13) 0.2259(2) 0.9467(2) 0.0382(9) Uani 1 1 d . . . . .
H40 H 0.5693 0.1654 0.9492 0.051 Uiso 1 1 calc R . . . .
C41 C 0.57103(13) 0.2601(2) 0.89590(19) 0.0323(8) Uani 1 1 d . . . . .
C42 C 0.59083(15) 0.4954(2) 0.94479(19) 0.0331(8) Uani 1 1 d . . . . .
H42a H 0.5894 0.5226 0.9787 0.050 Uiso 1 1 calc GR . . . .
H42b H 0.5623 0.5218 0.8993 0.050 Uiso 1 1 calc GR . . . .
H42c H 0.6289 0.5032 0.9591 0.050 Uiso 1 1 calc GR . . . .
C43 C 0.57402(17) 0.2363(3) 1.0483(2) 0.0530(11) Uani 1 1 d . . . . .
H43a H 0.5928 0.2750 1.0881 0.080 Uiso 1 1 calc GR . . . .
H43b H 0.5947 0.1818 1.0632 0.080 Uiso 1 1 calc GR . . . .
H43c H 0.5347 0.2260 1.0291 0.080 Uiso 1 1 calc GR . . . .
C44 C 0.57267(16) 0.2012(2) 0.8503(2) 0.0443(10) Uani 1 1 d . . . . .
H44a H 0.5654 0.1423 0.8563 0.066 Uiso 1 1 calc GR . . . .
H44b H 0.6103 0.2044 0.8628 0.066 Uiso 1 1 calc GR . . . .
H44c H 0.5434 0.2184 0.8018 0.066 Uiso 1 1 calc GR . . . .
C45 C 0.7180(2) 0.02396(18) 0.8249(2) 0.097(2) Uani 1 1 d . . . . .
H45 H 0.7000 -0.0294 0.8180 0.129 Uiso 1 1 calc R . . . .
C46 C 0.71519(18) 0.0899(2) 0.8600(2) 0.090(2) Uani 1 1 d G . . . .
H46 H 0.6954 0.0814 0.8771 0.120 Uiso 1 1 calc R . . . .
C47 C 0.74152(16) 0.16830(17) 0.87018(19) 0.0679(14) Uani 1 1 d G . . . .
H47 H 0.7396 0.2132 0.8941 0.090 Uiso 1 1 calc R . . . .
C48 C 0.77063(16) 0.18075(19) 0.8452(2) 0.0779(16) Uani 1 1 d G . . . .
H48 H 0.7886 0.2341 0.8521 0.104 Uiso 1 1 calc R . . . .
C49 C 0.77340(17) 0.1148(3) 0.8101(2) 0.0893(19) Uani 1 1 d G . . . .
H49 H 0.7932 0.1233 0.7931 0.119 Uiso 1 1 calc R . . . .
C50 C 0.7471(2) 0.0364(2) 0.8000(2) 0.104(2) Uani 1 1 d G . . . .
H50 H 0.7490 -0.0085 0.7760 0.138 Uiso 1 1 calc R . . . .


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 P1 2.6763(7) 2_656 ?
Ti1 P1 2.6763(8) . ?
Ti1 N1 2.107(3) 2_656 ?
Ti1 N1 2.107(3) . ?
Ti1 N4 1.832(3) . ?
Ti2 P2 2.7306(8) 2_656 ?
Ti2 P2 2.7306(8) . ?
Ti2 N2 2.091(2) 2_656 ?
Ti2 N2 2.091(2) . ?
Ti2 N3 1.833(3) . ?
P1 C6 1.818(3) . ?
P1 C8 1.853(3) . ?
P1 C11 1.861(3) . ?
P2 C28 1.820(3) . ?
P2 C30 1.848(4) . ?
P2 C33 1.862(3) . ?
N1 C1 1.412(3) . ?
N1 C14 1.442(4) . ?
N2 C23 1.412(3) . ?
N2 C36 1.437(4) . ?
N3 N4 1.250(4) . ?
C1 C2 1.412(5) . ?
C1 C6 1.415(5) . ?
C2 C3 1.387(4) . ?
C3 C4 1.388(5) . ?
C4 C5 1.388(5) . ?
C4 C7 1.521(4) . ?
C5 C6 1.402(4) . ?
C8 C9 1.525(4) . ?
C8 C10 1.528(5) . ?
C11 C12 1.517(5) . ?
C11 C13 1.537(4) . ?
C14 C15 1.408(5) . ?
C14 C19 1.411(4) . ?
C15 C16 1.393(5) . ?
C15 C20 1.493(4) . ?
C16 C17 1.388(5) . ?
C17 C18 1.381(5) . ?
C17 C21 1.512(5) . ?
C18 C19 1.403(5) . ?
C19 C22 1.498(5) . ?
C23 C24 1.416(4) . ?
C23 C28 1.407(4) . ?
C24 C25 1.390(4) . ?
C25 C26 1.387(5) . ?
C26 C27 1.382(5) . ?
C26 C29 1.517(4) . ?
C27 C28 1.401(4) . ?
C30 C31 1.466(5) . ?
C30 C32 1.523(5) . ?
C33 C34 1.514(5) . ?
C33 C35 1.543(5) . ?
C36 C37 1.399(5) . ?
C36 C41 1.409(4) . ?
C37 C38 1.391(5) . ?
C37 C42 1.505(5) . ?
C38 C39 1.382(5) . ?
C39 C40 1.383(6) . ?
C39 C43 1.500(5) . ?
C40 C41 1.385(5) . ?
C41 C44 1.498(5) . ?
C45 C46 1.3951 . ?
C45 C50 1.3948 . ?
C46 C47 1.3952 . ?
C47 C48 1.3948 . ?
C48 C49 1.3950 . ?
C49 C50 1.3949 . ?

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
P1 Ti1 P1 165.37(4) . 2_656 ?
N1 Ti1 P1 76.29(7) . . ?
N1 Ti1 P1 76.30(7) 2_656 2_656 ?
N1 Ti1 P1 97.00(7) . 2_656 ?
N1 Ti1 P1 97.00(7) 2_656 . ?
N1 Ti1 N1 126.29(14) . 2_656 ?
N4 Ti1 P1 97.31(2) . . ?
N4 Ti1 P1 97.31(2) . 2_656 ?
N4 Ti1 N1 116.86(7) . 2_656 ?
N4 Ti1 N1 116.86(7) . . ?
P2 Ti2 P2 166.03(4) 2_656 . ?
N2 Ti2 P2 98.67(7) 2_656 . ?
N2 Ti2 P2 98.66(7) . 2_656 ?
N2 Ti2 P2 75.18(7) 2_656 2_656 ?
N2 Ti2 P2 75.18(7) . . ?
N2 Ti2 N2 128.79(14) . 2_656 ?
N3 Ti2 P2 96.99(2) . . ?
N3 Ti2 P2 96.99(2) . 2_656 ?
N3 Ti2 N2 115.61(7) . . ?
N3 Ti2 N2 115.61(7) . 2_656 ?
C6 P1 Ti1 95.23(10) . . ?
C6 P1 C8 103.08(14) . . ?
C6 P1 C11 104.27(15) . . ?
C8 P1 Ti1 127.99(10) . . ?
C8 P1 C11 102.98(14) . . ?
C11 P1 Ti1 119.03(10) . . ?
C28 P2 Ti2 95.07(10) . . ?
C28 P2 C30 104.35(15) . . ?
C28 P2 C33 104.02(15) . . ?
C30 P2 Ti2 126.66(14) . . ?
C30 P2 C33 100.95(18) . . ?
C33 P2 Ti2 121.90(11) . . ?
C1 N1 Ti1 123.1(2) . . ?
C1 N1 C14 112.0(2) . . ?
C14 N1 Ti1 123.08(17) . . ?
C23 N2 Ti2 125.5(2) . . ?
C23 N2 C36 112.4(2) . . ?
C36 N2 Ti2 121.53(17) . . ?
N4 N3 Ti2 180.0 . . ?
N3 N4 Ti1 180.0 . . ?
N1 C1 C2 122.5(3) . . ?
N1 C1 C6 120.7(3) . . ?
C2 C1 C6 116.8(3) . . ?
C3 C2 C1 121.2(3) . . ?
C2 C3 C4 122.1(3) . . ?
C3 C4 C7 121.3(3) . . ?
C5 C4 C3 117.1(3) . . ?
C5 C4 C7 121.6(3) . . ?
C4 C5 C6 122.3(3) . . ?
C1 C6 P1 116.8(2) . . ?
C5 C6 P1 122.9(3) . . ?
C5 C6 C1 120.2(3) . . ?
C9 C8 P1 110.5(2) . . ?
C9 C8 C10 112.5(3) . . ?
C10 C8 P1 113.0(2) . . ?
C12 C11 P1 109.3(2) . . ?
C12 C11 C13 109.5(3) . . ?
C13 C11 P1 115.2(2) . . ?
C15 C14 N1 120.2(3) . . ?
C15 C14 C19 118.4(3) . . ?
C19 C14 N1 121.0(3) . . ?
C14 C15 C20 119.7(3) . . ?
C16 C15 C14 120.2(3) . . ?
C16 C15 C20 119.8(3) . . ?
C17 C16 C15 122.3(3) . . ?
C16 C17 C21 121.6(4) . . ?
C18 C17 C16 116.8(3) . . ?
C18 C17 C21 121.5(3) . . ?
C17 C18 C19 123.5(3) . . ?
C14 C19 C22 121.0(3) . . ?
C18 C19 C14 118.7(3) . . ?
C18 C19 C22 120.2(3) . . ?
N2 C23 C24 121.9(3) . . ?
C28 C23 N2 120.9(3) . . ?
C28 C23 C24 117.2(3) . . ?
C25 C24 C23 120.8(3) . . ?
C26 C25 C24 122.2(3) . . ?
C25 C26 C29 121.2(3) . . ?
C27 C26 C25 116.9(3) . . ?
C27 C26 C29 121.9(3) . . ?
C26 C27 C28 122.8(3) . . ?
C23 C28 P2 116.8(2) . . ?
C27 C28 P2 123.1(3) . . ?
C27 C28 C23 119.9(3) . . ?
C31 C30 P2 113.1(3) . . ?
C31 C30 C32 115.6(3) . . ?
C32 C30 P2 111.6(2) . . ?
C34 C33 P2 110.4(3) . . ?
C34 C33 C35 108.2(3) . . ?
C35 C33 P2 116.5(3) . . ?
C37 C36 N2 121.0(3) . . ?
C37 C36 C41 118.8(3) . . ?
C41 C36 N2 120.0(3) . . ?
C36 C37 C42 120.3(3) . . ?
C38 C37 C36 119.8(3) . . ?
C38 C37 C42 119.6(3) . . ?
C39 C38 C37 122.0(4) . . ?
C38 C39 C40 117.4(3) . . ?
C38 C39 C43 121.6(4) . . ?
C40 C39 C43 120.9(4) . . ?
C39 C40 C41 122.8(3) . . ?
C36 C41 C44 121.4(3) . . ?
C40 C41 C36 119.0(3) . . ?
C40 C41 C44 119.5(3) . . ?
C50 C45 C46 120.0 . . ?
C45 C46 C47 120.0 . . ?
C48 C47 C46 120.0 . . ?
C47 C48 C49 120.0 . . ?
C50 C49 C48 120.0 . . ?
C45 C50 C49 120.0 . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_9152
_database_code_depnum_ccdc_archive 'CCDC 1490139'
_audit_update_record             
;
2016-07-04 deposited with the CCDC.
2016-09-22 downloaded from the CCDC.
;

# Crystallographer: Patrick J. Carroll

# Compound 5

_audit_creation_date             2016-06-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_formula_moiety         '2(C50 H76 N3 P3 Ti), 2(C5 H12)'
_chemical_formula_sum            'C110 H176 N6 P6 Ti2'
_chemical_formula_weight         1864.18

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   18.5929(8)
_cell_length_b                   12.9042(5)
_cell_length_c                   22.7421(14)
_cell_angle_alpha                90
_cell_angle_beta                 98.499(2)
_cell_angle_gamma                90
_cell_volume                     5396.5(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9815
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.22
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/4'
_exptl_crystal_color             red
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       prism
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            84659
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.590
_diffrn_reflns_theta_min         1.811
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_number_gt                5325
_reflns_number_total             6146
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        'Bruker SAINT v8.34A'
_computing_molecular_graphics    'Mercury v3.6'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         1.262
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6146
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0662
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1013P)²+16.4956P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1786
_refine_ls_wR_factor_ref         0.1890
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct

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
Ti1 Ti 0.2500 0.24079(4) 0.5000 0.01619(16) Uani 1 2 d S T P . .
P1 P 0.10610(3) 0.25694(4) 0.45990(3) 0.01867(16) Uani 1 1 d . . . . .
P2 P 0.26882(8) -0.02285(11) 0.51988(7) 0.0344(3) Uani 0.5 1 d . . . . .
N1 N 0.20758(9) 0.30854(14) 0.56988(8) 0.0173(4) Uani 1 1 d . . . . .
N2 N 0.2500 0.1049(2) 0.5000 0.0280(6) Uani 1 2 d S T P A .
C1 C 0.13539(11) 0.29916(17) 0.58000(10) 0.0191(4) Uani 1 1 d . . . . .
C2 C 0.11349(13) 0.32258(19) 0.63524(10) 0.0246(5) Uani 1 1 d . . . . .
H2 H 0.1472 0.3498 0.6656 0.033 Uiso 1 1 calc R . . . .
C3 C 0.04241(14) 0.3057(2) 0.64508(11) 0.0287(5) Uani 1 1 d . . . . .
H3 H 0.0297 0.3221 0.6820 0.038 Uiso 1 1 calc R . . . .
C4 C -0.01018(13) 0.26518(19) 0.60167(12) 0.0280(5) Uani 1 1 d . . . . .
C5 C 0.00988(13) 0.24734(18) 0.54617(12) 0.0246(5) Uani 1 1 d . . . . .
H5 H -0.0249 0.2226 0.5158 0.033 Uiso 1 1 calc R . . . .
C6 C 0.08050(12) 0.26520(17) 0.53408(10) 0.0197(4) Uani 1 1 d . . . . .
C7 C -0.08644(16) 0.2437(2) 0.61365(15) 0.0395(7) Uani 1 1 d . . . . .
H7a H -0.1192 0.2933 0.5928 0.059 Uiso 1 1 calc GR . . . .
H7b H -0.0880 0.2489 0.6555 0.059 Uiso 1 1 calc GR . . . .
H7c H -0.1006 0.1751 0.6002 0.059 Uiso 1 1 calc GR . . . .
C8 C 0.04496(15) 0.1574(2) 0.42090(13) 0.0372(6) Uani 1 1 d . . . . .
H8 H -0.0045 0.1754 0.4273 0.049 Uiso 1 1 calc R . . . .
C9 C 0.0596(3) 0.0514(3) 0.4451(2) 0.0685(12) Uani 1 1 d . . . . .
H9a H 0.0204 0.0062 0.4293 0.103 Uiso 1 1 calc GR . . . .
H9b H 0.0635 0.0532 0.4877 0.103 Uiso 1 1 calc GR . . . .
H9c H 0.1043 0.0262 0.4341 0.103 Uiso 1 1 calc GR . . . .
C10 C 0.04479(17) 0.1570(3) 0.35310(14) 0.0477(8) Uani 1 1 d . . . . .
H10a H 0.0910 0.1329 0.3446 0.072 Uiso 1 1 calc GR . . . .
H10b H 0.0362 0.2259 0.3378 0.072 Uiso 1 1 calc GR . . . .
H10c H 0.0071 0.1118 0.3346 0.072 Uiso 1 1 calc GR . . . .
C11 C 0.06678(13) 0.3777(2) 0.42312(10) 0.0262(5) Uani 1 1 d . . . . .
H11 H 0.0835 0.3820 0.3843 0.035 Uiso 1 1 calc R . . . .
C12 C 0.09745(16) 0.4715(2) 0.45912(12) 0.0319(6) Uani 1 1 d . . . . .
H12a H 0.0814 0.5338 0.4381 0.048 Uiso 1 1 calc GR . . . .
H12b H 0.1496 0.4687 0.4649 0.048 Uiso 1 1 calc GR . . . .
H12c H 0.0807 0.4711 0.4971 0.048 Uiso 1 1 calc GR . . . .
C13 C -0.01630(15) 0.3842(3) 0.41206(14) 0.0399(7) Uani 1 1 d . . . . .
H13a H -0.0348 0.3769 0.4491 0.060 Uiso 1 1 calc GR . . . .
H13b H -0.0354 0.3298 0.3855 0.060 Uiso 1 1 calc GR . . . .
H13c H -0.0309 0.4501 0.3947 0.060 Uiso 1 1 calc GR . . . .
C14 C 0.25625(11) 0.34618(17) 0.62070(9) 0.0185(4) Uani 1 1 d . . . . .
C15 C 0.28818(12) 0.27609(19) 0.66451(10) 0.0221(4) Uani 1 1 d . . . . .
C16 C 0.33678(13) 0.3135(2) 0.71251(10) 0.0272(5) Uani 1 1 d . . . . .
H16 H 0.3583 0.2671 0.7411 0.036 Uiso 1 1 calc R . . . .
C17 C 0.35385(13) 0.4181(2) 0.71870(10) 0.0291(5) Uani 1 1 d . . . . .
C18 C 0.31879(14) 0.4866(2) 0.67704(11) 0.0274(5) Uani 1 1 d . . . . .
H18 H 0.3284 0.5571 0.6815 0.036 Uiso 1 1 calc R . . . .
C19 C 0.26946(12) 0.45268(18) 0.62848(10) 0.0220(4) Uani 1 1 d . . . . .
C20 C 0.26724(14) 0.16361(19) 0.66156(11) 0.0270(5) Uani 1 1 d . . . . .
H20a H 0.2924 0.1281 0.6956 0.040 Uiso 1 1 calc GR . . . .
H20b H 0.2802 0.1335 0.6260 0.040 Uiso 1 1 calc GR . . . .
H20c H 0.2157 0.1574 0.6612 0.040 Uiso 1 1 calc GR . . . .
C21 C 0.40940(17) 0.4563(3) 0.76950(13) 0.0420(7) Uani 1 1 d . . . . .
H21a H 0.4570 0.4538 0.7580 0.063 Uiso 1 1 calc GR . . . .
H21b H 0.4082 0.4130 0.8037 0.063 Uiso 1 1 calc GR . . . .
H21c H 0.3982 0.5264 0.7791 0.063 Uiso 1 1 calc GR . . . .
C22 C 0.22853(15) 0.53135(19) 0.58755(11) 0.0293(5) Uani 1 1 d . . . . .
H22a H 0.1776 0.5268 0.5902 0.044 Uiso 1 1 calc GR . . . .
H22b H 0.2361 0.5178 0.5474 0.044 Uiso 1 1 calc GR . . . .
H22c H 0.2458 0.5996 0.5989 0.044 Uiso 1 1 calc GR . . . .
C23 C 0.1838(4) -0.0858(4) 0.5370(3) 0.0426(14) Uani 0.5 1 d D . . A 1
H23 H 0.1475 -0.0911 0.5012 0.057 Uiso 0.5 1 calc R . . A 1
C23' C 0.2235(4) -0.0732(4) 0.5568(3) 0.0432(14) Uani 0.5 1 d D . . A 2
H23' H 0.2684 -0.0572 0.5836 0.057 Uiso 0.5 1 calc R . . A 2
C24 C 0.15654(19) -0.0226(3) 0.58245(17) 0.0531(8) Uani 1 1 d D . . . .
H24a H 0.1420 0.0441 0.5661 0.080 Uiso 0.5 1 calc R . . A 1
H24b H 0.1155 -0.0565 0.5952 0.080 Uiso 0.5 1 calc R . . A 1
H24c H 0.1942 -0.0141 0.6158 0.080 Uiso 0.5 1 calc R . . A 1
H24x H 0.1611 0.0515 0.5823 0.080 Uiso 0.5 1 calc R . . A 2
H24y H 0.1120 -0.0425 0.5581 0.080 Uiso 0.5 1 calc R . . A 2
H24z H 0.1560 -0.0463 0.6224 0.080 Uiso 0.5 1 calc R . . A 2
C25 C 0.2076(2) -0.1921(3) 0.5601(2) 0.0670(11) Uani 1 1 d D . . . .
H25a H 0.2251 -0.2311 0.5292 0.100 Uiso 0.5 1 calc R . . A 1
H25b H 0.2458 -0.1852 0.5933 0.100 Uiso 0.5 1 calc R . . A 1
H25c H 0.1671 -0.2276 0.5727 0.100 Uiso 0.5 1 calc R . . A 1
H25x H 0.2455 -0.2303 0.5454 0.100 Uiso 0.5 1 calc R . . A 2
H25y H 0.2058 -0.2114 0.6007 0.100 Uiso 0.5 1 calc R . . A 2
H25z H 0.1618 -0.2075 0.5363 0.100 Uiso 0.5 1 calc R . . A 2
C26 C 0.1418(5) 0.6063(10) 0.7430(5) 0.114(5) Uani 0.5 1 d . U . B -1
H26a H 0.1310 0.5425 0.7616 0.171 Uiso 0.5 1 calc R . . B -1
H26b H 0.1050 0.6567 0.7476 0.171 Uiso 0.5 1 calc R . . B -1
H26c H 0.1428 0.5945 0.7015 0.171 Uiso 0.5 1 calc R . . B -1
C27 C 0.2159(4) 0.6466(7) 0.7723(3) 0.096(3) Uani 0.5 1 d G U . B -1
H27a H 0.2526 0.5946 0.7683 0.128 Uiso 0.5 1 calc R . . B -1
H27b H 0.2147 0.6567 0.8144 0.128 Uiso 0.5 1 calc R . . B -1
C28 C 0.2380(5) 0.7487(8) 0.7455(5) 0.102(4) Uani 0.5 1 d G U . B -1
H28a H 0.2391 0.7385 0.7033 0.136 Uiso 0.5 1 calc R . . B -1
H28b H 0.2012 0.8006 0.7494 0.136 Uiso 0.5 1 calc R . . B -1
C29 C 0.3122(4) 0.7900(7) 0.7744(3) 0.105(4) Uani 0.5 1 d G U . B -1
H29a H 0.3112 0.8004 0.8165 0.139 Uiso 0.5 1 calc R . . B -1
H29b H 0.3490 0.7383 0.7704 0.139 Uiso 0.5 1 calc R . . B -1
C30 C 0.3335(6) 0.8919(8) 0.7471(6) 0.125(6) Uani 0.5 1 d G U . B -1
H30a H 0.3802 0.9138 0.7670 0.187 Uiso 0.5 1 calc R . . B -1
H30b H 0.3358 0.8819 0.7056 0.187 Uiso 0.5 1 calc R . . B -1
H30c H 0.2979 0.9440 0.7518 0.187 Uiso 0.5 1 calc R . . B -1


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 P1 2.7040(6) 2_556 ?
Ti1 P1 2.7041(6) . ?
Ti1 N1 2.0695(18) . ?
Ti1 N1 2.0695(18) 2_556 ?
Ti1 N2 1.753(3) . ?
P1 C6 1.822(2) . ?
P1 C8 1.852(3) . ?
P1 C11 1.866(2) . ?
P2 N2 1.732(3) . ?
P2 C23 1.868(7) . ?
P2 C23' 1.887(7) 2_556 ?
N1 C1 1.400(3) . ?
N1 C14 1.443(3) . ?
N2 P2 1.732(3) 2_556 ?
C1 C2 1.410(3) . ?
C1 C6 1.417(3) . ?
C2 C3 1.390(3) . ?
C3 C4 1.385(4) . ?
C4 C5 1.387(4) . ?
C4 C7 1.509(3) . ?
C5 C6 1.400(3) . ?
C8 C9 1.485(5) . ?
C8 C10 1.541(4) . ?
C11 C12 1.524(4) . ?
C11 C13 1.530(3) . ?
C14 C15 1.410(3) . ?
C14 C19 1.403(3) . ?
C15 C16 1.396(3) . ?
C15 C20 1.502(3) . ?
C16 C17 1.388(4) . ?
C17 C18 1.386(4) . ?
C17 C21 1.514(3) . ?
C18 C19 1.397(3) . ?
C19 C22 1.506(3) . ?
C23 C24 1.466(6) . ?
C23 C25 1.512(6) . ?
C23' P2 1.887(7) 2_556 ?
C23' C24 1.591(6) . ?
C23' C25 1.566(6) . ?
C26 C27 1.5310 . ?
C27 C28 1.5331 . ?
C28 C29 1.5331 . ?
C29 C30 1.5310 . ?

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
P1 Ti1 P1 171.16(3) 2_556 . ?
N1 Ti1 P1 75.88(5) 2_556 2_556 ?
N1 Ti1 P1 100.30(5) 2_556 . ?
N1 Ti1 P1 75.88(5) . . ?
N1 Ti1 P1 100.30(5) . 2_556 ?
N1 Ti1 N1 130.02(10) 2_556 . ?
N2 Ti1 P1 94.419(17) . . ?
N2 Ti1 P1 94.420(17) . 2_556 ?
N2 Ti1 N1 114.99(5) . . ?
N2 Ti1 N1 114.99(5) . 2_556 ?
C6 P1 Ti1 94.19(7) . . ?
C6 P1 C8 104.96(12) . . ?
C6 P1 C11 103.15(10) . . ?
C8 P1 Ti1 127.94(10) . . ?
C8 P1 C11 101.08(13) . . ?
C11 P1 Ti1 121.21(8) . . ?
N2 P2 C23 108.90(19) . . ?
N2 P2 C23' 97.3(2) . 2_556 ?
C1 N1 Ti1 124.96(14) . . ?
C1 N1 C14 113.61(17) . . ?
C14 N1 Ti1 119.49(13) . . ?
P2 N2 Ti1 162.21(6) . . ?
P2 N2 Ti1 162.21(6) 2_556 . ?
P2 N2 P2 35.59(12) 2_556 . ?
N1 C1 C2 122.6(2) . . ?
N1 C1 C6 120.60(19) . . ?
C2 C1 C6 116.8(2) . . ?
C3 C2 C1 121.1(2) . . ?
C4 C3 C2 122.2(2) . . ?
C3 C4 C5 117.0(2) . . ?
C3 C4 C7 121.6(3) . . ?
C5 C4 C7 121.3(3) . . ?
C4 C5 C6 122.5(2) . . ?
C1 C6 P1 116.23(16) . . ?
C5 C6 P1 123.58(18) . . ?
C5 C6 C1 120.0(2) . . ?
C9 C8 P1 113.3(2) . . ?
C9 C8 C10 109.9(3) . . ?
C10 C8 P1 113.1(2) . . ?
C12 C11 P1 109.36(16) . . ?
C12 C11 C13 109.5(2) . . ?
C13 C11 P1 116.02(19) . . ?
C15 C14 N1 119.9(2) . . ?
C19 C14 N1 120.54(19) . . ?
C19 C14 C15 119.5(2) . . ?
C14 C15 C20 120.6(2) . . ?
C16 C15 C14 119.1(2) . . ?
C16 C15 C20 120.2(2) . . ?
C17 C16 C15 121.8(2) . . ?
C16 C17 C21 120.9(2) . . ?
C18 C17 C16 118.2(2) . . ?
C18 C17 C21 120.8(3) . . ?
C17 C18 C19 121.9(2) . . ?
C14 C19 C22 121.3(2) . . ?
C18 C19 C14 119.2(2) . . ?
C18 C19 C22 119.4(2) . . ?
C24 C23 P2 107.2(4) . . ?
C24 C23 C25 111.9(5) . . ?
C25 C23 P2 104.7(4) . . ?
C24 C23' P2 111.6(4) . 2_556 ?
C25 C23' P2 115.0(4) . 2_556 ?
C25 C23' C24 102.8(4) . . ?
C26 C27 C28 113.3 . . ?
C29 C28 C27 113.8 . . ?
C30 C29 C28 113.3 . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_9172
_database_code_depnum_ccdc_archive 'CCDC 1490140'
_audit_update_record             
;
2016-07-04 deposited with the CCDC.
2016-09-22 downloaded from the CCDC.
;

# Crystallographer: Patrick J. Carroll

# Compound 4

_audit_creation_date             2016-06-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_formula_moiety         'C47 H71 N3 P2 Si Ti'
_chemical_formula_sum            'C47 H71 N3 P2 Si Ti'
_chemical_formula_weight         815.99

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   30.336(2)
_cell_length_b                   12.1037(10)
_cell_length_c                   29.271(2)
_cell_angle_alpha                90
_cell_angle_beta                 118.588(4)
_cell_angle_gamma                90
_cell_volume                     9437.3(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.88
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/4'
_exptl_crystal_color             orange
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       plate
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            183594
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.547
_diffrn_reflns_theta_min         1.591
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_number_gt                17991
_reflns_number_total             21655
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        'Bruker SAINT v8.34A'
_computing_molecular_graphics    'Mercury v3.6'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1011
_refine_ls_number_reflns         21655
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0506
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0342P)²+16.0780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1276
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct

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
Ti1 Ti 0.37164(2) 0.20524(3) 0.25465(2) 0.01609(9) Uani 1 1 d . . . . .
P1 P 0.29694(2) 0.20549(5) 0.15478(2) 0.01771(12) Uani 1 1 d . . . . .
P2 P 0.45131(2) 0.24848(5) 0.34782(2) 0.01914(12) Uani 1 1 d . . . . .
Si1 Si 0.36825(3) -0.05734(6) 0.29901(3) 0.02547(15) Uani 1 1 d . . . . .
N1 N 0.31951(7) 0.32228(16) 0.25186(7) 0.0193(4) Uani 1 1 d . . . . .
N2 N 0.43181(7) 0.21170(16) 0.23962(7) 0.0169(4) Uani 1 1 d . . . . .
N3 N 0.36425(7) 0.07510(17) 0.27446(8) 0.0219(4) Uani 1 1 d . . . . .
C1 C 0.27078(9) 0.3432(2) 0.21203(9) 0.0212(5) Uani 1 1 d . . . . .
C2 C 0.23640(9) 0.4105(2) 0.21876(10) 0.0262(5) Uani 1 1 d . . . . .
H2 H 0.2458 0.4411 0.2521 0.035 Uiso 1 1 calc R . . . .
C3 C 0.18927(10) 0.4330(2) 0.17799(11) 0.0281(5) Uani 1 1 d . . . . .
H3 H 0.1673 0.4792 0.1841 0.037 Uiso 1 1 calc R . . . .
C4 C 0.17285(9) 0.3904(2) 0.12825(10) 0.0275(5) Uani 1 1 d . . . . .
C5 C 0.20575(9) 0.3203(2) 0.12179(10) 0.0244(5) Uani 1 1 d . . . . .
H5 H 0.1952 0.2876 0.0887 0.032 Uiso 1 1 calc R . . . .
C6 C 0.25373(9) 0.2961(2) 0.16221(9) 0.0203(5) Uani 1 1 d . . . . .
C7 C 0.12202(10) 0.4192(3) 0.08354(11) 0.0380(7) Uani 1 1 d . . . . .
H7a H 0.0961 0.4054 0.0937 0.057 Uiso 1 1 calc GR . . . .
H7b H 0.1155 0.3735 0.0533 0.057 Uiso 1 1 calc GR . . . .
H7c H 0.1215 0.4974 0.0746 0.057 Uiso 1 1 calc GR . . . .
C8 C 0.30331(9) 0.2646(2) 0.09960(9) 0.0225(5) Uani 1 1 d . . . . .
H8 H 0.3357 0.2355 0.1031 0.030 Uiso 1 1 calc R . . . .
C9 C 0.30939(10) 0.3901(2) 0.10557(11) 0.0288(5) Uani 1 1 d . . . . .
H9a H 0.3220 0.4183 0.0826 0.043 Uiso 1 1 calc GR . . . .
H9b H 0.3333 0.4083 0.1417 0.043 Uiso 1 1 calc GR . . . .
H9c H 0.2768 0.4240 0.0962 0.043 Uiso 1 1 calc GR . . . .
C10 C 0.26259(10) 0.2336(3) 0.04450(10) 0.0332(6) Uani 1 1 d . . . . .
H10a H 0.2305 0.2659 0.0379 0.050 Uiso 1 1 calc GR . . . .
H10b H 0.2594 0.1531 0.0414 0.050 Uiso 1 1 calc GR . . . .
H10c H 0.2719 0.2622 0.0190 0.050 Uiso 1 1 calc GR . . . .
C11 C 0.25867(9) 0.0796(2) 0.12866(10) 0.0230(5) Uani 1 1 d . . . . .
H11 H 0.2295 0.0995 0.0943 0.031 Uiso 1 1 calc R . . . .
C12 C 0.23751(10) 0.0426(2) 0.16381(11) 0.0302(6) Uani 1 1 d . . . . .
H12a H 0.2207 -0.0289 0.1518 0.045 Uiso 1 1 calc GR . . . .
H12b H 0.2133 0.0974 0.1627 0.045 Uiso 1 1 calc GR . . . .
H12c H 0.2649 0.0354 0.1996 0.045 Uiso 1 1 calc GR . . . .
C13 C 0.28707(10) -0.0140(2) 0.11888(11) 0.0314(6) Uani 1 1 d . . . . .
H13a H 0.3138 -0.0411 0.1522 0.047 Uiso 1 1 calc GR . . . .
H13b H 0.3018 0.0136 0.0977 0.047 Uiso 1 1 calc GR . . . .
H13c H 0.2638 -0.0745 0.1005 0.047 Uiso 1 1 calc GR . . . .
C14 C 0.33247(8) 0.3888(2) 0.29720(9) 0.0196(5) Uani 1 1 d . . . . .
C15 C 0.32573(9) 0.3469(2) 0.33834(10) 0.0240(5) Uani 1 1 d . . . . .
C16 C 0.33941(10) 0.4130(2) 0.38212(10) 0.0269(5) Uani 1 1 d . . . . .
H16 H 0.3364 0.3837 0.4106 0.036 Uiso 1 1 calc R . . . .
C17 C 0.35728(9) 0.5198(2) 0.38555(9) 0.0259(5) Uani 1 1 d . . . . .
C18 C 0.36031(9) 0.5620(2) 0.34277(9) 0.0240(5) Uani 1 1 d . . . . .
H18 H 0.3712 0.6360 0.3438 0.032 Uiso 1 1 calc R . . . .
C19 C 0.34782(9) 0.4986(2) 0.29868(9) 0.0218(5) Uani 1 1 d . . . . .
C20 C 0.30150(11) 0.2360(2) 0.33325(11) 0.0325(6) Uani 1 1 d . . . . .
H20a H 0.3010 0.2183 0.3657 0.049 Uiso 1 1 calc GR . . . .
H20b H 0.3207 0.1795 0.3263 0.049 Uiso 1 1 calc GR . . . .
H20c H 0.2670 0.2380 0.3045 0.049 Uiso 1 1 calc GR . . . .
C21 C 0.37318(11) 0.5888(3) 0.43387(10) 0.0359(7) Uani 1 1 d . . . . .
H21a H 0.3514 0.5723 0.4492 0.054 Uiso 1 1 calc GR . . . .
H21b H 0.3704 0.6673 0.4247 0.054 Uiso 1 1 calc GR . . . .
H21c H 0.4081 0.5716 0.4591 0.054 Uiso 1 1 calc GR . . . .
C22 C 0.34845(11) 0.5489(2) 0.25197(10) 0.0281(5) Uani 1 1 d . . . . .
H22a H 0.3144 0.5716 0.2266 0.042 Uiso 1 1 calc GR . . . .
H22b H 0.3608 0.4944 0.2361 0.042 Uiso 1 1 calc GR . . . .
H22c H 0.3706 0.6136 0.2628 0.042 Uiso 1 1 calc GR . . . .
C23 C 0.48275(8) 0.20637(18) 0.27590(9) 0.0175(4) Uani 1 1 d . . . . .
C24 C 0.52053(9) 0.1902(2) 0.26125(9) 0.0203(5) Uani 1 1 d . . . . .
H24 H 0.5111 0.1792 0.2256 0.027 Uiso 1 1 calc R . . . .
C25 C 0.57087(9) 0.1900(2) 0.29769(10) 0.0225(5) Uani 1 1 d . . . . .
H25 H 0.5950 0.1796 0.2862 0.030 Uiso 1 1 calc R . . . .
C26 C 0.58748(9) 0.2045(2) 0.35052(10) 0.0221(5) Uani 1 1 d . . . . .
C27 C 0.55106(9) 0.2188(2) 0.36564(9) 0.0219(5) Uani 1 1 d . . . . .
H27 H 0.5613 0.2284 0.4016 0.029 Uiso 1 1 calc R . . . .
C28 C 0.49956(8) 0.2195(2) 0.33002(9) 0.0190(4) Uani 1 1 d . . . . .
C29 C 0.64271(9) 0.2046(2) 0.38920(11) 0.0311(6) Uani 1 1 d . . . . .
H29a H 0.6507 0.2697 0.4117 0.047 Uiso 1 1 calc GR . . . .
H29b H 0.6623 0.2067 0.3706 0.047 Uiso 1 1 calc GR . . . .
H29c H 0.6511 0.1375 0.4105 0.047 Uiso 1 1 calc GR . . . .
C30 C 0.46506(9) 0.3899(2) 0.37526(10) 0.0259(5) Uani 1 1 d . . . . .
H30 H 0.4350 0.4146 0.3780 0.034 Uiso 1 1 calc R . . . .
C31 C 0.46903(10) 0.4655(2) 0.33574(11) 0.0302(6) Uani 1 1 d . . . . .
H31a H 0.4671 0.5427 0.3447 0.045 Uiso 1 1 calc GR . . . .
H31b H 0.4414 0.4497 0.3009 0.045 Uiso 1 1 calc GR . . . .
H31c H 0.5011 0.4527 0.3362 0.045 Uiso 1 1 calc GR . . . .
C32 C 0.51064(11) 0.4058(3) 0.42926(11) 0.0390(7) Uani 1 1 d . . . . .
H32a H 0.5414 0.3878 0.4277 0.058 Uiso 1 1 calc GR . . . .
H32b H 0.5076 0.3569 0.4543 0.058 Uiso 1 1 calc GR . . . .
H32c H 0.5120 0.4828 0.4402 0.058 Uiso 1 1 calc GR . . . .
C33 C 0.45945(11) 0.1496(3) 0.40011(11) 0.0345(6) Uani 1 1 d . . . . .
H33 H 0.4402 0.0826 0.3809 0.046 Uiso 1 1 calc R . . . .
C34 C 0.51081(13) 0.1059(3) 0.43771(13) 0.0463(8) Uani 1 1 d . . . . .
H34a H 0.5321 0.1670 0.4586 0.069 Uiso 1 1 calc GR . . . .
H34b H 0.5259 0.0711 0.4183 0.069 Uiso 1 1 calc GR . . . .
H34c H 0.5077 0.0512 0.4607 0.069 Uiso 1 1 calc GR . . . .
C35 C 0.43184(11) 0.1902(3) 0.42916(11) 0.0356(6) Uani 1 1 d . . . . .
H35a H 0.4322 0.1321 0.4526 0.053 Uiso 1 1 calc GR . . . .
H35b H 0.3971 0.2084 0.4040 0.053 Uiso 1 1 calc GR . . . .
H35c H 0.4487 0.2562 0.4494 0.053 Uiso 1 1 calc GR . . . .
C36 C 0.42336(8) 0.20406(19) 0.18673(9) 0.0175(4) Uani 1 1 d . . . . .
C37 C 0.41448(8) 0.1003(2) 0.16244(9) 0.0201(5) Uani 1 1 d . . . . .
C38 C 0.40675(9) 0.0941(2) 0.11145(9) 0.0243(5) Uani 1 1 d . . . . .
H38 H 0.3993 0.0245 0.0944 0.032 Uiso 1 1 calc R . . . .
C39 C 0.40964(10) 0.1870(2) 0.08503(9) 0.0268(5) Uani 1 1 d . . . . .
C40 C 0.42129(9) 0.2876(2) 0.11105(10) 0.0247(5) Uani 1 1 d . . . . .
H40 H 0.4249 0.3512 0.0940 0.033 Uiso 1 1 calc R . . . .
C41 C 0.42793(9) 0.2980(2) 0.16156(9) 0.0201(5) Uani 1 1 d . . . . .
C42 C 0.41762(10) -0.0034(2) 0.19193(10) 0.0244(5) Uani 1 1 d . . . . .
H42a H 0.4524 -0.0150 0.2190 0.037 Uiso 1 1 calc GR . . . .
H42b H 0.4066 -0.0664 0.1680 0.037 Uiso 1 1 calc GR . . . .
H42c H 0.3960 0.0036 0.2081 0.037 Uiso 1 1 calc GR . . . .
C43 C 0.40045(14) 0.1781(3) 0.02958(11) 0.0431(8) Uani 1 1 d . . . . .
H43a H 0.3643 0.1724 0.0059 0.065 Uiso 1 1 calc GR . . . .
H43b H 0.4174 0.1121 0.0261 0.065 Uiso 1 1 calc GR . . . .
H43c H 0.4137 0.2439 0.0209 0.065 Uiso 1 1 calc GR . . . .
C44 C 0.44208(10) 0.4080(2) 0.18874(10) 0.0248(5) Uani 1 1 d . . . . .
H44a H 0.4180 0.4278 0.2008 0.037 Uiso 1 1 calc GR . . . .
H44b H 0.4416 0.4645 0.1645 0.037 Uiso 1 1 calc GR . . . .
H44c H 0.4759 0.4034 0.2186 0.037 Uiso 1 1 calc GR . . . .
C45 C 0.31943(15) -0.1526(3) 0.25192(14) 0.0532(10) Uani 1 1 d . . . . .
H45a H 0.2861 -0.1249 0.2436 0.080 Uiso 1 1 calc GR . . . .
H45b H 0.3242 -0.2264 0.2673 0.080 Uiso 1 1 calc GR . . . .
H45c H 0.3223 -0.1565 0.2200 0.080 Uiso 1 1 calc GR . . . .
C46 C 0.35782(12) -0.0578(3) 0.35737(13) 0.0393(7) Uani 1 1 d . . . . .
H46a H 0.3833 -0.0115 0.3848 0.059 Uiso 1 1 calc GR . . . .
H46b H 0.3604 -0.1336 0.3702 0.059 Uiso 1 1 calc GR . . . .
H46c H 0.3243 -0.0285 0.3475 0.059 Uiso 1 1 calc GR . . . .
C47 C 0.43095(12) -0.1202(3) 0.31796(13) 0.0429(8) Uani 1 1 d . . . . .
H47a H 0.4335 -0.1371 0.2866 0.064 Uiso 1 1 calc GR . . . .
H47b H 0.4347 -0.1883 0.3376 0.064 Uiso 1 1 calc GR . . . .
H47c H 0.4575 -0.0680 0.3397 0.064 Uiso 1 1 calc GR . . . .
Ti1' Ti 0.12635(2) 0.68353(3) 0.39519(2) 0.01577(9) Uani 1 1 d . . . . .
P1' P 0.09089(2) 0.64908(5) 0.46316(2) 0.01855(12) Uani 1 1 d . . . . .
P2' P 0.15267(2) 0.77521(5) 0.32727(2) 0.01761(12) Uani 1 1 d . . . . .
Si1' Si 0.16020(3) 0.42166(6) 0.37791(3) 0.02369(14) Uani 1 1 d . . . . .
N1' N 0.17272(8) 0.77554(17) 0.46216(7) 0.0209(4) Uani 1 1 d . . . . .
N2' N 0.05813(7) 0.71415(16) 0.32842(7) 0.0160(4) Uani 1 1 d . . . . .
N3' N 0.14764(7) 0.55232(17) 0.39341(8) 0.0215(4) Uani 1 1 d . . . . .
C1' C 0.17666(9) 0.7721(2) 0.51168(9) 0.0198(5) Uani 1 1 d . . . . .
C2' C 0.21554(9) 0.8245(2) 0.55563(9) 0.0239(5) Uani 1 1 d . . . . .
H2' H 0.2409 0.8634 0.5519 0.032 Uiso 1 1 calc R . . . .
C3' C 0.21773(9) 0.8206(2) 0.60401(9) 0.0239(5) Uani 1 1 d . . . . .
H3' H 0.2441 0.8583 0.6324 0.032 Uiso 1 1 calc R . . . .
C4' C 0.18234(9) 0.7628(2) 0.61219(9) 0.0226(5) Uani 1 1 d . . . . .
C5' C 0.14437(9) 0.7098(2) 0.56946(9) 0.0218(5) Uani 1 1 d . . . . .
H5' H 0.1199 0.6691 0.5739 0.029 Uiso 1 1 calc R . . . .
C6' C 0.14066(9) 0.7141(2) 0.51982(9) 0.0197(5) Uani 1 1 d . . . . .
C7' C 0.18483(10) 0.7592(2) 0.66499(9) 0.0279(5) Uani 1 1 d . . . . .
H7a' H 0.1629 0.8165 0.6669 0.042 Uiso 1 1 calc GR . . . .
H7b' H 0.2195 0.7722 0.6921 0.042 Uiso 1 1 calc GR . . . .
H7c' H 0.1737 0.6865 0.6702 0.042 Uiso 1 1 calc GR . . . .
C8' C 0.03273(9) 0.7203(2) 0.45312(9) 0.0238(5) Uani 1 1 d . . . . .
H8' H 0.0065 0.7033 0.4167 0.032 Uiso 1 1 calc R . . . .
C9' C 0.04129(11) 0.8448(2) 0.45570(11) 0.0321(6) Uani 1 1 d . . . . .
H9a' H 0.0090 0.8831 0.4421 0.048 Uiso 1 1 calc GR . . . .
H9b' H 0.0575 0.8644 0.4348 0.048 Uiso 1 1 calc GR . . . .
H9c' H 0.0629 0.8669 0.4919 0.048 Uiso 1 1 calc GR . . . .
C10' C 0.01110(11) 0.6858(3) 0.48864(10) 0.0337(6) Uani 1 1 d . . . . .
H10a' H 0.0361 0.6991 0.5250 0.051 Uiso 1 1 calc GR . . . .
H10b' H 0.0025 0.6071 0.4836 0.051 Uiso 1 1 calc GR . . . .
H10c' H -0.0191 0.7292 0.4801 0.051 Uiso 1 1 calc GR . . . .
C11' C 0.08828(9) 0.5100(2) 0.48788(9) 0.0237(5) Uani 1 1 d . . . . .
H11' H 0.0794 0.5193 0.5164 0.032 Uiso 1 1 calc R . . . .
C12' C 0.14032(10) 0.4564(2) 0.51141(10) 0.0318(6) Uani 1 1 d . . . . .
H12a' H 0.1381 0.3798 0.5210 0.048 Uiso 1 1 calc GR . . . .
H12b' H 0.1637 0.4976 0.5425 0.048 Uiso 1 1 calc GR . . . .
H12c' H 0.1524 0.4576 0.4858 0.048 Uiso 1 1 calc GR . . . .
C13' C 0.04825(10) 0.4372(2) 0.44622(10) 0.0282(5) Uani 1 1 d . . . . .
H13a' H 0.0559 0.4273 0.4175 0.042 Uiso 1 1 calc GR . . . .
H13b' H 0.0153 0.4725 0.4332 0.042 Uiso 1 1 calc GR . . . .
H13c' H 0.0478 0.3651 0.4612 0.042 Uiso 1 1 calc GR . . . .
C14' C 0.21016(11) 0.8452(2) 0.46105(9) 0.0326(6) Uani 1 1 d . . . . .
C15' C 0.25525(12) 0.8007(3) 0.46867(11) 0.0419(8) Uani 1 1 d . . . . .
C16' C 0.29185(14) 0.8746(4) 0.46932(13) 0.0579(11) Uani 1 1 d . . . . .
H16' H 0.3232 0.8471 0.4743 0.077 Uiso 1 1 calc R . . . .
C17' C 0.28158(17) 0.9890(3) 0.46255(12) 0.0574(12) Uani 1 1 d . . . . .
C18' C 0.23772(16) 1.0310(3) 0.45680(12) 0.0526(10) Uani 1 1 d . . . . .
H18' H 0.2320 1.1084 0.4529 0.070 Uiso 1 1 calc R . . . .
C19' C 0.20133(15) 0.9624(3) 0.45662(11) 0.0473(9) Uani 1 1 d . . . . .
C20' C 0.26522(11) 0.6802(3) 0.47900(12) 0.0447(8) Uani 1 1 d . . . . .
H20a' H 0.2616 0.6596 0.5094 0.067 Uiso 1 1 calc GR . . . .
H20b' H 0.2994 0.6637 0.4857 0.067 Uiso 1 1 calc GR . . . .
H20c' H 0.2412 0.6382 0.4486 0.067 Uiso 1 1 calc GR . . . .
C21' C 0.3237(2) 1.0644(5) 0.46459(17) 0.095(2) Uani 1 1 d . . . . .
H21a' H 0.3245 1.1334 0.4824 0.142 Uiso 1 1 calc GR . . . .
H21b' H 0.3171 1.0807 0.4291 0.142 Uiso 1 1 calc GR . . . .
H21c' H 0.3561 1.0266 0.4835 0.142 Uiso 1 1 calc GR . . . .
C22' C 0.15621(15) 1.0118(3) 0.45642(13) 0.0507(9) Uani 1 1 d . . . . .
H22a' H 0.1615 1.0157 0.4921 0.076 Uiso 1 1 calc GR . . . .
H22b' H 0.1268 0.9658 0.4354 0.076 Uiso 1 1 calc GR . . . .
H22c' H 0.1507 1.0863 0.4416 0.076 Uiso 1 1 calc GR . . . .
C23' C 0.05259(8) 0.71636(18) 0.27808(8) 0.0165(4) Uani 1 1 d . . . . .
C24' C 0.00644(9) 0.69416(19) 0.23326(8) 0.0182(4) Uani 1 1 d . . . . .
H24' H -0.0227 0.6815 0.2368 0.024 Uiso 1 1 calc R . . . .
C25' C 0.00264(9) 0.69051(19) 0.18416(9) 0.0200(5) Uani 1 1 d . . . . .
H25' H -0.0289 0.6738 0.1550 0.027 Uiso 1 1 calc R . . . .
C26' C 0.04366(9) 0.7105(2) 0.17643(9) 0.0214(5) Uani 1 1 d . . . . .
C27' C 0.08852(9) 0.7378(2) 0.21991(9) 0.0211(5) Uani 1 1 d . . . . .
H27' H 0.1168 0.7548 0.2154 0.028 Uiso 1 1 calc R . . . .
C28' C 0.09404(8) 0.74128(19) 0.27020(8) 0.0176(4) Uani 1 1 d . . . . .
C29' C 0.03957(10) 0.7026(3) 0.12286(9) 0.0323(6) Uani 1 1 d . . . . .
H29a' H 0.0532 0.7700 0.1157 0.048 Uiso 1 1 calc GR . . . .
H29b' H 0.0042 0.6943 0.0967 0.048 Uiso 1 1 calc GR . . . .
H29c' H 0.0587 0.6386 0.1215 0.048 Uiso 1 1 calc GR . . . .
C30' C 0.15819(9) 0.9284(2) 0.32564(9) 0.0227(5) Uani 1 1 d . . . . .
H30' H 0.1863 0.9514 0.3601 0.030 Uiso 1 1 calc R . . . .
C31' C 0.11039(11) 0.9820(2) 0.32035(12) 0.0315(6) Uani 1 1 d . . . . .
H31a' H 0.1157 1.0617 0.3263 0.047 Uiso 1 1 calc GR . . . .
H31b' H 0.1021 0.9499 0.3461 0.047 Uiso 1 1 calc GR . . . .
H31c' H 0.0827 0.9687 0.2853 0.047 Uiso 1 1 calc GR . . . .
C32' C 0.16985(11) 0.9741(2) 0.28385(10) 0.0318(6) Uani 1 1 d . . . . .
H32a' H 0.1445 0.9479 0.2496 0.048 Uiso 1 1 calc GR . . . .
H32b' H 0.2031 0.9485 0.2906 0.048 Uiso 1 1 calc GR . . . .
H32c' H 0.1695 1.0550 0.2846 0.048 Uiso 1 1 calc GR . . . .
C33' C 0.20115(9) 0.7284(2) 0.31003(9) 0.0239(5) Uani 1 1 d . . . . .
H33' H 0.1952 0.7696 0.2780 0.032 Uiso 1 1 calc R . . . .
C34' C 0.19783(11) 0.6063(2) 0.29709(11) 0.0338(6) Uani 1 1 d . . . . .
H34a' H 0.2242 0.5870 0.2882 0.051 Uiso 1 1 calc GR . . . .
H34b' H 0.1649 0.5901 0.2675 0.051 Uiso 1 1 calc GR . . . .
H34c' H 0.2023 0.5629 0.3273 0.051 Uiso 1 1 calc GR . . . .
C35' C 0.25420(9) 0.7576(3) 0.35227(10) 0.0324(6) Uani 1 1 d . . . . .
H35a' H 0.2629 0.7128 0.3833 0.049 Uiso 1 1 calc GR . . . .
H35b' H 0.2556 0.8361 0.3611 0.049 Uiso 1 1 calc GR . . . .
H35c' H 0.2781 0.7427 0.3395 0.049 Uiso 1 1 calc GR . . . .
C36' C 0.01115(8) 0.69687(19) 0.32883(8) 0.0165(4) Uani 1 1 d . . . . .
C37' C -0.00643(8) 0.58871(19) 0.32725(8) 0.0181(4) Uani 1 1 d . . . . .
C38' C -0.05076(9) 0.5737(2) 0.32981(9) 0.0220(5) Uani 1 1 d . . . . .
H38' H -0.0617 0.5006 0.3308 0.029 Uiso 1 1 calc R . . . .
C39' C -0.07938(9) 0.6618(2) 0.33104(9) 0.0240(5) Uani 1 1 d . . . . .
C40' C -0.06342(9) 0.7680(2) 0.32823(9) 0.0220(5) Uani 1 1 d . . . . .
H40' H -0.0836 0.8291 0.3271 0.029 Uiso 1 1 calc R . . . .
C41' C -0.01860(8) 0.7874(2) 0.32701(8) 0.0187(4) Uani 1 1 d . . . . .
C42' C 0.01948(9) 0.4916(2) 0.31903(9) 0.0218(5) Uani 1 1 d . . . . .
H42a' H 0.0038 0.4232 0.3221 0.033 Uiso 1 1 calc GR . . . .
H42b' H 0.0550 0.4921 0.3453 0.033 Uiso 1 1 calc GR . . . .
H42c' H 0.0166 0.4958 0.2843 0.033 Uiso 1 1 calc GR . . . .
C43' C -0.12636(10) 0.6432(3) 0.33548(12) 0.0335(6) Uani 1 1 d . . . . .
H43a' H -0.1368 0.5658 0.3276 0.050 Uiso 1 1 calc GR . . . .
H43b' H -0.1532 0.6913 0.3108 0.050 Uiso 1 1 calc GR . . . .
H43c' H -0.1196 0.6604 0.3710 0.050 Uiso 1 1 calc GR . . . .
C44' C -0.00390(9) 0.9037(2) 0.32210(10) 0.0231(5) Uani 1 1 d . . . . .
H44a' H -0.0305 0.9546 0.3185 0.035 Uiso 1 1 calc GR . . . .
H44b' H 0.0009 0.9093 0.2914 0.035 Uiso 1 1 calc GR . . . .
H44c' H 0.0275 0.9229 0.3532 0.035 Uiso 1 1 calc GR . . . .
C45' C 0.13854(11) 0.3065(2) 0.40494(12) 0.0332(6) Uani 1 1 d . . . . .
H45a' H 0.1579 0.3073 0.4430 0.050 Uiso 1 1 calc GR . . . .
H45b' H 0.1436 0.2357 0.3919 0.050 Uiso 1 1 calc GR . . . .
H45c' H 0.1028 0.3160 0.3941 0.050 Uiso 1 1 calc GR . . . .
C46' C 0.22971(10) 0.3998(3) 0.40652(12) 0.0345(6) Uani 1 1 d . . . . .
H46a' H 0.2436 0.4552 0.3925 0.052 Uiso 1 1 calc GR . . . .
H46b' H 0.2361 0.3257 0.3975 0.052 Uiso 1 1 calc GR . . . .
H46c' H 0.2457 0.4071 0.4444 0.052 Uiso 1 1 calc GR . . . .
C47' C 0.12691(11) 0.3981(3) 0.30562(11) 0.0362(6) Uani 1 1 d . . . . .
H47a' H 0.0985 0.3480 0.2964 0.054 Uiso 1 1 calc GR . . . .
H47b' H 0.1503 0.3654 0.2952 0.054 Uiso 1 1 calc GR . . . .
H47c' H 0.1146 0.4688 0.2877 0.054 Uiso 1 1 calc GR . . . .


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 P1 2.7094(7) . ?
Ti1 P2 2.6917(7) . ?
Ti1 N1 2.095(2) . ?
Ti1 N2 2.0735(19) . ?
Ti1 N3 1.730(2) . ?
P1 C6 1.800(2) . ?
P1 C8 1.859(2) . ?
P1 C11 1.845(2) . ?
P2 C28 1.807(2) . ?
P2 C30 1.851(3) . ?
P2 C33 1.864(3) . ?
Si1 N3 1.737(2) . ?
Si1 C45 1.862(3) . ?
Si1 C46 1.880(3) . ?
Si1 C47 1.869(3) . ?
N1 C1 1.400(3) . ?
N1 C14 1.437(3) . ?
N2 C23 1.396(3) . ?
N2 C36 1.446(3) . ?
C1 C2 1.410(3) . ?
C1 C6 1.413(3) . ?
C2 C3 1.382(4) . ?
C3 C4 1.393(4) . ?
C4 C5 1.390(4) . ?
C4 C7 1.510(4) . ?
C5 C6 1.399(3) . ?
C8 C9 1.530(4) . ?
C8 C10 1.537(3) . ?
C11 C12 1.518(4) . ?
C11 C13 1.531(3) . ?
C14 C15 1.408(3) . ?
C14 C19 1.403(3) . ?
C15 C16 1.394(4) . ?
C15 C20 1.503(4) . ?
C16 C17 1.388(4) . ?
C17 C18 1.395(4) . ?
C17 C21 1.509(3) . ?
C18 C19 1.389(3) . ?
C19 C22 1.505(3) . ?
C23 C24 1.416(3) . ?
C23 C28 1.422(3) . ?
C24 C25 1.382(3) . ?
C25 C26 1.389(3) . ?
C26 C27 1.383(3) . ?
C26 C29 1.508(3) . ?
C27 C28 1.403(3) . ?
C30 C31 1.524(4) . ?
C30 C32 1.535(4) . ?
C33 C34 1.509(4) . ?
C33 C35 1.532(4) . ?
C36 C37 1.404(3) . ?
C36 C41 1.397(3) . ?
C37 C38 1.398(3) . ?
C37 C42 1.500(3) . ?
C38 C39 1.391(4) . ?
C39 C40 1.390(4) . ?
C39 C43 1.514(3) . ?
C40 C41 1.399(3) . ?
C41 C44 1.504(3) . ?
Ti1' P1' 2.7088(7) . ?
Ti1' P2' 2.7093(7) . ?
Ti1' N1' 2.103(2) . ?
Ti1' N2' 2.0903(19) . ?
Ti1' N3' 1.725(2) . ?
P1' C6' 1.804(2) . ?
P1' C8' 1.856(3) . ?
P1' C11' 1.849(3) . ?
P2' C28' 1.811(2) . ?
P2' C30' 1.865(3) . ?
P2' C33' 1.857(2) . ?
Si1' N3' 1.737(2) . ?
Si1' C45' 1.871(3) . ?
Si1' C46' 1.878(3) . ?
Si1' C47' 1.879(3) . ?
N1' C1' 1.397(3) . ?
N1' C14' 1.427(3) . ?
N2' C23' 1.401(3) . ?
N2' C36' 1.446(3) . ?
C1' C2' 1.413(3) . ?
C1' C6' 1.411(3) . ?
C2' C3' 1.386(3) . ?
C3' C4' 1.395(4) . ?
C4' C5' 1.387(3) . ?
C4' C7' 1.511(3) . ?
C5' C6' 1.404(3) . ?
C8' C9' 1.525(4) . ?
C8' C10' 1.529(3) . ?
C11' C12' 1.532(4) . ?
C11' C13' 1.523(4) . ?
C14' C15' 1.385(5) . ?
C14' C19' 1.438(5) . ?
C15' C16' 1.418(4) . ?
C15' C20' 1.491(5) . ?
C16' C17' 1.413(6) . ?
C17' C18' 1.357(6) . ?
C17' C21' 1.547(5) . ?
C18' C19' 1.379(4) . ?
C19' C22' 1.491(6) . ?
C23' C24' 1.413(3) . ?
C23' C28' 1.415(3) . ?
C24' C25' 1.387(3) . ?
C25' C26' 1.388(3) . ?
C26' C27' 1.387(3) . ?
C26' C29' 1.516(3) . ?
C27' C28' 1.400(3) . ?
C30' C31' 1.527(4) . ?
C30' C32' 1.530(3) . ?
C33' C34' 1.517(4) . ?
C33' C35' 1.530(4) . ?
C36' C37' 1.406(3) . ?
C36' C41' 1.404(3) . ?
C37' C38' 1.394(3) . ?
C37' C42' 1.496(3) . ?
C38' C39' 1.386(4) . ?
C39' C40' 1.390(4) . ?
C39' C43' 1.509(3) . ?
C40' C41' 1.397(3) . ?
C41' C44' 1.504(3) . ?

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
P2 Ti1 P1 167.14(3) . . ?
N1 Ti1 P1 74.40(5) . . ?
N1 Ti1 P2 101.72(6) . . ?
N2 Ti1 P1 97.92(5) . . ?
N2 Ti1 P2 75.69(5) . . ?
N2 Ti1 N1 133.70(8) . . ?
N3 Ti1 P1 100.78(7) . . ?
N3 Ti1 P2 92.00(7) . . ?
N3 Ti1 N1 114.33(9) . . ?
N3 Ti1 N2 111.96(9) . . ?
C6 P1 Ti1 98.73(8) . . ?
C6 P1 C8 104.78(11) . . ?
C6 P1 C11 101.71(11) . . ?
C8 P1 Ti1 123.82(8) . . ?
C11 P1 Ti1 118.80(8) . . ?
C11 P1 C8 105.32(11) . . ?
C28 P2 Ti1 97.38(8) . . ?
C28 P2 C30 105.03(11) . . ?
C28 P2 C33 107.73(12) . . ?
C30 P2 Ti1 121.74(9) . . ?
C30 P2 C33 108.87(13) . . ?
C33 P2 Ti1 114.14(11) . . ?
N3 Si1 C45 113.05(13) . . ?
N3 Si1 C46 111.69(12) . . ?
N3 Si1 C47 110.99(13) . . ?
C45 Si1 C46 104.51(17) . . ?
C45 Si1 C47 107.69(18) . . ?
C47 Si1 C46 108.60(15) . . ?
C1 N1 Ti1 129.15(15) . . ?
C1 N1 C14 112.41(19) . . ?
C14 N1 Ti1 118.35(14) . . ?
C23 N2 Ti1 127.10(15) . . ?
C23 N2 C36 112.09(18) . . ?
C36 N2 Ti1 120.10(14) . . ?
Ti1 N3 Si1 169.87(13) . . ?
N1 C1 C2 123.0(2) . . ?
N1 C1 C6 120.4(2) . . ?
C2 C1 C6 116.6(2) . . ?
C3 C2 C1 121.5(2) . . ?
C2 C3 C4 122.3(2) . . ?
C3 C4 C7 121.8(2) . . ?
C5 C4 C3 116.6(2) . . ?
C5 C4 C7 121.7(2) . . ?
C4 C5 C6 122.5(2) . . ?
C1 C6 P1 116.25(17) . . ?
C5 C6 P1 123.26(19) . . ?
C5 C6 C1 120.5(2) . . ?
C9 C8 P1 109.86(17) . . ?
C9 C8 C10 110.7(2) . . ?
C10 C8 P1 116.91(18) . . ?
C12 C11 P1 110.43(18) . . ?
C12 C11 C13 111.5(2) . . ?
C13 C11 P1 112.93(17) . . ?
C15 C14 N1 120.1(2) . . ?
C19 C14 N1 120.0(2) . . ?
C19 C14 C15 119.7(2) . . ?
C14 C15 C20 120.0(2) . . ?
C16 C15 C14 118.6(2) . . ?
C16 C15 C20 121.3(2) . . ?
C17 C16 C15 122.3(2) . . ?
C16 C17 C18 117.9(2) . . ?
C16 C17 C21 121.5(2) . . ?
C18 C17 C21 120.7(3) . . ?
C19 C18 C17 121.7(2) . . ?
C14 C19 C22 120.2(2) . . ?
C18 C19 C14 119.4(2) . . ?
C18 C19 C22 120.3(2) . . ?
N2 C23 C24 122.5(2) . . ?
N2 C23 C28 121.2(2) . . ?
C24 C23 C28 116.2(2) . . ?
C25 C24 C23 121.5(2) . . ?
C24 C25 C26 122.5(2) . . ?
C25 C26 C29 121.1(2) . . ?
C27 C26 C25 116.9(2) . . ?
C27 C26 C29 122.0(2) . . ?
C26 C27 C28 122.6(2) . . ?
C23 C28 P2 115.77(17) . . ?
C27 C28 P2 123.66(18) . . ?
C27 C28 C23 120.4(2) . . ?
C31 C30 P2 108.00(17) . . ?
C31 C30 C32 110.3(2) . . ?
C32 C30 P2 117.9(2) . . ?
C34 C33 P2 120.6(2) . . ?
C34 C33 C35 110.8(2) . . ?
C35 C33 P2 110.9(2) . . ?
C37 C36 N2 119.5(2) . . ?
C41 C36 N2 120.1(2) . . ?
C41 C36 C37 120.3(2) . . ?
C36 C37 C42 120.8(2) . . ?
C38 C37 C36 118.8(2) . . ?
C38 C37 C42 120.1(2) . . ?
C39 C38 C37 121.8(2) . . ?
C38 C39 C43 120.7(3) . . ?
C40 C39 C38 118.1(2) . . ?
C40 C39 C43 121.2(3) . . ?
C39 C40 C41 121.9(2) . . ?
C36 C41 C40 118.9(2) . . ?
C36 C41 C44 121.1(2) . . ?
C40 C41 C44 119.9(2) . . ?
P1' Ti1' P2' 164.16(3) . . ?
N1' Ti1' P1' 73.77(6) . . ?
N1' Ti1' P2' 99.58(6) . . ?
N2' Ti1' P1' 98.66(5) . . ?
N2' Ti1' P2' 75.46(5) . . ?
N2' Ti1' N1' 134.35(8) . . ?
N3' Ti1' P1' 99.59(7) . . ?
N3' Ti1' P2' 96.25(7) . . ?
N3' Ti1' N1' 115.00(9) . . ?
N3' Ti1' N2' 110.65(9) . . ?
C6' P1' Ti1' 98.99(8) . . ?
C6' P1' C8' 104.90(11) . . ?
C6' P1' C11' 102.19(11) . . ?
C8' P1' Ti1' 119.58(8) . . ?
C11' P1' Ti1' 122.28(8) . . ?
C11' P1' C8' 105.62(12) . . ?
C28' P2' Ti1' 94.58(7) . . ?
C28' P2' C30' 105.22(11) . . ?
C28' P2' C33' 103.65(11) . . ?
C30' P2' Ti1' 119.19(8) . . ?
C33' P2' Ti1' 128.62(9) . . ?
C33' P2' C30' 101.78(12) . . ?
N3' Si1' C45' 113.74(12) . . ?
N3' Si1' C46' 110.59(12) . . ?
N3' Si1' C47' 111.41(12) . . ?
C45' Si1' C46' 104.65(13) . . ?
C45' Si1' C47' 104.77(14) . . ?
C46' Si1' C47' 111.38(14) . . ?
C1' N1' Ti1' 129.66(16) . . ?
C1' N1' C14' 111.56(19) . . ?
C14' N1' Ti1' 118.44(15) . . ?
C23' N2' Ti1' 123.60(14) . . ?
C23' N2' C36' 112.87(17) . . ?
C36' N2' Ti1' 120.36(13) . . ?
Ti1' N3' Si1' 168.06(13) . . ?
N1' C1' C2' 123.4(2) . . ?
N1' C1' C6' 120.1(2) . . ?
C6' C1' C2' 116.5(2) . . ?
C3' C2' C1' 121.7(2) . . ?
C2' C3' C4' 121.9(2) . . ?
C3' C4' C7' 121.6(2) . . ?
C5' C4' C3' 116.9(2) . . ?
C5' C4' C7' 121.5(2) . . ?
C4' C5' C6' 122.5(2) . . ?
C1' C6' P1' 115.90(17) . . ?
C5' C6' P1' 123.57(18) . . ?
C5' C6' C1' 120.5(2) . . ?
C9' C8' P1' 108.94(18) . . ?
C9' C8' C10' 110.8(2) . . ?
C10' C8' P1' 116.75(18) . . ?
C12' C11' P1' 109.49(18) . . ?
C13' C11' P1' 112.35(17) . . ?
C13' C11' C12' 111.7(2) . . ?
N1' C14' C19' 118.0(3) . . ?
C15' C14' N1' 120.1(3) . . ?
C15' C14' C19' 121.7(3) . . ?
C14' C15' C16' 117.6(3) . . ?
C14' C15' C20' 120.1(3) . . ?
C16' C15' C20' 122.2(3) . . ?
C17' C16' C15' 119.8(4) . . ?
C16' C17' C21' 116.7(4) . . ?
C18' C17' C16' 121.4(3) . . ?
C18' C17' C21' 121.8(4) . . ?
C17' C18' C19' 120.7(4) . . ?
C14' C19' C22' 121.8(3) . . ?
C18' C19' C14' 118.6(4) . . ?
C18' C19' C22' 119.4(3) . . ?
N2' C23' C24' 122.7(2) . . ?
N2' C23' C28' 120.45(19) . . ?
C24' C23' C28' 116.9(2) . . ?
C25' C24' C23' 121.5(2) . . ?
C24' C25' C26' 121.8(2) . . ?
C25' C26' C29' 121.4(2) . . ?
C27' C26' C25' 117.0(2) . . ?
C27' C26' C29' 121.5(2) . . ?
C26' C27' C28' 122.9(2) . . ?
C23' C28' P2' 117.05(16) . . ?
C27' C28' P2' 123.19(17) . . ?
C27' C28' C23' 119.8(2) . . ?
C31' C30' P2' 109.39(17) . . ?
C31' C30' C32' 109.7(2) . . ?
C32' C30' P2' 115.93(18) . . ?
C34' C33' P2' 113.49(18) . . ?
C34' C33' C35' 110.2(2) . . ?
C35' C33' P2' 111.92(17) . . ?
C37' C36' N2' 119.6(2) . . ?
C41' C36' N2' 120.3(2) . . ?
C41' C36' C37' 119.9(2) . . ?
C36' C37' C42' 121.1(2) . . ?
C38' C37' C36' 118.7(2) . . ?
C38' C37' C42' 120.0(2) . . ?
C39' C38' C37' 122.2(2) . . ?
C38' C39' C40' 118.0(2) . . ?
C38' C39' C43' 121.1(2) . . ?
C40' C39' C43' 120.9(2) . . ?
C39' C40' C41' 121.8(2) . . ?
C36' C41' C44' 121.3(2) . . ?
C40' C41' C36' 119.0(2) . . ?
C40' C41' C44' 119.7(2) . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_9178
_database_code_depnum_ccdc_archive 'CCDC 1490141'
_audit_update_record             
;
2016-07-04 deposited with the CCDC.
2016-09-22 downloaded from the CCDC.
;

# Crystallographer: Patrick J. Carroll

# Compound 7

_audit_creation_date             2016-06-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_formula_moiety         'C44 H62.8 N3 P2 Ti'
_chemical_formula_sum            'C48 H72.80 N3 O P2 Ti'
_chemical_formula_weight         817.73

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.3708(10)
_cell_length_b                   12.8618(8)
_cell_length_c                   23.2563(15)
_cell_angle_alpha                90
_cell_angle_beta                 92.737(4)
_cell_angle_gamma                90
_cell_volume                     4592.4(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9779
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.36
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/4'
_exptl_crystal_color             orange
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_F_000             1767
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            77037
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.540
_diffrn_reflns_theta_min         1.753
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_number_gt                8553
_reflns_number_total             10568
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        'Bruker SAINT v8.34A'
_computing_molecular_graphics    'Mercury v3.6'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         10568
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0418
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0368P)²+4.3098P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1020
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_refine_special_details          
;
The data were corrected for the presence of disordered solvent using the
program SQUEEZE. The formula of the SQUEEZED solvent was included in 
_chemical_formula_moiety and _chemical_formula_sum in the CIF.
;

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
Ti1 Ti 0.18382(2) 0.59766(2) 0.26572(2) 0.01397(8) Uani 1 1 d . . . . .
P1 P 0.10075(3) 0.67695(3) 0.35453(2) 0.01425(9) Uani 1 1 d . . . . .
P2 P 0.27374(9) 0.51913(11) 0.18066(5) 0.0123(2) Uani 0.8 1 d D . P A 1
N3 N 0.08641(12) 0.56005(15) 0.22988(8) 0.0193(4) Uani 0.8 1 d . . P A 1
H3a H 0.0402 0.5380 0.2108 0.032 Uiso 0.8 1 d . . P B 1
P2' P 0.2808(4) 0.5036(5) 0.1633(2) 0.0201(10) Uani 0.2 1 d D . P A 2
N3' N 0.2180(5) 0.5830(5) 0.1946(3) 0.0162(15) Uani 0.2 1 d . . P A 2
N1 N 0.21689(9) 0.75598(11) 0.26743(6) 0.0154(3) Uani 1 1 d . . . . .
N2 N 0.24650(9) 0.47023(11) 0.30193(6) 0.0151(3) Uani 1 1 d . . . . .
C1 C 0.18043(11) 0.83603(13) 0.29915(7) 0.0159(3) Uani 1 1 d . . . . .
C2 C 0.19690(12) 0.94248(14) 0.28925(8) 0.0197(4) Uani 1 1 d . . . . .
H2 H 0.2335 0.9612 0.2603 0.026 Uiso 1 1 calc R . . . .
C3 C 0.15973(12) 1.01946(14) 0.32169(8) 0.0217(4) Uani 1 1 d . . . . .
H3 H 0.1722 1.0886 0.3138 0.029 Uiso 1 1 calc R . . . .
C4 C 0.10414(12) 0.99691(14) 0.36577(8) 0.0211(4) Uani 1 1 d . . . . .
C5 C 0.08681(11) 0.89222(14) 0.37513(8) 0.0191(4) Uani 1 1 d . . . . .
H5 H 0.0494 0.8744 0.4038 0.025 Uiso 1 1 calc R . . . .
C6 C 0.12346(11) 0.81287(13) 0.34312(7) 0.0160(3) Uani 1 1 d . . . . .
C7 C 0.06478(14) 1.08136(15) 0.40145(9) 0.0300(5) Uani 1 1 d . . . . .
H7a H 0.0168 1.1127 0.3799 0.045 Uiso 1 1 calc GR . . . .
H7b H 0.1081 1.1332 0.4109 0.045 Uiso 1 1 calc GR . . . .
H7c H 0.0444 1.0518 0.4362 0.045 Uiso 1 1 calc GR . . . .
C8 C -0.01996(11) 0.66991(14) 0.34886(8) 0.0182(3) Uani 1 1 d . . . . .
H8 H -0.0425 0.7073 0.3817 0.024 Uiso 1 1 calc R . . . .
C9 C -0.05680(12) 0.72132(15) 0.29377(8) 0.0233(4) Uani 1 1 d . . . . .
H9a H -0.0333 0.6879 0.2610 0.035 Uiso 1 1 calc GR . . . .
H9b H -0.0411 0.7936 0.2939 0.035 Uiso 1 1 calc GR . . . .
H9c H -0.1191 0.7149 0.2917 0.035 Uiso 1 1 calc GR . . . .
C10 C -0.04980(13) 0.55675(15) 0.35218(9) 0.0261(4) Uani 1 1 d . . . . .
H10a H -0.1122 0.5544 0.3528 0.039 Uiso 1 1 calc GR . . . .
H10b H -0.0249 0.5254 0.3866 0.039 Uiso 1 1 calc GR . . . .
H10c H -0.0311 0.5195 0.3192 0.039 Uiso 1 1 calc GR . . . .
C11 C 0.13225(12) 0.65227(15) 0.43175(7) 0.0209(4) Uani 1 1 d . . . . .
H11 H 0.1453 0.5779 0.4350 0.028 Uiso 1 1 calc R . . . .
C12 C 0.21715(13) 0.70959(16) 0.44731(9) 0.0281(4) Uani 1 1 d . . . . .
H12a H 0.2054 0.7824 0.4517 0.042 Uiso 1 1 calc GR . . . .
H12b H 0.2571 0.6999 0.4173 0.042 Uiso 1 1 calc GR . . . .
H12c H 0.2423 0.6825 0.4828 0.042 Uiso 1 1 calc GR . . . .
C13 C 0.06380(14) 0.67556(18) 0.47584(8) 0.0325(5) Uani 1 1 d . . . . .
H13a H 0.0865 0.6573 0.5137 0.049 Uiso 1 1 calc GR . . . .
H13b H 0.0122 0.6357 0.4667 0.049 Uiso 1 1 calc GR . . . .
H13c H 0.0498 0.7483 0.4748 0.049 Uiso 1 1 calc GR . . . .
C14 C 0.27141(11) 0.79246(13) 0.22293(7) 0.0157(3) Uani 1 1 d . . . . .
C15 C 0.23353(11) 0.81053(13) 0.16761(7) 0.0174(3) Uani 1 1 d . . . . .
C16 C 0.28686(12) 0.84046(13) 0.12361(7) 0.0193(4) Uani 1 1 d . . . . .
H16 H 0.2619 0.8516 0.0869 0.026 Uiso 1 1 calc R . . . .
C17 C 0.37597(12) 0.85418(13) 0.13296(8) 0.0188(4) Uani 1 1 d . . . . .
C18 C 0.41126(11) 0.84152(13) 0.18874(7) 0.0176(3) Uani 1 1 d . . . . .
H18 H 0.4706 0.8522 0.1959 0.023 Uiso 1 1 calc R . . . .
C19 C 0.36018(11) 0.81323(13) 0.23430(7) 0.0169(3) Uani 1 1 d . . . . .
C20 C 0.13655(12) 0.80118(15) 0.15683(8) 0.0212(4) Uani 1 1 d . . . . .
H20a H 0.1212 0.8211 0.1179 0.032 Uiso 1 1 calc GR . . . .
H20b H 0.1076 0.8460 0.1828 0.032 Uiso 1 1 calc GR . . . .
H20c H 0.1191 0.7305 0.1629 0.032 Uiso 1 1 calc GR . . . .
C21 C 0.43163(13) 0.88539(16) 0.08418(8) 0.0273(4) Uani 1 1 d . . . . .
H21a H 0.4330 0.9598 0.0813 0.041 Uiso 1 1 calc GR . . . .
H21b H 0.4076 0.8566 0.0488 0.041 Uiso 1 1 calc GR . . . .
H21c H 0.4897 0.8596 0.0914 0.041 Uiso 1 1 calc GR . . . .
C22 C 0.40008(12) 0.80966(15) 0.29464(8) 0.0213(4) Uani 1 1 d . . . . .
H22a H 0.3941 0.8764 0.3125 0.032 Uiso 1 1 calc GR . . . .
H22b H 0.4607 0.7923 0.2935 0.032 Uiso 1 1 calc GR . . . .
H22c H 0.3708 0.7580 0.3164 0.032 Uiso 1 1 calc GR . . . .
C23 C 0.28142(10) 0.38618(13) 0.27220(7) 0.0148(3) Uani 1 1 d . . . . .
C24 C 0.30527(11) 0.29148(14) 0.29955(7) 0.0177(3) Uani 1 1 d . . . . .
H24 H 0.3010 0.2855 0.3392 0.024 Uiso 1 1 calc R . . . .
C25 C 0.33488(11) 0.20756(13) 0.26877(8) 0.0183(3) Uani 1 1 d . . . . .
H25 H 0.3490 0.1463 0.2883 0.024 Uiso 1 1 calc R . . . .
C26 C 0.34422(11) 0.21187(13) 0.20956(8) 0.0179(3) Uani 1 1 d . . . . .
C27 C 0.32464(11) 0.30615(13) 0.18264(7) 0.0169(3) Uani 1 1 d . . . . .
H27 H 0.3316 0.3119 0.1433 0.023 Uiso 1 1 calc R . . . .
C28 C 0.29488(11) 0.39253(13) 0.21237(7) 0.0150(3) Uani 1 1 d . . . . .
C29 C 0.37395(14) 0.11877(15) 0.17626(9) 0.0272(4) Uani 1 1 d . . . . .
H29a H 0.3746 0.1360 0.1361 0.041 Uiso 1 1 calc GR . . . .
H29b H 0.3347 0.0619 0.1814 0.041 Uiso 1 1 calc GR . . . .
H29c H 0.4315 0.0992 0.1901 0.041 Uiso 1 1 calc GR . . . .
C30 C 0.22877(12) 0.48765(16) 0.10766(11) 0.0166(5) Uani 0.8 1 d D U P A 1
H30 H 0.2725 0.4468 0.0882 0.022 Uiso 0.8 1 calc R . P A 1
C31 C 0.14561(16) 0.4214(2) 0.10970(16) 0.0216(6) Uani 0.8 1 d G U P A 1
H31a H 0.1576 0.3601 0.1322 0.032 Uiso 0.8 1 calc R . P A 1
H31b H 0.1007 0.4611 0.1268 0.032 Uiso 0.8 1 calc R . P A 1
H31c H 0.1266 0.4017 0.0713 0.032 Uiso 0.8 1 calc R . P A 1
C32 C 0.20960(19) 0.58599(19) 0.07152(14) 0.0266(7) Uani 0.8 1 d G U P A 1
H32a H 0.2615 0.6273 0.0703 0.040 Uiso 0.8 1 calc R . P A 1
H32b H 0.1906 0.5663 0.0331 0.040 Uiso 0.8 1 calc R . P A 1
H32c H 0.1647 0.6257 0.0886 0.040 Uiso 0.8 1 calc R . P A 1
C30' C 0.23840(8) 0.46565(13) 0.09232(2) 0.015(3) Uani 0.2 1 d D U P A 2
H30' H 0.2811 0.4228 0.0732 0.020 Uiso 0.2 1 calc R . P A 2
C31' C 0.15196(9) 0.40623(15) 0.09587(3) 0.026(4) Uani 0.2 1 d G U P A 2
H31a' H 0.1619 0.3426 0.1168 0.039 Uiso 0.2 1 calc R . P A 2
H31b' H 0.1110 0.4483 0.1153 0.039 Uiso 0.2 1 calc R . P A 2
H31c' H 0.1291 0.3907 0.0577 0.039 Uiso 0.2 1 calc R . P A 2
C32' C 0.22245(8) 0.56760(14) 0.05879(3) 0.025(4) Uani 0.2 1 d G U P A 2
H32a' H 0.2764 0.6047 0.0566 0.038 Uiso 0.2 1 calc R . P A 2
H32b' H 0.1995 0.5521 0.0206 0.038 Uiso 0.2 1 calc R . P A 2
H32c' H 0.1815 0.6097 0.0783 0.038 Uiso 0.2 1 calc R . P A 2
C33 C 0.38377(6) 0.57149(8) 0.16708(3) 0.0225(4) Uani 1 1 d G . . . .
H33 H 0.3760 0.6440 0.1549 0.030 Uiso 0.8 1 calc R . P A 1
H33' H 0.3734 0.6436 0.1549 0.030 Uiso 0.2 1 calc R . P A 2
C34 C 0.43618(7) 0.51756(9) 0.12172(3) 0.0306(4) Uani 1 1 d G . . . .
H34a H 0.4915 0.5514 0.1193 0.046 Uiso 1 1 calc GR . . . .
H34b H 0.4049 0.5212 0.0851 0.046 Uiso 1 1 calc GR . . . .
H34c H 0.4451 0.4461 0.1322 0.046 Uiso 1 1 calc GR . . . .
C35 C 0.43539(5) 0.57285(7) 0.22442(3) 0.0251(4) Uani 1 1 d G . . . .
H35a H 0.4540 0.5035 0.2341 0.038 Uiso 1 1 calc GR . . . .
H35b H 0.3994 0.5990 0.2538 0.038 Uiso 1 1 calc GR . . . .
H35c H 0.4854 0.6169 0.2216 0.038 Uiso 1 1 calc GR . . . .
C36 C 0.23706(3) 0.44905(4) 0.36189(2) 0.0150(3) Uani 1 1 d G . . . .
C37 C 0.16627(4) 0.38986(6) 0.37987(3) 0.0165(3) Uani 1 1 d G . . . .
C38 C 0.16048(4) 0.36749(6) 0.43829(3) 0.0191(4) Uani 1 1 d G . . . .
H38 H 0.1128 0.3300 0.4502 0.025 Uiso 1 1 calc R . . . .
C39 C 0.22375(5) 0.39940(6) 0.47931(2) 0.0220(4) Uani 1 1 d G . . . .
C40 C 0.29354(5) 0.45685(6) 0.46047(2) 0.0211(4) Uani 1 1 d G . . . .
H40 H 0.3364 0.4790 0.4873 0.028 Uiso 1 1 calc R . . . .
C41 C 0.30141(4) 0.48230(5) 0.40270(2) 0.0182(3) Uani 1 1 d G . . . .
C42 C 0.10028(5) 0.34630(9) 0.33669(3) 0.0195(4) Uani 1 1 d G . . . .
H42a H 0.1242 0.2864 0.3186 0.029 Uiso 1 1 calc GR . . . .
H42b H 0.0857 0.3980 0.3081 0.029 Uiso 1 1 calc GR . . . .
H42c H 0.0488 0.3267 0.3558 0.029 Uiso 1 1 calc GR . . . .
C43 C 0.21773(6) 0.37154(8) 0.54193(3) 0.0351(5) Uani 1 1 d G . . . .
H43a H 0.1600 0.3472 0.5486 0.053 Uiso 1 1 calc GR . . . .
H43b H 0.2302 0.4318 0.5652 0.053 Uiso 1 1 calc GR . . . .
H43c H 0.2591 0.3178 0.5519 0.053 Uiso 1 1 calc GR . . . .
C44 C 0.37862(5) 0.54257(7) 0.38363(3) 0.0240(4) Uani 1 1 d G . . . .
H44a H 0.4102 0.5013 0.3573 0.036 Uiso 1 1 calc GR . . . .
H44b H 0.4160 0.5595 0.4165 0.036 Uiso 1 1 calc GR . . . .
H44c H 0.3590 0.6054 0.3649 0.036 Uiso 1 1 calc GR . . . .


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 P1 2.6810(5) . ?
Ti1 P2 2.6656(10) . ?
Ti1 N3 1.747(2) . ?
Ti1 N3' 1.769(7) . ?
Ti1 N1 2.0987(15) . ?
Ti1 N2 2.0605(14) . ?
P1 C6 1.8048(17) . ?
P1 C8 1.8560(18) . ?
P1 C11 1.8649(18) . ?
P2 C28 1.810(2) . ?
P2 C30 1.847(3) . ?
P2 C33 1.8614(16) . ?
P2' N3' 1.604(8) . ?
P2' C28 1.834(7) . ?
P2' C30' 1.813(5) . ?
P2' C33 1.805(7) . ?
N1 C1 1.399(2) . ?
N1 C14 1.441(2) . ?
N2 C23 1.404(2) . ?
N2 C36 1.4350(15) . ?
C1 C2 1.413(2) . ?
C1 C6 1.410(2) . ?
C2 C3 1.385(3) . ?
C3 C4 1.396(3) . ?
C4 C5 1.392(3) . ?
C4 C7 1.511(3) . ?
C5 C6 1.397(2) . ?
C8 C9 1.526(2) . ?
C8 C10 1.529(3) . ?
C11 C12 1.527(3) . ?
C11 C13 1.533(3) . ?
C14 C15 1.406(2) . ?
C14 C19 1.403(2) . ?
C15 C16 1.395(2) . ?
C15 C20 1.505(2) . ?
C16 C17 1.388(3) . ?
C17 C18 1.392(3) . ?
C17 C21 1.508(2) . ?
C18 C19 1.397(2) . ?
C19 C22 1.505(2) . ?
C23 C24 1.414(2) . ?
C23 C28 1.419(2) . ?
C24 C25 1.384(2) . ?
C25 C26 1.392(2) . ?
C26 C27 1.391(2) . ?
C26 C29 1.509(2) . ?
C27 C28 1.397(2) . ?
C30 C31 1.5387 . ?
C30 C32 1.5392 . ?
C30' C31' 1.5383 . ?
C30' C32' 1.5394 . ?
C33 C34 1.5245 . ?
C33 C35 1.5189 . ?
C36 C37 1.4078 . ?
C36 C41 1.4044 . ?
C37 C38 1.3958 . ?
C37 C42 1.5013 . ?
C38 C39 1.3913 . ?
C39 C40 1.3905 . ?
C39 C43 1.5069 . ?
C40 C41 1.3937 . ?
C41 C44 1.5020 . ?

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
P2 Ti1 P1 177.16(3) . . ?
N3 Ti1 P1 92.52(6) . . ?
N3 Ti1 P2 90.22(7) . . ?
N3 Ti1 N1 118.62(7) . . ?
N3 Ti1 N2 110.37(7) . . ?
N3' Ti1 P1 159.1(2) . . ?
N3' Ti1 N1 92.2(2) . . ?
N3' Ti1 N2 98.2(2) . . ?
N1 Ti1 P1 74.94(4) . . ?
N1 Ti1 P2 104.36(5) . . ?
N2 Ti1 P1 102.62(4) . . ?
N2 Ti1 P2 75.70(5) . . ?
N2 Ti1 N1 130.99(6) . . ?
C6 P1 Ti1 98.78(6) . . ?
C6 P1 C8 103.68(8) . . ?
C6 P1 C11 105.27(8) . . ?
C8 P1 Ti1 115.97(6) . . ?
C8 P1 C11 105.84(8) . . ?
C11 P1 Ti1 124.46(6) . . ?
C28 P2 Ti1 97.34(7) . . ?
C28 P2 C30 103.26(10) . . ?
C28 P2 C33 104.33(9) . . ?
C30 P2 Ti1 125.50(9) . . ?
C30 P2 C33 103.09(9) . . ?
C33 P2 Ti1 119.76(6) . . ?
N3' P2' C28 105.6(4) . . ?
N3' P2' C30' 112.7(5) . . ?
N3' P2' C33 102.5(4) . . ?
C30' P2' C28 112.5(3) . . ?
C33 P2' C28 105.6(3) . . ?
C33 P2' C30' 116.8(3) . . ?
P2' N3' Ti1 134.8(5) . . ?
C1 N1 Ti1 128.40(11) . . ?
C1 N1 C14 113.60(14) . . ?
C14 N1 Ti1 116.81(10) . . ?
C23 N2 Ti1 126.42(11) . . ?
C23 N2 C36 113.03(12) . . ?
C36 N2 Ti1 118.75(8) . . ?
N1 C1 C2 123.20(15) . . ?
N1 C1 C6 120.35(15) . . ?
C6 C1 C2 116.44(15) . . ?
C3 C2 C1 121.48(17) . . ?
C2 C3 C4 122.31(17) . . ?
C3 C4 C7 121.95(17) . . ?
C5 C4 C3 116.37(16) . . ?
C5 C4 C7 121.68(17) . . ?
C4 C5 C6 122.57(16) . . ?
C1 C6 P1 116.27(13) . . ?
C5 C6 P1 122.91(13) . . ?
C5 C6 C1 120.82(16) . . ?
C9 C8 P1 111.59(12) . . ?
C9 C8 C10 110.77(15) . . ?
C10 C8 P1 110.13(12) . . ?
C12 C11 P1 109.00(13) . . ?
C12 C11 C13 110.68(16) . . ?
C13 C11 P1 117.11(13) . . ?
C15 C14 N1 118.78(15) . . ?
C19 C14 N1 121.34(15) . . ?
C19 C14 C15 119.84(15) . . ?
C14 C15 C20 120.20(15) . . ?
C16 C15 C14 118.98(16) . . ?
C16 C15 C20 120.79(16) . . ?
C17 C16 C15 122.02(16) . . ?
C16 C17 C18 117.97(16) . . ?
C16 C17 C21 120.49(17) . . ?
C18 C17 C21 121.51(17) . . ?
C17 C18 C19 121.97(16) . . ?
C14 C19 C22 121.29(16) . . ?
C18 C19 C14 118.90(16) . . ?
C18 C19 C22 119.76(16) . . ?
N2 C23 C24 122.60(15) . . ?
N2 C23 C28 121.05(15) . . ?
C24 C23 C28 116.35(15) . . ?
C25 C24 C23 121.58(16) . . ?
C24 C25 C26 122.16(16) . . ?
C25 C26 C29 121.60(16) . . ?
C27 C26 C25 116.71(16) . . ?
C27 C26 C29 121.68(16) . . ?
C26 C27 C28 122.64(16) . . ?
C23 C28 P2 114.80(13) . . ?
C23 C28 P2' 129.51(18) . . ?
C27 C28 P2 124.77(13) . . ?
C27 C28 P2' 110.07(18) . . ?
C27 C28 C23 120.40(15) . . ?
C31 C30 P2 111.59(19) . . ?
C31 C30 C32 109.5 . . ?
C32 C30 P2 112.04(18) . . ?
C31' C30' P2' 111.0(2) . . ?
C31' C30' C32' 109.5 . . ?
C32' C30' P2' 105.9(2) . . ?
C34 C33 P2 117.9 . . ?
C34 C33 P2' 103.73(13) . . ?
C35 C33 P2 107.2 . . ?
C35 C33 P2' 117.90(17) . . ?
C35 C33 C34 110.0 . . ?
C37 C36 N2 120.45(6) . . ?
C41 C36 N2 119.89(6) . . ?
C41 C36 C37 119.6 . . ?
C36 C37 C42 120.7 . . ?
C38 C37 C36 119.1 . . ?
C38 C37 C42 120.1 . . ?
C39 C38 C37 122.1 . . ?
C38 C39 C43 121.3 . . ?
C40 C39 C38 117.7 . . ?
C40 C39 C43 121.0 . . ?
C39 C40 C41 122.2 . . ?
C36 C41 C44 119.9 . . ?
C40 C41 C36 119.3 . . ?
C40 C41 C44 120.8 . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.500 308 93 ' '
2 0.500 0.500 0.000 308 93 ' '
_platon_squeeze_void_probe_radius 1.20
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_9191
_database_code_depnum_ccdc_archive 'CCDC 1490142'
_audit_update_record             
;
2016-07-04 deposited with the CCDC.
2016-09-22 downloaded from the CCDC.
;

# Crystallographer: Brian C. Manor

# Compound 8

_audit_creation_date             2016-06-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_formula_moiety         'C44 H62 N2 O P2 Ti'
_chemical_formula_sum            'C44 H62 N2 O P2 Ti'
_chemical_formula_weight         744.79

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.5295(4)
_cell_length_b                   19.5970(6)
_cell_length_c                   16.8163(5)
_cell_angle_alpha                90
_cell_angle_beta                 111.694(2)
_cell_angle_gamma                90
_cell_volume                     4142.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      2.45
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  0.745552
_exptl_absorpt_correction_T_min  0.567959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS v2012/1'
_exptl_crystal_color             'dark orange'
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       prism
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_diffrn_reflns_av_R_equivalents  0.0998
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            121090
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         1.620
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_number_gt                7230
_reflns_number_total             9527
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        'Bruker SAINT v8.34A'
_computing_molecular_graphics    'Mercury v3.6'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         9527
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0582
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0766P)²+2.2453P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1504
_refine_special_details          
;
 Refined as a 2-component twin.
 Scales: 0.5035(11) 0.4965(11)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct

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
Ti1 Ti 0.39041(5) 0.67127(3) 0.35572(4) 0.02131(14) Uani 1 1 d . . . . .
P1 P 0.59170(7) 0.70780(4) 0.43763(5) 0.02118(18) Uani 1 1 d . . . . .
P2 P 0.18769(7) 0.63674(4) 0.27319(5) 0.02393(19) Uani 1 1 d . . . . .
O1 O 0.3788(2) 0.64824(12) 0.44589(14) 0.0303(5) Uani 1 1 d . . . . .
N1 N 0.3908(2) 0.77643(13) 0.33934(16) 0.0224(5) Uani 1 1 d . . . . .
N2 N 0.3974(2) 0.58939(13) 0.27952(17) 0.0229(6) Uani 1 1 d . . . . .
C1 C 0.4688(3) 0.82268(16) 0.3871(2) 0.0231(7) Uani 1 1 d . . . . .
C2 C 0.4536(3) 0.89378(16) 0.3829(2) 0.0251(7) Uani 1 1 d . . . . .
H2 H 0.3893 0.9116 0.3462 0.033 Uiso 1 1 calc R . . . .
C3 C 0.5321(3) 0.93758(17) 0.4322(2) 0.0264(7) Uani 1 1 d . . . . .
H3 H 0.5190 0.9843 0.4276 0.035 Uiso 1 1 calc R . . . .
C4 C 0.6301(3) 0.91455(16) 0.4884(2) 0.0246(7) Uani 1 1 d . . . . .
C5 C 0.6468(3) 0.84430(16) 0.4929(2) 0.0250(7) Uani 1 1 d . . . . .
H5 H 0.7113 0.8272 0.5304 0.033 Uiso 1 1 calc R . . . .
C6 C 0.5690(3) 0.79843(16) 0.4427(2) 0.0224(7) Uani 1 1 d . . . . .
C7 C 0.7161(3) 0.96389(18) 0.5387(2) 0.0302(8) Uani 1 1 d . . . . .
H7a H 0.7369 0.9910 0.5000 0.045 Uiso 1 1 calc GR . . . .
H7b H 0.7765 0.9389 0.5760 0.045 Uiso 1 1 calc GR . . . .
H7c H 0.6896 0.9931 0.5721 0.045 Uiso 1 1 calc GR . . . .
C8 C 0.6617(3) 0.68138(17) 0.5502(2) 0.0252(7) Uani 1 1 d . . . . .
H8 H 0.7254 0.7098 0.5747 0.034 Uiso 1 1 calc R . . . .
C9 C 0.5919(3) 0.69331(18) 0.6021(2) 0.0323(8) Uani 1 1 d . . . . .
H9a H 0.5247 0.6709 0.5747 0.048 Uiso 1 1 calc GR . . . .
H9b H 0.5805 0.7414 0.6056 0.048 Uiso 1 1 calc GR . . . .
H9c H 0.6264 0.6751 0.6586 0.048 Uiso 1 1 calc GR . . . .
C10 C 0.6971(3) 0.60670(17) 0.5570(2) 0.0298(8) Uani 1 1 d . . . . .
H10a H 0.7400 0.5963 0.6154 0.045 Uiso 1 1 calc GR . . . .
H10b H 0.7378 0.5993 0.5216 0.045 Uiso 1 1 calc GR . . . .
H10c H 0.6356 0.5776 0.5383 0.045 Uiso 1 1 calc GR . . . .
C11 C 0.6913(3) 0.70111(17) 0.3862(2) 0.0250(7) Uani 1 1 d . . . . .
H11 H 0.6957 0.6528 0.3727 0.033 Uiso 1 1 calc R . . . .
C12 C 0.6498(3) 0.73977(17) 0.3014(2) 0.0287(7) Uani 1 1 d . . . . .
H12a H 0.6552 0.7880 0.3124 0.043 Uiso 1 1 calc GR . . . .
H12b H 0.5767 0.7279 0.2706 0.043 Uiso 1 1 calc GR . . . .
H12c H 0.6913 0.7278 0.2680 0.043 Uiso 1 1 calc GR . . . .
C13 C 0.8038(3) 0.72437(19) 0.4405(2) 0.0331(8) Uani 1 1 d . . . . .
H13a H 0.8498 0.7171 0.4094 0.050 Uiso 1 1 calc GR . . . .
H13b H 0.8294 0.6986 0.4928 0.050 Uiso 1 1 calc GR . . . .
H13c H 0.8029 0.7720 0.4535 0.050 Uiso 1 1 calc GR . . . .
C14 C 0.2913(3) 0.80816(16) 0.2883(2) 0.0246(7) Uani 1 1 d . . . . .
C15 C 0.2175(3) 0.82458(17) 0.3259(2) 0.0288(7) Uani 1 1 d . . . . .
C16 C 0.1200(3) 0.85270(19) 0.2754(3) 0.0366(9) Uani 1 1 d . . . . .
H16 H 0.0702 0.8626 0.2999 0.049 Uiso 1 1 calc R . . . .
C17 C 0.0953(3) 0.86638(19) 0.1886(3) 0.0371(9) Uani 1 1 d . . . . .
C18 C 0.1715(3) 0.85349(18) 0.1544(2) 0.0334(8) Uani 1 1 d . . . . .
H18 H 0.1561 0.8636 0.0971 0.044 Uiso 1 1 calc R . . . .
C19 C 0.2705(3) 0.82594(16) 0.2023(2) 0.0269(7) Uani 1 1 d . . . . .
C20 C 0.2464(3) 0.8162(2) 0.4217(2) 0.0356(8) Uani 1 1 d . . . . .
H20a H 0.3009 0.8484 0.4517 0.053 Uiso 1 1 calc GR . . . .
H20b H 0.2720 0.7707 0.4383 0.053 Uiso 1 1 calc GR . . . .
H20c H 0.1847 0.8242 0.4356 0.053 Uiso 1 1 calc GR . . . .
C21 C -0.0123(3) 0.8956(2) 0.1353(3) 0.0518(12) Uani 1 1 d . . . . .
H21a H -0.0137 0.9068 0.0794 0.078 Uiso 1 1 calc GR . . . .
H21b H -0.0249 0.9361 0.1624 0.078 Uiso 1 1 calc GR . . . .
H21c H -0.0666 0.8626 0.1305 0.078 Uiso 1 1 calc GR . . . .
C22 C 0.3535(3) 0.81798(18) 0.1640(2) 0.0333(8) Uani 1 1 d . . . . .
H22a H 0.4040 0.8545 0.1831 0.050 Uiso 1 1 calc GR . . . .
H22b H 0.3204 0.8191 0.1027 0.050 Uiso 1 1 calc GR . . . .
H22c H 0.3894 0.7751 0.1816 0.050 Uiso 1 1 calc GR . . . .
C23 C 0.3169(3) 0.54228(16) 0.2408(2) 0.0243(7) Uani 1 1 d . . . . .
C24 C 0.3355(3) 0.48105(17) 0.2040(2) 0.0280(7) Uani 1 1 d . . . . .
H24 H 0.4042 0.4702 0.2083 0.037 Uiso 1 1 calc R . . . .
C25 C 0.2527(3) 0.43706(18) 0.1619(2) 0.0333(8) Uani 1 1 d . . . . .
H25 H 0.2674 0.3976 0.1376 0.044 Uiso 1 1 calc R . . . .
C26 C 0.1485(3) 0.44938(19) 0.1544(3) 0.0369(9) Uani 1 1 d . . . . .
C27 C 0.1304(3) 0.50838(19) 0.1926(2) 0.0319(8) Uani 1 1 d . . . . .
H27 H 0.0620 0.5173 0.1906 0.042 Uiso 1 1 calc R . . . .
C28 C 0.2118(3) 0.55490(17) 0.2340(2) 0.0270(7) Uani 1 1 d . . . . .
C29 C 0.0592(4) 0.4021(2) 0.1041(3) 0.0553(13) Uani 1 1 d . . . . .
H29a H 0.0637 0.3926 0.0495 0.083 Uiso 1 1 calc GR . . . .
H29b H -0.0079 0.4233 0.0957 0.083 Uiso 1 1 calc GR . . . .
H29c H 0.0650 0.3602 0.1351 0.083 Uiso 1 1 calc GR . . . .
C30 C 0.1047(3) 0.61537(18) 0.3368(2) 0.0286(8) Uani 1 1 d . . . . .
H30 H 0.0414 0.5914 0.2987 0.038 Uiso 1 1 calc R . . . .
C31 C 0.1633(3) 0.56711(19) 0.4101(2) 0.0326(8) Uani 1 1 d . . . . .
H31a H 0.2239 0.5901 0.4504 0.049 Uiso 1 1 calc GR . . . .
H31b H 0.1867 0.5277 0.3879 0.049 Uiso 1 1 calc GR . . . .
H31c H 0.1164 0.5531 0.4381 0.049 Uiso 1 1 calc GR . . . .
C32 C 0.0669(4) 0.6788(2) 0.3698(3) 0.0424(10) Uani 1 1 d . . . . .
H32a H 0.0167 0.6659 0.3951 0.064 Uiso 1 1 calc GR . . . .
H32b H 0.0336 0.7096 0.3230 0.064 Uiso 1 1 calc GR . . . .
H32c H 0.1267 0.7010 0.4119 0.064 Uiso 1 1 calc GR . . . .
C33 C 0.0984(3) 0.6826(2) 0.1772(2) 0.0325(8) Uani 1 1 d . . . . .
H33 H 0.0995 0.7307 0.1933 0.043 Uiso 1 1 calc R . . . .
C34 C 0.1454(3) 0.6790(2) 0.1079(2) 0.0363(9) Uani 1 1 d . . . . .
H34a H 0.1374 0.6335 0.0850 0.054 Uiso 1 1 calc GR . . . .
H34b H 0.2195 0.6905 0.1319 0.054 Uiso 1 1 calc GR . . . .
H34c H 0.1088 0.7105 0.0629 0.054 Uiso 1 1 calc GR . . . .
C35 C -0.0183(3) 0.6605(2) 0.1416(3) 0.0476(11) Uani 1 1 d . . . . .
H35a H -0.0566 0.6871 0.0918 0.071 Uiso 1 1 calc GR . . . .
H35b H -0.0488 0.6674 0.1842 0.071 Uiso 1 1 calc GR . . . .
H35c H -0.0229 0.6130 0.1263 0.071 Uiso 1 1 calc GR . . . .
C36 C 0.4995(3) 0.57184(16) 0.2781(2) 0.0234(7) Uani 1 1 d . . . . .
C37 C 0.5690(3) 0.52877(16) 0.3414(2) 0.0253(7) Uani 1 1 d . . . . .
C38 C 0.6711(3) 0.51676(17) 0.3423(2) 0.0272(7) Uani 1 1 d . . . . .
H38 H 0.7175 0.4894 0.3850 0.036 Uiso 1 1 calc R . . . .
C39 C 0.7052(3) 0.54496(17) 0.2805(2) 0.0276(7) Uani 1 1 d . . . . .
C40 C 0.6317(3) 0.58177(16) 0.2143(2) 0.0267(7) Uani 1 1 d . . . . .
H40 H 0.6519 0.5984 0.1707 0.036 Uiso 1 1 calc R . . . .
C41 C 0.5294(3) 0.59468(16) 0.2106(2) 0.0244(7) Uani 1 1 d . . . . .
C42 C 0.5310(3) 0.49383(17) 0.4048(2) 0.0296(7) Uani 1 1 d . . . . .
H42a H 0.5001 0.5270 0.4307 0.044 Uiso 1 1 calc GR . . . .
H42b H 0.5900 0.4721 0.4482 0.044 Uiso 1 1 calc GR . . . .
H42c H 0.4785 0.4602 0.3757 0.044 Uiso 1 1 calc GR . . . .
C43 C 0.8176(3) 0.5355(2) 0.2851(3) 0.0380(9) Uani 1 1 d . . . . .
H43a H 0.8198 0.4989 0.2478 0.057 Uiso 1 1 calc GR . . . .
H43b H 0.8628 0.5248 0.3428 0.057 Uiso 1 1 calc GR . . . .
H43c H 0.8418 0.5769 0.2676 0.057 Uiso 1 1 calc GR . . . .
C44 C 0.4510(3) 0.63116(18) 0.1353(2) 0.0295(8) Uani 1 1 d . . . . .
H44a H 0.4794 0.6353 0.0910 0.044 Uiso 1 1 calc GR . . . .
H44b H 0.4375 0.6758 0.1526 0.044 Uiso 1 1 calc GR . . . .
H44c H 0.3857 0.6058 0.1141 0.044 Uiso 1 1 calc GR . . . .


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 P1 2.6559(10) . ?
Ti1 P2 2.6632(11) . ?
Ti1 O1 1.644(2) . ?
Ti1 N1 2.079(3) . ?
Ti1 N2 2.077(3) . ?
P1 C6 1.810(3) . ?
P1 C8 1.851(3) . ?
P1 C11 1.855(3) . ?
P2 C28 1.808(3) . ?
P2 C30 1.863(4) . ?
P2 C33 1.852(4) . ?
N1 C1 1.398(4) . ?
N1 C14 1.443(4) . ?
N2 C23 1.392(4) . ?
N2 C36 1.433(4) . ?
C1 C2 1.406(4) . ?
C1 C6 1.414(4) . ?
C2 C3 1.378(5) . ?
C3 C4 1.389(5) . ?
C4 C5 1.393(4) . ?
C4 C7 1.508(5) . ?
C5 C6 1.404(5) . ?
C8 C9 1.522(5) . ?
C8 C10 1.531(5) . ?
C11 C12 1.527(5) . ?
C11 C13 1.527(5) . ?
C14 C15 1.403(5) . ?
C14 C19 1.411(5) . ?
C15 C16 1.392(5) . ?
C15 C20 1.519(5) . ?
C16 C17 1.397(6) . ?
C17 C18 1.376(6) . ?
C17 C21 1.512(5) . ?
C18 C19 1.393(5) . ?
C19 C22 1.494(5) . ?
C23 C24 1.414(4) . ?
C23 C28 1.406(5) . ?
C24 C25 1.383(5) . ?
C25 C26 1.389(5) . ?
C26 C27 1.388(5) . ?
C26 C29 1.510(5) . ?
C27 C28 1.400(5) . ?
C30 C31 1.522(5) . ?
C30 C32 1.524(5) . ?
C33 C34 1.522(5) . ?
C33 C35 1.530(5) . ?
C36 C37 1.410(5) . ?
C36 C41 1.411(4) . ?
C37 C38 1.395(5) . ?
C37 C42 1.508(4) . ?
C38 C39 1.399(5) . ?
C39 C40 1.389(5) . ?
C39 C43 1.505(5) . ?
C40 C41 1.386(5) . ?
C41 C44 1.500(5) . ?

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
P1 Ti1 P2 179.08(3) . . ?
O1 Ti1 P1 91.42(9) . . ?
O1 Ti1 P2 88.85(9) . . ?
O1 Ti1 N1 113.58(11) . . ?
O1 Ti1 N2 113.49(11) . . ?
N1 Ti1 P1 75.47(8) . . ?
N1 Ti1 P2 103.62(8) . . ?
N2 Ti1 P1 104.86(8) . . ?
N2 Ti1 P2 75.83(8) . . ?
N2 Ti1 N1 132.91(10) . . ?
C6 P1 Ti1 97.46(11) . . ?
C6 P1 C8 104.94(15) . . ?
C6 P1 C11 104.85(15) . . ?
C8 P1 Ti1 119.60(11) . . ?
C8 P1 C11 105.78(15) . . ?
C11 P1 Ti1 121.43(11) . . ?
C28 P2 Ti1 97.21(12) . . ?
C28 P2 C30 103.76(16) . . ?
C28 P2 C33 105.07(17) . . ?
C30 P2 Ti1 118.75(12) . . ?
C33 P2 Ti1 123.04(12) . . ?
C33 P2 C30 105.81(17) . . ?
C1 N1 Ti1 127.2(2) . . ?
C1 N1 C14 113.8(2) . . ?
C14 N1 Ti1 117.3(2) . . ?
C23 N2 Ti1 126.5(2) . . ?
C23 N2 C36 115.2(3) . . ?
C36 N2 Ti1 117.4(2) . . ?
N1 C1 C2 123.3(3) . . ?
N1 C1 C6 119.8(3) . . ?
C2 C1 C6 116.9(3) . . ?
C3 C2 C1 121.4(3) . . ?
C2 C3 C4 122.4(3) . . ?
C3 C4 C5 116.9(3) . . ?
C3 C4 C7 121.2(3) . . ?
C5 C4 C7 121.8(3) . . ?
C4 C5 C6 122.0(3) . . ?
C1 C6 P1 115.9(2) . . ?
C5 C6 P1 123.7(3) . . ?
C5 C6 C1 120.3(3) . . ?
C9 C8 P1 110.6(2) . . ?
C9 C8 C10 110.3(3) . . ?
C10 C8 P1 111.8(2) . . ?
C12 C11 P1 108.7(2) . . ?
C13 C11 P1 115.8(2) . . ?
C13 C11 C12 110.6(3) . . ?
C15 C14 N1 119.6(3) . . ?
C15 C14 C19 120.1(3) . . ?
C19 C14 N1 120.3(3) . . ?
C14 C15 C20 120.4(3) . . ?
C16 C15 C14 119.1(3) . . ?
C16 C15 C20 120.3(3) . . ?
C15 C16 C17 121.4(4) . . ?
C16 C17 C21 119.8(4) . . ?
C18 C17 C16 118.3(3) . . ?
C18 C17 C21 121.9(4) . . ?
C17 C18 C19 122.6(3) . . ?
C14 C19 C22 121.3(3) . . ?
C18 C19 C14 118.2(3) . . ?
C18 C19 C22 120.5(3) . . ?
N2 C23 C24 122.2(3) . . ?
N2 C23 C28 120.9(3) . . ?
C28 C23 C24 116.9(3) . . ?
C25 C24 C23 120.8(3) . . ?
C24 C25 C26 122.7(3) . . ?
C25 C26 C29 121.3(3) . . ?
C27 C26 C25 116.7(3) . . ?
C27 C26 C29 122.0(4) . . ?
C26 C27 C28 122.2(3) . . ?
C23 C28 P2 116.1(2) . . ?
C27 C28 P2 123.0(3) . . ?
C27 C28 C23 120.7(3) . . ?
C31 C30 P2 111.1(2) . . ?
C31 C30 C32 110.9(3) . . ?
C32 C30 P2 112.3(2) . . ?
C34 C33 P2 108.8(3) . . ?
C34 C33 C35 110.5(3) . . ?
C35 C33 P2 116.8(3) . . ?
C37 C36 N2 120.6(3) . . ?
C37 C36 C41 119.2(3) . . ?
C41 C36 N2 120.1(3) . . ?
C36 C37 C42 119.9(3) . . ?
C38 C37 C36 119.3(3) . . ?
C38 C37 C42 120.7(3) . . ?
C37 C38 C39 121.5(3) . . ?
C38 C39 C43 121.2(3) . . ?
C40 C39 C38 117.8(3) . . ?
C40 C39 C43 121.0(3) . . ?
C41 C40 C39 122.5(3) . . ?
C36 C41 C44 120.4(3) . . ?
C40 C41 C36 119.0(3) . . ?
C40 C41 C44 120.5(3) . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_9205
_database_code_depnum_ccdc_archive 'CCDC 1490143'
_audit_update_record             
;
2016-07-04 deposited with the CCDC.
2016-09-22 downloaded from the CCDC.
;

# Crystallographer: Patrick J. Carroll

# Compound 3

_audit_creation_date             2016-06-25
_audit_creation_method           
;
Olex2 1.2-dev
(compiled 2016.05.11 svn.r3296 for OlexSys, GUI svn.r5177)
;
_chemical_formula_moiety         'C45 H65 N3 P2 Ti, C5 H12'
_chemical_formula_sum            'C50 H77 N3 P2 Ti'
_chemical_formula_weight         829.98

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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'

_cell_length_a                   12.7371(6)
_cell_length_b                   14.7015(7)
_cell_length_c                   26.1005(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4887.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.63
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/4'
_exptl_crystal_color             'reddish orange'
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_description       plate
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.06
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            100964
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.619
_diffrn_reflns_theta_min         1.560
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                10377
_reflns_number_total             11259
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        'Bruker SAINT v8.34A'
_computing_molecular_graphics    'Mercury v3.6'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 
;
 Flack x determined using 4346 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_chemical_absolute_configuration ad
_refine_ls_abs_structure_Flack   0.023(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         11259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0589
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0447P)²+9.5891P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1483
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual

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
Ti1 Ti 0.25009(6) 0.38204(5) 0.17526(3) 0.01467(17) Uani 1 1 d . . . . .
P1 P 0.18350(9) 0.55511(8) 0.17703(5) 0.0166(2) Uani 1 1 d . . . . .
P2 P 0.31402(9) 0.21030(8) 0.16131(4) 0.0157(2) Uani 1 1 d . . . . .
N1 N 0.3732(3) 0.4572(3) 0.14279(14) 0.0154(7) Uani 1 1 d . . . . .
N2 N 0.1229(3) 0.3171(3) 0.13997(15) 0.0161(8) Uani 1 1 d . . . . .
N3 N 0.2530(4) 0.3736(3) 0.24055(15) 0.0241(8) Uani 1 1 d . . . . .
C1 C 0.3866(3) 0.5515(3) 0.14294(17) 0.0154(8) Uani 1 1 d . . . . .
C2 C 0.4788(4) 0.5942(3) 0.12493(19) 0.0207(10) Uani 1 1 d . . . . .
H2 H 0.5340 0.5578 0.1115 0.028 Uiso 1 1 calc R . . . .
C3 C 0.4909(4) 0.6878(3) 0.1263(2) 0.0230(10) Uani 1 1 d . . . . .
H3 H 0.5543 0.7140 0.1140 0.031 Uiso 1 1 calc R . . . .
C4 C 0.4124(4) 0.7448(3) 0.14545(19) 0.0204(10) Uani 1 1 d . . . . .
C5 C 0.3208(4) 0.7059(3) 0.16248(18) 0.0197(9) Uani 1 1 d . . . . .
H5 H 0.2665 0.7435 0.1756 0.026 Uiso 1 1 calc R . . . .
C6 C 0.3063(3) 0.6101(3) 0.16080(17) 0.0188(9) Uani 1 1 d . . . . .
C7 C 0.4269(4) 0.8470(3) 0.1467(2) 0.0273(11) Uani 1 1 d . . . . .
H7a H 0.3630 0.8757 0.1600 0.041 Uiso 1 1 calc GR . . . .
H7b H 0.4409 0.8693 0.1120 0.041 Uiso 1 1 calc GR . . . .
H7c H 0.4863 0.8622 0.1690 0.041 Uiso 1 1 calc GR . . . .
C8 C 0.0890(4) 0.5984(3) 0.1282(2) 0.0235(10) Uani 1 1 d . . . . .
H8 H 0.0281 0.5555 0.1279 0.031 Uiso 1 1 calc R . . . .
C9 C 0.1400(4) 0.5929(4) 0.0757(2) 0.0327(12) Uani 1 1 d . . . . .
H9a H 0.0862 0.6000 0.0492 0.049 Uiso 1 1 calc GR . . . .
H9b H 0.1746 0.5338 0.0718 0.049 Uiso 1 1 calc GR . . . .
H9c H 0.1922 0.6416 0.0723 0.049 Uiso 1 1 calc GR . . . .
C10 C 0.0446(5) 0.6938(4) 0.1370(3) 0.0427(16) Uani 1 1 d . . . . .
H10a H 0.1018 0.7383 0.1362 0.064 Uiso 1 1 calc GR . . . .
H10b H 0.0096 0.6962 0.1704 0.064 Uiso 1 1 calc GR . . . .
H10c H -0.0062 0.7082 0.1099 0.064 Uiso 1 1 calc GR . . . .
C11 C 0.1417(4) 0.6101(3) 0.23685(19) 0.0235(10) Uani 1 1 d . . . . .
H11 H 0.1284 0.6756 0.2288 0.031 Uiso 1 1 calc R . . . .
C12 C 0.2262(5) 0.6072(4) 0.2782(2) 0.0370(14) Uani 1 1 d . . . . .
H12a H 0.1991 0.6347 0.3097 0.056 Uiso 1 1 calc GR . . . .
H12b H 0.2880 0.6411 0.2666 0.056 Uiso 1 1 calc GR . . . .
H12c H 0.2459 0.5439 0.2849 0.056 Uiso 1 1 calc GR . . . .
C13 C 0.0380(5) 0.5697(4) 0.2553(2) 0.0402(16) Uani 1 1 d . . . . .
H13a H 0.0497 0.5074 0.2674 0.060 Uiso 1 1 calc GR . . . .
H13b H -0.0125 0.5691 0.2270 0.060 Uiso 1 1 calc GR . . . .
H13c H 0.0102 0.6068 0.2834 0.060 Uiso 1 1 calc GR . . . .
C14 C 0.4634(3) 0.4075(3) 0.12429(18) 0.0155(9) Uani 1 1 d . . . . .
C15 C 0.4796(3) 0.3944(3) 0.07190(18) 0.0167(9) Uani 1 1 d . . . . .
C16 C 0.5670(4) 0.3446(3) 0.05592(19) 0.0178(9) Uani 1 1 d . . . . .
H16 H 0.5785 0.3363 0.0203 0.024 Uiso 1 1 calc R . . . .
C17 C 0.6377(3) 0.3069(3) 0.0905(2) 0.0207(10) Uani 1 1 d . . . . .
C18 C 0.6229(3) 0.3253(3) 0.14219(19) 0.0189(9) Uani 1 1 d . . . . .
H18 H 0.6721 0.3022 0.1663 0.025 Uiso 1 1 calc R . . . .
C19 C 0.5385(3) 0.3765(3) 0.15996(18) 0.0174(9) Uani 1 1 d . . . . .
C20 C 0.4072(4) 0.4347(3) 0.03284(18) 0.0203(9) Uani 1 1 d . . . . .
H20a H 0.4186 0.4050 -0.0003 0.030 Uiso 1 1 calc GR . . . .
H20b H 0.4213 0.5000 0.0296 0.030 Uiso 1 1 calc GR . . . .
H20c H 0.3343 0.4255 0.0436 0.030 Uiso 1 1 calc GR . . . .
C21 C 0.7293(4) 0.2501(4) 0.0728(2) 0.0264(11) Uani 1 1 d . . . . .
H21a H 0.7166 0.2290 0.0378 0.040 Uiso 1 1 calc GR . . . .
H21b H 0.7373 0.1975 0.0956 0.040 Uiso 1 1 calc GR . . . .
H21c H 0.7935 0.2868 0.0737 0.040 Uiso 1 1 calc GR . . . .
C22 C 0.5323(4) 0.4035(4) 0.21549(19) 0.0234(10) Uani 1 1 d . . . . .
H22a H 0.5850 0.3697 0.2351 0.035 Uiso 1 1 calc GR . . . .
H22b H 0.4622 0.3897 0.2288 0.035 Uiso 1 1 calc GR . . . .
H22c H 0.5458 0.4689 0.2187 0.035 Uiso 1 1 calc GR . . . .
C23 C 0.1078(3) 0.2251(3) 0.13332(17) 0.0158(9) Uani 1 1 d . . . . .
C24 C 0.0127(4) 0.1873(3) 0.11429(19) 0.0187(9) Uani 1 1 d . . . . .
H24 H -0.0432 0.2268 0.1052 0.025 Uiso 1 1 calc R . . . .
C25 C -0.0002(4) 0.0949(3) 0.1087(2) 0.0218(10) Uani 1 1 d . . . . .
H25 H -0.0648 0.0729 0.0954 0.029 Uiso 1 1 calc R . . . .
C26 C 0.0775(4) 0.0318(3) 0.1218(2) 0.0247(11) Uani 1 1 d . . . . .
C27 C 0.1726(4) 0.0687(3) 0.1399(2) 0.0213(10) Uani 1 1 d . . . . .
H27 H 0.2279 0.0285 0.1491 0.028 Uiso 1 1 calc R . . . .
C28 C 0.1884(4) 0.1617(3) 0.14473(18) 0.0176(9) Uani 1 1 d . . . . .
C29 C 0.0610(5) -0.0693(4) 0.1178(3) 0.0386(15) Uani 1 1 d . . . . .
H29a H 0.1252 -0.1010 0.1283 0.058 Uiso 1 1 calc GR . . . .
H29b H 0.0443 -0.0853 0.0823 0.058 Uiso 1 1 calc GR . . . .
H29c H 0.0029 -0.0875 0.1401 0.058 Uiso 1 1 calc GR . . . .
C30 C 0.3612(4) 0.1387(3) 0.21484(19) 0.0224(10) Uani 1 1 d . . . . .
H30 H 0.3715 0.0757 0.2013 0.030 Uiso 1 1 calc R . . . .
C31 C 0.2804(5) 0.1336(4) 0.2581(2) 0.0373(14) Uani 1 1 d . . . . .
H31a H 0.3091 0.0977 0.2865 0.056 Uiso 1 1 calc GR . . . .
H31b H 0.2161 0.1046 0.2454 0.056 Uiso 1 1 calc GR . . . .
H31c H 0.2641 0.1951 0.2702 0.056 Uiso 1 1 calc GR . . . .
C32 C 0.4669(5) 0.1726(4) 0.2341(3) 0.0395(15) Uani 1 1 d . . . . .
H32a H 0.4585 0.2332 0.2492 0.059 Uiso 1 1 calc GR . . . .
H32b H 0.5165 0.1757 0.2055 0.059 Uiso 1 1 calc GR . . . .
H32c H 0.4938 0.1306 0.2602 0.059 Uiso 1 1 calc GR . . . .
C33 C 0.3988(4) 0.1796(3) 0.10610(19) 0.0205(10) Uani 1 1 d . . . . .
H33 H 0.4619 0.2199 0.1079 0.027 Uiso 1 1 calc R . . . .
C34 C 0.3410(4) 0.2038(4) 0.05654(19) 0.0244(10) Uani 1 1 d . . . . .
H34a H 0.3897 0.1998 0.0276 0.037 Uiso 1 1 calc GR . . . .
H34b H 0.3134 0.2659 0.0590 0.037 Uiso 1 1 calc GR . . . .
H34c H 0.2827 0.1612 0.0513 0.037 Uiso 1 1 calc GR . . . .
C35 C 0.4393(5) 0.0821(4) 0.1043(2) 0.0349(13) Uani 1 1 d . . . . .
H35a H 0.3797 0.0399 0.1038 0.052 Uiso 1 1 calc GR . . . .
H35b H 0.4825 0.0702 0.1347 0.052 Uiso 1 1 calc GR . . . .
H35c H 0.4817 0.0735 0.0734 0.052 Uiso 1 1 calc GR . . . .
C36 C 0.0306(3) 0.3702(3) 0.12883(19) 0.0171(9) Uani 1 1 d . . . . .
C37 C -0.0426(3) 0.3872(3) 0.16769(19) 0.0201(10) Uani 1 1 d . . . . .
C38 C -0.1313(4) 0.4388(3) 0.1561(2) 0.0242(10) Uani 1 1 d . . . . .
H38 H -0.1801 0.4522 0.1825 0.032 Uiso 1 1 calc R . . . .
C39 C -0.1506(4) 0.4712(3) 0.1069(2) 0.0233(10) Uani 1 1 d . . . . .
C40 C -0.0789(3) 0.4498(3) 0.0682(2) 0.0194(9) Uani 1 1 d . . . . .
H40 H -0.0919 0.4699 0.0342 0.026 Uiso 1 1 calc R . . . .
C41 C 0.0114(3) 0.3994(3) 0.07873(19) 0.0183(9) Uani 1 1 d . . . . .
C42 C -0.0294(4) 0.3456(4) 0.2201(2) 0.0290(12) Uani 1 1 d . . . . .
H42a H -0.0351 0.2793 0.2175 0.044 Uiso 1 1 calc GR . . . .
H42b H -0.0842 0.3687 0.2430 0.044 Uiso 1 1 calc GR . . . .
H42c H 0.0398 0.3618 0.2338 0.044 Uiso 1 1 calc GR . . . .
C43 C -0.2467(4) 0.5279(4) 0.0962(2) 0.0318(12) Uani 1 1 d . . . . .
H43a H -0.3061 0.5046 0.1161 0.048 Uiso 1 1 calc GR . . . .
H43b H -0.2636 0.5248 0.0596 0.048 Uiso 1 1 calc GR . . . .
H43c H -0.2331 0.5913 0.1058 0.048 Uiso 1 1 calc GR . . . .
C44 C 0.0844(4) 0.3726(4) 0.03575(18) 0.0232(10) Uani 1 1 d . . . . .
H44a H 0.1573 0.3773 0.0475 0.035 Uiso 1 1 calc GR . . . .
H44b H 0.0736 0.4132 0.0065 0.035 Uiso 1 1 calc GR . . . .
H44c H 0.0697 0.3098 0.0254 0.035 Uiso 1 1 calc GR . . . .
C45 C 0.2529(8) 0.3662(5) 0.2952(2) 0.061(2) Uani 1 1 d . . . . .
H45a H 0.1810 0.3731 0.3080 0.091 Uiso 1 1 calc GR . . . .
H45b H 0.2973 0.4140 0.3099 0.091 Uiso 1 1 calc GR . . . .
H45c H 0.2802 0.3065 0.3052 0.091 Uiso 1 1 calc GR . . . .
C46 C 0.7389(9) 0.9134(6) 0.0638(3) 0.073(3) Uani 1 1 d . . . . .
H46a H 0.7961 0.9341 0.0861 0.109 Uiso 1 1 calc GR . . . .
H46b H 0.6721 0.9181 0.0822 0.109 Uiso 1 1 calc GR . . . .
H46c H 0.7365 0.9514 0.0330 0.109 Uiso 1 1 calc GR . . . .
C47 C 0.7578(7) 0.8151(5) 0.0485(3) 0.0573(19) Uani 1 1 d . . . . .
H47a H 0.7660 0.7788 0.0802 0.076 Uiso 1 1 calc R . . . .
H47b H 0.6941 0.7926 0.0308 0.076 Uiso 1 1 calc R . . . .
C48 C 0.8512(6) 0.7967(6) 0.0145(3) 0.058(2) Uani 1 1 d . . . . .
H48a H 0.9152 0.8191 0.0320 0.078 Uiso 1 1 calc R . . . .
H48b H 0.8430 0.8322 -0.0174 0.078 Uiso 1 1 calc R . . . .
C49 C 0.8677(6) 0.6973(5) 0.0004(3) 0.0525(18) Uani 1 1 d . . . . .
H49a H 0.9321 0.6923 -0.0206 0.070 Uiso 1 1 calc R . . . .
H49b H 0.8793 0.6621 0.0323 0.070 Uiso 1 1 calc R . . . .
C50 C 0.7783(6) 0.6554(6) -0.0284(3) 0.0566(19) Uani 1 1 d . . . . .
H50a H 0.7136 0.6618 -0.0084 0.085 Uiso 1 1 calc GR . . . .
H50b H 0.7928 0.5908 -0.0342 0.085 Uiso 1 1 calc GR . . . .
H50c H 0.7700 0.6864 -0.0614 0.085 Uiso 1 1 calc GR . . . .


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 P1 2.6824(14) . ?
Ti1 P2 2.6778(14) . ?
Ti1 N1 2.097(4) . ?
Ti1 N2 2.094(4) . ?
Ti1 N3 1.709(4) . ?
P1 C6 1.811(5) . ?
P1 C8 1.865(5) . ?
P1 C11 1.837(5) . ?
P2 C28 1.805(5) . ?
P2 C30 1.850(5) . ?
P2 C33 1.856(5) . ?
N1 C1 1.396(6) . ?
N1 C14 1.445(5) . ?
N2 C23 1.377(6) . ?
N2 C36 1.441(6) . ?
N3 C45 1.431(7) . ?
C1 C2 1.413(6) . ?
C1 C6 1.416(6) . ?
C2 C3 1.385(7) . ?
C3 C4 1.396(7) . ?
C4 C5 1.373(7) . ?
C4 C7 1.514(7) . ?
C5 C6 1.421(6) . ?
C8 C9 1.518(8) . ?
C8 C10 1.530(7) . ?
C11 C12 1.526(8) . ?
C11 C13 1.526(7) . ?
C14 C15 1.396(7) . ?
C14 C19 1.411(6) . ?
C15 C16 1.396(6) . ?
C15 C20 1.497(6) . ?
C16 C17 1.391(7) . ?
C17 C18 1.390(7) . ?
C17 C21 1.506(6) . ?
C18 C19 1.391(6) . ?
C19 C22 1.505(7) . ?
C23 C24 1.422(6) . ?
C23 C28 1.419(6) . ?
C24 C25 1.377(7) . ?
C25 C26 1.400(7) . ?
C26 C27 1.408(7) . ?
C26 C29 1.505(7) . ?
C27 C28 1.387(6) . ?
C30 C31 1.530(7) . ?
C30 C32 1.521(7) . ?
C33 C34 1.531(7) . ?
C33 C35 1.523(7) . ?
C36 C37 1.400(6) . ?
C36 C41 1.398(7) . ?
C37 C38 1.394(7) . ?
C37 C42 1.507(7) . ?
C38 C39 1.390(8) . ?
C39 C40 1.397(7) . ?
C39 C43 1.508(7) . ?
C40 C41 1.396(6) . ?
C41 C44 1.509(7) . ?
C46 C47 1.518(11) . ?
C47 C48 1.510(12) . ?
C48 C49 1.521(11) . ?
C49 C50 1.497(10) . ?

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
P2 Ti1 P1 173.15(5) . . ?
N1 Ti1 P1 75.14(10) . . ?
N1 Ti1 P2 102.39(11) . . ?
N2 Ti1 P1 101.28(11) . . ?
N2 Ti1 P2 75.25(11) . . ?
N2 Ti1 N1 129.86(15) . . ?
N3 Ti1 P1 93.36(14) . . ?
N3 Ti1 P2 93.47(14) . . ?
N3 Ti1 N1 115.13(18) . . ?
N3 Ti1 N2 115.00(19) . . ?
C6 P1 Ti1 98.40(16) . . ?
C6 P1 C8 104.2(2) . . ?
C6 P1 C11 104.6(2) . . ?
C8 P1 Ti1 121.06(16) . . ?
C11 P1 Ti1 121.58(18) . . ?
C11 P1 C8 104.1(2) . . ?
C28 P2 Ti1 97.85(15) . . ?
C28 P2 C30 104.1(2) . . ?
C28 P2 C33 103.5(2) . . ?
C30 P2 Ti1 122.18(17) . . ?
C30 P2 C33 105.0(2) . . ?
C33 P2 Ti1 120.79(16) . . ?
C1 N1 Ti1 127.8(3) . . ?
C1 N1 C14 113.9(4) . . ?
C14 N1 Ti1 117.6(3) . . ?
C23 N2 Ti1 127.7(3) . . ?
C23 N2 C36 113.1(4) . . ?
C36 N2 Ti1 118.2(3) . . ?
C45 N3 Ti1 178.6(5) . . ?
N1 C1 C2 122.8(4) . . ?
N1 C1 C6 121.1(4) . . ?
C2 C1 C6 116.0(4) . . ?
C3 C2 C1 121.7(4) . . ?
C2 C3 C4 121.7(4) . . ?
C3 C4 C7 121.0(5) . . ?
C5 C4 C3 118.3(4) . . ?
C5 C4 C7 120.7(4) . . ?
C4 C5 C6 120.9(4) . . ?
C1 C6 P1 115.4(3) . . ?
C1 C6 C5 121.3(4) . . ?
C5 C6 P1 123.2(3) . . ?
C9 C8 P1 108.8(4) . . ?
C9 C8 C10 110.0(5) . . ?
C10 C8 P1 116.7(4) . . ?
C12 C11 P1 112.6(4) . . ?
C12 C11 C13 112.1(5) . . ?
C13 C11 P1 110.4(3) . . ?
C15 C14 N1 121.0(4) . . ?
C15 C14 C19 120.1(4) . . ?
C19 C14 N1 118.8(4) . . ?
C14 C15 C20 121.5(4) . . ?
C16 C15 C14 118.9(4) . . ?
C16 C15 C20 119.7(4) . . ?
C17 C16 C15 122.2(4) . . ?
C16 C17 C21 121.7(5) . . ?
C18 C17 C16 117.7(4) . . ?
C18 C17 C21 120.6(4) . . ?
C17 C18 C19 122.3(4) . . ?
C14 C19 C22 121.0(4) . . ?
C18 C19 C14 118.6(4) . . ?
C18 C19 C22 120.3(4) . . ?
N2 C23 C24 123.2(4) . . ?
N2 C23 C28 121.2(4) . . ?
C28 C23 C24 115.6(4) . . ?
C25 C24 C23 121.7(4) . . ?
C24 C25 C26 122.9(4) . . ?
C25 C26 C27 115.8(4) . . ?
C25 C26 C29 122.6(5) . . ?
C27 C26 C29 121.6(5) . . ?
C28 C27 C26 122.3(4) . . ?
C23 C28 P2 115.5(3) . . ?
C27 C28 P2 122.7(4) . . ?
C27 C28 C23 121.6(4) . . ?
C31 C30 P2 111.6(4) . . ?
C32 C30 P2 110.6(4) . . ?
C32 C30 C31 111.5(5) . . ?
C34 C33 P2 108.6(3) . . ?
C35 C33 P2 116.7(4) . . ?
C35 C33 C34 110.9(5) . . ?
C37 C36 N2 119.6(4) . . ?
C41 C36 N2 119.8(4) . . ?
C41 C36 C37 120.4(4) . . ?
C36 C37 C42 120.7(4) . . ?
C38 C37 C36 118.6(5) . . ?
C38 C37 C42 120.6(4) . . ?
C39 C38 C37 122.0(5) . . ?
C38 C39 C40 118.3(4) . . ?
C38 C39 C43 120.3(5) . . ?
C40 C39 C43 121.4(5) . . ?
C41 C40 C39 121.1(5) . . ?
C36 C41 C44 120.5(4) . . ?
C40 C41 C36 119.4(4) . . ?
C40 C41 C44 120.0(4) . . ?
C48 C47 C46 116.7(8) . . ?
C47 C48 C49 115.0(7) . . ?
C50 C49 C48 114.3(7) . . ?
