# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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 
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data_2b'
_database_code_depnum_ccdc_archive 'CCDC 1985134'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne Franche Comte
France
;
_audit_update_record             
;
2020-02-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_audit_creation_date             2019-06-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H46 Li N2 O P3'
_chemical_formula_sum            'C28 H46 Li N2 O P3'
_chemical_formula_weight         526.52
_chemical_melting_point          ?
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'
Li Li -0.0003 0.0001 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.215(4)
_cell_length_b                   30.038(9)
_cell_length_c                   10.723(4)
_cell_angle_alpha                90
_cell_angle_beta                 116.107(12)
_cell_angle_gamma                90
_cell_volume                     2954.5(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9759
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.94
_shelx_estimated_absorpt_T_max   0.957
_shelx_estimated_absorpt_T_min   0.928
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.6468
_exptl_absorpt_correction_T_min  0.6133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0516 before and 0.0418 after correction. The Ratio of minimum to maximum transmission is 0.9482. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_recrystallization_method 
'The material was recrystallised from pentane by slow evaporation'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            48835
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.547
_diffrn_reflns_theta_min         2.935
_diffrn_ambient_temperature      100.0
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'κ-geometry diffractometer triump Mo'
_diffrn_measurement_device_type  'Bruker D8 Venture triumph Mo'
_diffrn_measurement_method       "φ and ω scans'"
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-90C'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5996
_reflns_number_total             6783
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.025
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         6783
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0680
_refine_ls_restrained_S_all      1.024
_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)+(0.0873P)²+7.4284P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1835
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(C1D) = Uiso(C1E) = Uiso(C1A) = Uiso(C1H)
Uiso(C1G) = Uiso(C1B) = Uiso(C1F) = Uiso(C1C)
Uiso(O1) = Uiso(O2)
3. Others
 Fixed Sof: H7A(0.62) H7B(0.38) C8(0.63) H8A(0.63) H8B(0.63) H8C(0.63)
 C8A(0.37) H8AA(0.37) H8AB(0.37) H8AC(0.37) C10(0.63) H10(0.63) C10A(0.37)
 H10A(0.37) C11(0.63) H11A(0.63) H11B(0.63) H11C(0.63) C11A(0.37) H11D(0.37)
 H11E(0.37) H11F(0.37) H12A(0.62) H12B(0.62) H12C(0.62) H12D(0.38) H12E(0.38)
 H12F(0.38) O2(0.63) C1A(0.63) H1AA(0.63) H1AB(0.63) C1B(0.63) H1BA(0.63)
 H1BB(0.63) C1C(0.63) H1CA(0.63) H1CB(0.63) C1D(0.63) H1DA(0.63) H1DB(0.63)
 O1(0.37) C1E(0.37) H1EA(0.37) H1EB(0.37) C1F(0.37) H1FA(0.37) H1FB(0.37)
 C1G(0.37) H1GA(0.37) H1GB(0.37) C1H(0.37) H1HA(0.37) H1HB(0.37)
4.a Free rotating group:
 O2(C1A,C1B,C1C,C1D), O1(C1E,C1F,C1G,C1H)
4.b Ternary CH refined with riding coordinates:
 C7(H7A), C7(H7B), C10(H10), C10A(H10A), C13(H13), C16(H16)
4.c Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB), C1E(H1EA,
 H1EB), C1F(H1FA,H1FB), C1G(H1GA,H1GB), C1H(H1HA,H1HB)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C20(H20), C21(H21), C22(H22),
 C23(H23), C24(H24)
4.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C11A(H11D,H11E,H11F), C12(H12A,H12B,H12C), C12(H12D,H12E,H12F), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Li Li 0.3845(6) 0.65230(18) 0.7843(6) 0.0358(12) Uani 1 1 d . . . . .
C1 C 0.1532(3) 0.69004(9) 0.7883(3) 0.0230(5) Uani 1 1 d . . . . .
N1 N 0.2409(2) 0.65399(8) 0.8596(2) 0.0238(5) Uani 1 1 d . . . . .
P1 P 0.18265(7) 0.60407(2) 0.86272(7) 0.02256(18) Uani 1 1 d . . . . .
C2 C 0.2238(4) 0.73117(10) 0.7975(3) 0.0310(6) Uani 1 1 d . . . . .
H2 H 0.326389 0.733092 0.851709 0.037 Uiso 1 1 calc R . . . .
N2 N 0.3328(2) 0.60857(7) 0.6375(2) 0.0213(4) Uani 1 1 d . . . . .
P2 P 0.06423(7) 0.56699(2) 0.67660(7) 0.01889(17) Uani 1 1 d . . . . .
C3 C 0.1471(4) 0.76877(10) 0.7295(3) 0.0390(8) Uani 1 1 d . . . . .
H3 H 0.197601 0.796057 0.738700 0.047 Uiso 1 1 calc R . . . .
P3 P 0.18827(6) 0.57842(2) 0.56140(7) 0.01650(16) Uani 1 1 d . . . . .
C4 C -0.0024(4) 0.76712(10) 0.6481(3) 0.0389(8) Uani 1 1 d . . . . .
H4 H -0.054587 0.792880 0.600832 0.047 Uiso 1 1 calc R . . . .
C5 C -0.0740(4) 0.72705(10) 0.6373(3) 0.0322(7) Uani 1 1 d . . . . .
H5 H -0.176507 0.725468 0.582263 0.039 Uiso 1 1 calc R . . . .
C6 C 0.0018(3) 0.68910(9) 0.7058(3) 0.0249(5) Uani 1 1 d . . . . .
H6 H -0.049923 0.662058 0.696663 0.030 Uiso 1 1 calc R . . . .
C7 C 0.0538(4) 0.60560(11) 0.9405(3) 0.0365(7) Uani 1 1 d . . . . .
H7A H -0.026678 0.626542 0.883991 0.044 Uiso 0.62 1 calc R . P A 1
H7B H -0.031650 0.619733 0.862376 0.044 Uiso 0.38 1 calc R . P B 2
C8 C 0.1371(8) 0.6262(2) 1.0865(6) 0.0349(12) Uani 0.63 1 d . . P C 1
H8A H 0.206717 0.604380 1.148622 0.052 Uiso 0.63 1 calc GR . P C 1
H8B H 0.067800 0.634432 1.123005 0.052 Uiso 0.63 1 calc GR . P C 1
H8C H 0.189789 0.652736 1.080578 0.052 Uiso 0.63 1 calc GR . P C 1
C8A C 0.0821(13) 0.6416(4) 1.0591(11) 0.037(2) Uani 0.37 1 d . . P C 2
H8AA H 0.165144 0.632168 1.145033 0.056 Uiso 0.37 1 calc GR . P C 2
H8AB H -0.004855 0.644130 1.075175 0.056 Uiso 0.37 1 calc GR . P C 2
H8AC H 0.103516 0.670476 1.029874 0.056 Uiso 0.37 1 calc GR . P C 2
C9 C -0.0156(4) 0.56197(13) 0.9514(4) 0.0431(8) Uani 1 1 d . . . . .
H9A H -0.052322 0.546210 0.862403 0.065 Uiso 1 1 calc GR . . . .
H9B H -0.096624 0.568064 0.974561 0.065 Uiso 1 1 calc GR . . . .
H9C H 0.057216 0.543501 1.024238 0.065 Uiso 1 1 calc GR . . . .
C10 C 0.3582(5) 0.57272(16) 0.9630(5) 0.0230(9) Uani 0.63 1 d . . P D 1
H10 H 0.401922 0.566441 0.897759 0.028 Uiso 0.63 1 calc R . P D 1
C10A C 0.3303(10) 0.5783(3) 1.0133(11) 0.0318(19) Uani 0.37 1 d . . P D 2
H10A H 0.328485 0.589594 1.100266 0.038 Uiso 0.37 1 calc R . P D 2
C11 C 0.4723(6) 0.59849(19) 1.0875(6) 0.0360(12) Uani 0.63 1 d . . P D 1
H11A H 0.487112 0.627989 1.056803 0.054 Uiso 0.63 1 calc GR . P D 1
H11B H 0.564663 0.582089 1.125909 0.054 Uiso 0.63 1 calc GR . P D 1
H11C H 0.437780 0.601784 1.159022 0.054 Uiso 0.63 1 calc GR . P D 1
C11A C 0.4744(10) 0.5896(4) 1.0147(13) 0.044(2) Uani 0.37 1 d . . P D 2
H11D H 0.471661 0.581966 0.924734 0.066 Uiso 0.37 1 calc GR . P D 2
H11E H 0.552089 0.572650 1.088296 0.066 Uiso 0.37 1 calc GR . P D 2
H11F H 0.493397 0.621532 1.032047 0.066 Uiso 0.37 1 calc GR . P D 2
C12 C 0.3234(4) 0.52697(10) 1.0109(3) 0.0362(7) Uani 1 1 d . . . . .
H12A H 0.267469 0.531917 1.064083 0.054 Uiso 0.62 1 calc GR . P D 1
H12B H 0.414660 0.511639 1.069287 0.054 Uiso 0.62 1 calc GR . P D 1
H12C H 0.266075 0.508660 0.929227 0.054 Uiso 0.62 1 calc GR . P D 1
H12D H 0.231522 0.517203 0.934517 0.054 Uiso 0.38 1 calc GR . P D 2
H12E H 0.328692 0.516128 1.099171 0.054 Uiso 0.38 1 calc GR . P D 2
H12F H 0.405435 0.514996 0.997348 0.054 Uiso 0.38 1 calc GR . P D 2
C13 C 0.2299(3) 0.52268(8) 0.5158(3) 0.0197(5) Uani 1 1 d . . . . .
H13 H 0.139593 0.504302 0.487064 0.024 Uiso 1 1 calc R . . . .
C14 C 0.3485(3) 0.50041(9) 0.6440(3) 0.0233(5) Uani 1 1 d . . . . .
H14A H 0.440699 0.516411 0.671721 0.035 Uiso 1 1 calc GR . . . .
H14B H 0.360503 0.469438 0.622206 0.035 Uiso 1 1 calc GR . . . .
H14C H 0.320253 0.501102 0.720315 0.035 Uiso 1 1 calc GR . . . .
C15 C 0.2710(3) 0.52224(9) 0.3941(3) 0.0267(6) Uani 1 1 d . . . . .
H15A H 0.188892 0.533303 0.310158 0.040 Uiso 1 1 calc GR . . . .
H15B H 0.294411 0.491744 0.378318 0.040 Uiso 1 1 calc GR . . . .
H15C H 0.356097 0.541390 0.416328 0.040 Uiso 1 1 calc GR . . . .
C16 C 0.0588(3) 0.60117(8) 0.3915(3) 0.0201(5) Uani 1 1 d . . . . .
H16 H 0.111238 0.602977 0.331860 0.024 Uiso 1 1 calc R . . . .
C17 C 0.0122(3) 0.64843(9) 0.4068(3) 0.0252(5) Uani 1 1 d . . . . .
H17A H -0.049567 0.647459 0.455429 0.038 Uiso 1 1 calc GR . . . .
H17B H -0.042611 0.661607 0.314580 0.038 Uiso 1 1 calc GR . . . .
H17C H 0.098845 0.666513 0.460148 0.038 Uiso 1 1 calc GR . . . .
C18 C -0.0755(3) 0.57168(10) 0.3156(3) 0.0264(6) Uani 1 1 d . . . . .
H18A H -0.044465 0.541995 0.301482 0.040 Uiso 1 1 calc GR . . . .
H18B H -0.138264 0.584947 0.225308 0.040 Uiso 1 1 calc GR . . . .
H18C H -0.129669 0.569225 0.371323 0.040 Uiso 1 1 calc GR . . . .
C19 C 0.4277(3) 0.61624(9) 0.5758(3) 0.0234(5) Uani 1 1 d . . . . .
C20 C 0.3916(3) 0.64419(12) 0.4615(4) 0.0383(8) Uani 1 1 d . . . . .
H20 H 0.297107 0.657059 0.418333 0.046 Uiso 1 1 calc R . . . .
C21 C 0.4915(4) 0.65347(15) 0.4099(4) 0.0511(10) Uani 1 1 d . . . . .
H21 H 0.464774 0.672709 0.332229 0.061 Uiso 1 1 calc R . . . .
C22 C 0.6297(4) 0.63500(13) 0.4704(4) 0.0456(9) Uani 1 1 d . . . . .
H22 H 0.697073 0.641069 0.433615 0.055 Uiso 1 1 calc R . . . .
C23 C 0.6683(3) 0.60791(11) 0.5838(4) 0.0345(7) Uani 1 1 d . . . . .
H23 H 0.763090 0.595215 0.626030 0.041 Uiso 1 1 calc R . . . .
C24 C 0.5698(3) 0.59884(9) 0.6376(3) 0.0259(6) Uani 1 1 d . . . . .
H24 H 0.599111 0.580553 0.717705 0.031 Uiso 1 1 calc R . . . .
O2 O 0.5672(4) 0.68192(12) 0.8469(4) 0.0404(8) Uiso 0.63 1 d . . P E -1
C1A C 0.5861(5) 0.72269(14) 0.7853(5) 0.0639(12) Uiso 0.63 1 d G . P E -1
H1AA H 0.507370 0.744047 0.772413 0.077 Uiso 0.63 1 calc R . P E -1
H1AB H 0.584133 0.716639 0.693724 0.077 Uiso 0.63 1 calc R . P E -1
C1B C 0.7348(5) 0.74162(13) 0.8862(6) 0.0638(12) Uiso 0.63 1 d G . P E -1
H1BA H 0.726583 0.760637 0.957852 0.077 Uiso 0.63 1 calc R . P E -1
H1BB H 0.779782 0.758957 0.836659 0.077 Uiso 0.63 1 calc R . P E -1
C1C C 0.8212(3) 0.69883(18) 0.9498(6) 0.0638(12) Uiso 0.63 1 d G . P E -1
H1CA H 0.859448 0.685266 0.888333 0.077 Uiso 0.63 1 calc R . P E -1
H1CB H 0.903025 0.704535 1.042185 0.077 Uiso 0.63 1 calc R . P E -1
C1D C 0.7039(5) 0.66948(15) 0.9610(5) 0.0639(12) Uiso 0.63 1 d G . P E -1
H1DA H 0.724880 0.637613 0.954477 0.077 Uiso 0.63 1 calc R . P E -1
H1DB H 0.700503 0.674585 1.050727 0.077 Uiso 0.63 1 calc R . P E -1
O1 O 0.5489(7) 0.6896(2) 0.8178(7) 0.0404(8) Uiso 0.37 1 d . . P E 2
C1E C 0.6948(8) 0.6877(3) 0.9288(7) 0.0639(12) Uiso 0.37 1 d G . P E 2
H1EA H 0.729587 0.656529 0.946706 0.077 Uiso 0.37 1 calc R . P E 2
H1EB H 0.697391 0.700256 1.015264 0.077 Uiso 0.37 1 calc R . P E 2
C1F C 0.7908(6) 0.7153(3) 0.8811(10) 0.0638(12) Uiso 0.37 1 d G . P E 2
H1FA H 0.827915 0.697155 0.826490 0.077 Uiso 0.37 1 calc R . P E 2
H1FB H 0.873991 0.728907 0.960788 0.077 Uiso 0.37 1 calc R . P E 2
C1G C 0.6823(9) 0.7509(2) 0.7903(10) 0.0638(12) Uiso 0.37 1 d G . P E 2
H1GA H 0.671850 0.775310 0.847373 0.077 Uiso 0.37 1 calc R . P E 2
H1GB H 0.711920 0.763528 0.721264 0.077 Uiso 0.37 1 calc R . P E 2
C1H C 0.5414(8) 0.7236(3) 0.7199(7) 0.0639(12) Uiso 0.37 1 d G . P E 2
H1HA H 0.455159 0.742884 0.697264 0.077 Uiso 0.37 1 calc R . P E 2
H1HB H 0.534036 0.710010 0.633047 0.077 Uiso 0.37 1 calc R . P E 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Li N1 1.962(6) . ?
Li N2 1.936(6) . ?
Li O2 1.904(6) . ?
Li O1 1.917(7) . ?
C1 N1 1.399(3) . ?
C1 C2 1.412(4) . ?
C1 C6 1.404(4) . ?
N1 P1 1.619(2) . ?
P1 P2 2.1359(11) . ?
P1 C7 1.843(3) . ?
P1 C10 1.887(5) . ?
P1 C10A 1.827(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.385(4) . ?
N2 P3 1.614(2) . ?
N2 C19 1.413(3) . ?
P2 P3 2.1509(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.387(5) . ?
P3 C13 1.846(3) . ?
P3 C16 1.848(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.392(4) . ?
C6 H6 0.9500 . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C7 C8 1.544(7) . ?
C7 C8A 1.595(11) . ?
C7 C9 1.519(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.540(7) . ?
C10 C12 1.562(6) . ?
C10A H10A 1.0000 . ?
C10A C11A 1.504(15) . ?
C10A C12 1.544(10) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C11A H11D 0.9800 . ?
C11A H11E 0.9800 . ?
C11A H11F 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12 H12D 0.9800 . ?
C12 H12E 0.9800 . ?
C12 H12F 0.9800 . ?
C13 H13 1.0000 . ?
C13 C14 1.530(4) . ?
C13 C15 1.537(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16 1.0000 . ?
C16 C17 1.529(4) . ?
C16 C18 1.532(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.395(4) . ?
C19 C24 1.404(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.386(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.384(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.369(5) . ?
C23 H23 0.9500 . ?
C23 C24 1.389(4) . ?
C24 H24 0.9500 . ?
O2 C1A 1.4441 . ?
O2 C1D 1.4433 . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C1A C1B 1.5341 . ?
C1B H1BA 0.9900 . ?
C1B H1BB 0.9900 . ?
C1B C1C 1.5386 . ?
C1C H1CA 0.9900 . ?
C1C H1CB 0.9900 . ?
C1C C1D 1.5343 . ?
C1D H1DA 0.9900 . ?
C1D H1DB 0.9900 . ?
O1 C1E 1.4426 . ?
O1 C1H 1.4430 . ?
C1E H1EA 0.9900 . ?
C1E H1EB 0.9900 . ?
C1E C1F 1.5342 . ?
C1F H1FA 0.9900 . ?
C1F H1FB 0.9900 . ?
C1F C1G 1.5391 . ?
C1G H1GA 0.9900 . ?
C1G H1GB 0.9900 . ?
C1G C1H 1.5351 . ?
C1H H1HA 0.9900 . ?
C1H H1HB 0.9900 . ?

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
N2 Li N1 111.5(2) . . ?
O2 Li N1 129.6(3) . . ?
O2 Li N2 118.5(3) . . ?
O1 Li N1 131.3(4) . . ?
O1 Li N2 116.9(4) . . ?
N1 C1 C2 117.0(3) . . ?
N1 C1 C6 126.3(2) . . ?
C6 C1 C2 116.7(3) . . ?
C1 N1 Li 102.1(3) . . ?
C1 N1 P1 125.15(19) . . ?
P1 N1 Li 109.4(2) . . ?
N1 P1 P2 121.71(9) . . ?
N1 P1 C7 109.17(14) . . ?
N1 P1 C10 102.03(18) . . ?
N1 P1 C10A 104.0(3) . . ?
C7 P1 P2 102.25(11) . . ?
C7 P1 C10 116.3(2) . . ?
C10 P1 P2 106.12(16) . . ?
C10A P1 P2 120.9(3) . . ?
C10A P1 C7 95.0(4) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 C1 121.5(3) . . ?
C3 C2 H2 119.2 . . ?
P3 N2 Li 130.8(2) . . ?
C19 N2 Li 105.8(2) . . ?
C19 N2 P3 121.21(19) . . ?
P1 P2 P3 102.64(4) . . ?
C2 C3 H3 119.6 . . ?
C2 C3 C4 120.9(3) . . ?
C4 C3 H3 119.6 . . ?
N2 P3 P2 115.98(9) . . ?
N2 P3 C13 112.14(12) . . ?
N2 P3 C16 112.93(12) . . ?
C13 P3 P2 105.67(9) . . ?
C13 P3 C16 102.86(12) . . ?
C16 P3 P2 106.16(9) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 C3 118.6(3) . . ?
C5 C4 H4 120.7 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.1(3) . . ?
C6 C5 H5 119.5 . . ?
C1 C6 H6 119.4 . . ?
C5 C6 C1 121.2(3) . . ?
C5 C6 H6 119.4 . . ?
P1 C7 H7A 107.6 . . ?
P1 C7 H7B 99.5 . . ?
C8 C7 P1 106.5(3) . . ?
C8 C7 H7A 107.6 . . ?
C8A C7 P1 117.5(5) . . ?
C8A C7 H7B 99.5 . . ?
C9 C7 P1 117.6(3) . . ?
C9 C7 H7A 107.6 . . ?
C9 C7 H7B 99.5 . . ?
C9 C7 C8 109.6(3) . . ?
C9 C7 C8A 116.7(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C8A H8AA 109.5 . . ?
C7 C8A H8AB 109.5 . . ?
C7 C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P1 C10 H10 107.5 . . ?
C11 C10 P1 114.2(4) . . ?
C11 C10 H10 107.5 . . ?
C11 C10 C12 110.6(4) . . ?
C12 C10 P1 109.2(3) . . ?
C12 C10 H10 107.5 . . ?
P1 C10A H10A 109.5 . . ?
C11A C10A P1 109.7(7) . . ?
C11A C10A H10A 109.5 . . ?
C11A C10A C12 105.2(8) . . ?
C12 C10A P1 113.2(6) . . ?
C12 C10A H10A 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10A C11A H11D 109.5 . . ?
C10A C11A H11E 109.5 . . ?
C10A C11A H11F 109.5 . . ?
H11D C11A H11E 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
C10A C12 H12D 109.5 . . ?
C10A C12 H12E 109.5 . . ?
C10A C12 H12F 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
H12D C12 H12E 109.5 . . ?
H12D C12 H12F 109.5 . . ?
H12E C12 H12F 109.5 . . ?
P3 C13 H13 107.1 . . ?
C14 C13 P3 110.01(18) . . ?
C14 C13 H13 107.1 . . ?
C14 C13 C15 110.8(2) . . ?
C15 C13 P3 114.44(18) . . ?
C15 C13 H13 107.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
P3 C16 H16 107.3 . . ?
C17 C16 P3 111.05(19) . . ?
C17 C16 H16 107.3 . . ?
C17 C16 C18 110.2(2) . . ?
C18 C16 P3 113.27(18) . . ?
C18 C16 H16 107.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 N2 122.6(2) . . ?
C20 C19 C24 117.2(3) . . ?
C24 C19 N2 119.9(3) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 C19 121.0(3) . . ?
C21 C20 H20 119.5 . . ?
C20 C21 H21 119.7 . . ?
C22 C21 C20 120.7(3) . . ?
C22 C21 H21 119.7 . . ?
C21 C22 H22 120.3 . . ?
C23 C22 C21 119.4(3) . . ?
C23 C22 H22 120.3 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.5(3) . . ?
C24 C23 H23 119.8 . . ?
C19 C24 H24 119.4 . . ?
C23 C24 C19 121.2(3) . . ?
C23 C24 H24 119.4 . . ?
C1A O2 Li 122.9(3) . . ?
C1D O2 Li 127.6(3) . . ?
C1D O2 C1A 109.4 . . ?
O2 C1A H1AA 110.5 . . ?
O2 C1A H1AB 110.5 . . ?
O2 C1A C1B 106.4 . . ?
H1AA C1A H1AB 108.6 . . ?
C1B C1A H1AA 110.5 . . ?
C1B C1A H1AB 110.5 . . ?
C1A C1B H1BA 111.5 . . ?
C1A C1B H1BB 111.5 . . ?
C1A C1B C1C 101.5 . . ?
H1BA C1B H1BB 109.3 . . ?
C1C C1B H1BA 111.5 . . ?
C1C C1B H1BB 111.5 . . ?
C1B C1C H1CA 111.5 . . ?
C1B C1C H1CB 111.5 . . ?
H1CA C1C H1CB 109.3 . . ?
C1D C1C C1B 101.5 . . ?
C1D C1C H1CA 111.5 . . ?
C1D C1C H1CB 111.5 . . ?
O2 C1D C1C 106.4 . . ?
O2 C1D H1DA 110.4 . . ?
O2 C1D H1DB 110.4 . . ?
C1C C1D H1DA 110.4 . . ?
C1C C1D H1DB 110.4 . . ?
H1DA C1D H1DB 108.6 . . ?
C1E O1 Li 129.3(4) . . ?
C1E O1 C1H 109.5 . . ?
C1H O1 Li 121.1(5) . . ?
O1 C1E H1EA 110.4 . . ?
O1 C1E H1EB 110.4 . . ?
O1 C1E C1F 106.5 . . ?
H1EA C1E H1EB 108.6 . . ?
C1F C1E H1EA 110.4 . . ?
C1F C1E H1EB 110.4 . . ?
C1E C1F H1FA 111.5 . . ?
C1E C1F H1FB 111.5 . . ?
C1E C1F C1G 101.5 . . ?
H1FA C1F H1FB 109.3 . . ?
C1G C1F H1FA 111.5 . . ?
C1G C1F H1FB 111.5 . . ?
C1F C1G H1GA 111.5 . . ?
C1F C1G H1GB 111.5 . . ?
H1GA C1G H1GB 109.3 . . ?
C1H C1G C1F 101.5 . . ?
C1H C1G H1GA 111.5 . . ?
C1H C1G H1GB 111.5 . . ?
O1 C1H C1G 106.4 . . ?
O1 C1H H1HA 110.4 . . ?
O1 C1H H1HB 110.4 . . ?
C1G C1H H1HA 110.4 . . ?
C1G C1H H1HB 110.4 . . ?
H1HA C1H H1HB 108.6 . . ?

_vrf_PLAT097_2b'                 
;
PROBLEM: Large Reported Max.  (Positive) Residual Density
RESPONSE: The terahydrofuran molecule is not located very 
precisely. This tetrahydrofuran molecule was isotropically refined 
on two positions with a set of constraints (EADP) applied on the 
isotropic temperature factors. The occupations factors of the two 
components of the disorder converged to approximately the same 
values than for the disordered isopropyl groups. In view of the 
inter and intra-molecular interactions between these groups, the 
occupation factors for both groups (tetrahydrofuran and 
isopropyl) were set to the same value (0.63:037).
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_8b
_database_code_depnum_ccdc_archive 'CCDC 1985142'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne Franche Comte
France
;
_audit_update_record             
;
2020-02-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_audit_creation_date             2018-12-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C56 H94 Br2 Cl2 Cu2 N6 P6 Ti2, 2.28(C H2 Cl2)'
_chemical_formula_sum            'C58.28 H98.56 Br2 Cl6.56 Cu2 N6 P6 Ti2'
_chemical_formula_weight         1684.42
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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                   11.6149(6)
_cell_length_b                   16.6838(8)
_cell_length_c                   20.0416(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.810(2)
_cell_angle_gamma                90
_cell_volume                     3883.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.97
_shelx_estimated_absorpt_T_max   0.681
_shelx_estimated_absorpt_T_min   0.511
_exptl_absorpt_coefficient_mu    2.155
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0779 before and 0.0496 after correction. The Ratio of minimum to maximum transmission is 0.8248.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1728
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of DCM and pentane  by slow evaporation'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.193
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51118
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.585
_diffrn_reflns_theta_min         2.932
_diffrn_ambient_temperature      100.0
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'κ-geometry diffractometer triump Mo'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       "φ and ω scans'"
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-90C'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6922
_reflns_number_total             8943
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.230
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         8943
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0428
_refine_ls_restrained_S_all      1.062
_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)+(0.0341P)²+14.0897P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1094
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C13(0.52) C13A(0.48) C14(0.52) H14(0.52) C14A(0.48) H14A(0.48)
 C15(0.52) H15(0.52) C15A(0.48) H15A(0.48) C16(0.52) H16(0.52) C16A(0.48)
 H16A(0.48) C17(0.52) H17(0.52) C17A(0.48) H17A(0.48) C18(0.52) H18(0.52)
 C18A(0.48) H18A(0.48) Cl2A(0.5) Cl3A(0.5) C29A(0.5) H29A(0.5) H29B(0.5)
 Cl2(0.5) Cl3(0.5) C29(0.5) H29C(0.5) H29D(0.5) Cl4(0.14) Cl5(0.14) C30(0.14)
 H30A(0.14) H30B(0.14)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22)
3.b Secondary CH2 refined with riding coordinates:
 C29A(H29A,H29B), C29(H29C,H29D), C30(H30A,H30B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C14(H14), C14A(H14A), C15A(H15A),
 C16(H16), C16A(H16A), C17(H17), C17A(H17A), C18(H18), C18A(H18A)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Br Br 0.35545(3) 0.51387(2) 0.53744(2) 0.02594(10) Uani 1 1 d . . . . .
Cu Cu 0.43960(4) 0.48486(2) 0.43254(2) 0.01803(10) Uani 1 1 d . . . . .
Ti Ti 0.32383(5) 0.46619(3) 0.17625(3) 0.01341(12) Uani 1 1 d . . . . .
C1 C 0.4718(3) 0.31827(19) 0.15940(16) 0.0159(6) Uani 1 1 d . . . . .
Cl1 Cl 0.41465(7) 0.59009(4) 0.15729(4) 0.01807(17) Uani 1 1 d . . . . .
N1 N 0.4229(2) 0.37255(15) 0.20668(13) 0.0145(5) Uani 1 1 d . . . . .
P1 P 0.45529(7) 0.37118(5) 0.28615(4) 0.01461(17) Uani 1 1 d . . . . .
C2 C 0.5396(3) 0.3496(2) 0.10904(17) 0.0204(7) Uani 1 1 d . . . . .
H2 H 0.555575 0.405420 0.108306 0.024 Uiso 1 1 calc R . . . .
N2 N 0.1784(2) 0.45820(16) 0.23157(13) 0.0164(6) Uani 1 1 d . . . . .
P2 P 0.37807(7) 0.47754(5) 0.32866(4) 0.01387(17) Uani 1 1 d . . . . .
C3 C 0.5843(3) 0.3006(3) 0.05996(18) 0.0283(8) Uani 1 1 d . . . . .
H3 H 0.629773 0.322941 0.025559 0.034 Uiso 1 1 calc R . . . .
N3 N 0.2783(2) 0.43620(17) 0.09986(14) 0.0167(6) Uani 1 1 d . . . . .
P3 P 0.19337(7) 0.47423(5) 0.31182(4) 0.01436(17) Uani 1 1 d . . . . .
C4 C 0.5624(4) 0.2188(2) 0.06127(19) 0.0329(10) Uani 1 1 d . . . . .
H4 H 0.593242 0.184753 0.027992 0.040 Uiso 1 1 calc R . . . .
C5 C 0.4961(4) 0.1876(2) 0.11073(19) 0.0343(10) Uani 1 1 d . . . . .
H5 H 0.481801 0.131551 0.111682 0.041 Uiso 1 1 calc R . . . .
C6 C 0.4492(4) 0.2364(2) 0.15982(18) 0.0255(8) Uani 1 1 d . . . . .
H6 H 0.402051 0.213894 0.193338 0.031 Uiso 1 1 calc R . . . .
C7 C 0.4269(3) 0.27401(19) 0.32525(16) 0.0194(7) Uani 1 1 d . . . . .
H7 H 0.474994 0.233826 0.301282 0.023 Uiso 1 1 calc R . . . .
C8 C 0.4673(3) 0.2724(2) 0.39853(17) 0.0242(8) Uani 1 1 d . . . . .
H8A H 0.427540 0.314505 0.423357 0.036 Uiso 1 1 calc GR . . . .
H8B H 0.550584 0.281719 0.400973 0.036 Uiso 1 1 calc GR . . . .
H8C H 0.449632 0.220058 0.418008 0.036 Uiso 1 1 calc GR . . . .
C9 C 0.3031(3) 0.2466(2) 0.31729(19) 0.0260(8) Uani 1 1 d . . . . .
H9A H 0.274089 0.261365 0.272828 0.039 Uiso 1 1 calc GR . . . .
H9B H 0.255938 0.272320 0.351307 0.039 Uiso 1 1 calc GR . . . .
H9C H 0.299287 0.188230 0.322596 0.039 Uiso 1 1 calc GR . . . .
C10 C 0.6093(3) 0.3907(2) 0.30145(17) 0.0211(7) Uani 1 1 d . . . . .
H10 H 0.621316 0.396165 0.350748 0.025 Uiso 1 1 calc R . . . .
C11 C 0.6842(3) 0.3204(2) 0.27765(18) 0.0241(8) Uani 1 1 d . . . . .
H11A H 0.672871 0.312906 0.229498 0.036 Uiso 1 1 calc GR . . . .
H11B H 0.661906 0.271349 0.301094 0.036 Uiso 1 1 calc GR . . . .
H11C H 0.765421 0.332138 0.287207 0.036 Uiso 1 1 calc GR . . . .
C12 C 0.6458(3) 0.4698(2) 0.26924(19) 0.0248(8) Uani 1 1 d . . . . .
H12A H 0.596998 0.513305 0.285472 0.037 Uiso 1 1 calc GR . . . .
H12B H 0.637460 0.465550 0.220643 0.037 Uiso 1 1 calc GR . . . .
H12C H 0.726396 0.481008 0.280991 0.037 Uiso 1 1 calc GR . . . .
C13 C 0.0666(8) 0.4416(6) 0.2040(5) 0.015(3) Uiso 0.52 1 d . . P A 1
C13A C 0.0756(9) 0.4263(6) 0.2002(5) 0.014(3) Uiso 0.48 1 d . . P A 2
C14 C -0.0112(7) 0.5018(6) 0.1903(4) 0.0178(17) Uiso 0.52 1 d . . P A 1
H14 H 0.005552 0.555693 0.202456 0.021 Uiso 0.52 1 calc R . P A 1
C14A C -0.0177(8) 0.4775(6) 0.1852(4) 0.022(2) Uiso 0.48 1 d . . P A 2
H14A H -0.013814 0.532434 0.197454 0.027 Uiso 0.48 1 calc R . P A 2
C15 C -0.1148(6) 0.4825(6) 0.1584(4) 0.0227(15) Uiso 0.52 1 d . . P A 1
H15 H -0.166(7) 0.529(5) 0.155(4) 0.027 Uiso 0.52 1 d R . P B 1
C15A C -0.1176(7) 0.4475(7) 0.1518(4) 0.0256(18) Uiso 0.48 1 d . . P A 2
H15A H -0.180462 0.481692 0.140769 0.031 Uiso 0.48 1 calc R . P A 2
C16 C -0.1382(6) 0.4051(6) 0.1385(4) 0.0216(14) Uiso 0.52 1 d . . P A 1
H16 H -0.208626 0.393644 0.115795 0.026 Uiso 0.52 1 calc R . P A 1
C16A C -0.1199(8) 0.3681(6) 0.1361(4) 0.0271(18) Uiso 0.48 1 d . . P A 2
H16A H -0.186340 0.346750 0.114426 0.033 Uiso 0.48 1 calc R . P A 2
C17 C -0.0617(7) 0.3444(5) 0.1510(4) 0.0229(16) Uiso 0.52 1 d . . P A 1
H17 H -0.078186 0.290952 0.137635 0.027 Uiso 0.52 1 calc R . P A 1
C17A C -0.0288(8) 0.3176(6) 0.1507(4) 0.0274(19) Uiso 0.48 1 d . . P A 2
H17A H -0.032554 0.262649 0.138406 0.033 Uiso 0.48 1 calc R . P A 2
C18 C 0.0417(8) 0.3635(6) 0.1842(4) 0.023(2) Uiso 0.52 1 d . . P A 1
H18 H 0.095941 0.322210 0.193341 0.028 Uiso 0.52 1 calc R . P A 1
C18A C 0.0676(8) 0.3471(6) 0.1833(4) 0.017(2) Uiso 0.48 1 d . . P A 2
H18A H 0.129327 0.311869 0.194211 0.021 Uiso 0.48 1 calc R . P A 2
C19 C 0.1015(3) 0.4051(2) 0.35907(18) 0.0207(7) Uani 1 1 d . . . . .
H19 H 0.102001 0.353114 0.334310 0.025 Uiso 1 1 calc R . . . .
C20 C 0.1461(3) 0.3868(2) 0.42965(18) 0.0246(8) Uani 1 1 d . . . . .
H20A H 0.135926 0.434008 0.458036 0.037 Uiso 1 1 calc GR . . . .
H20B H 0.228035 0.372964 0.428053 0.037 Uiso 1 1 calc GR . . . .
H20C H 0.102966 0.341605 0.448053 0.037 Uiso 1 1 calc GR . . . .
C21 C -0.0252(3) 0.4324(2) 0.3609(2) 0.0267(8) Uani 1 1 d . . . . .
H21A H -0.053077 0.442723 0.315333 0.040 Uiso 1 1 calc GR . . . .
H21B H -0.031057 0.481476 0.387434 0.040 Uiso 1 1 calc GR . . . .
H21C H -0.071945 0.390162 0.381073 0.040 Uiso 1 1 calc GR . . . .
C22 C 0.1477(3) 0.57692(19) 0.33290(17) 0.0196(7) Uani 1 1 d . . . . .
H22 H 0.064520 0.581053 0.319775 0.024 Uiso 1 1 calc R . . . .
C23 C 0.1554(4) 0.5972(2) 0.40722(19) 0.0305(9) Uani 1 1 d . . . . .
H23A H 0.235626 0.593204 0.422599 0.046 Uiso 1 1 calc GR . . . .
H23B H 0.107935 0.559569 0.432366 0.046 Uiso 1 1 calc GR . . . .
H23C H 0.127467 0.651970 0.414323 0.046 Uiso 1 1 calc GR . . . .
C24 C 0.2115(3) 0.6389(2) 0.29124(19) 0.0259(8) Uani 1 1 d . . . . .
H24A H 0.211135 0.621929 0.244408 0.039 Uiso 1 1 calc GR . . . .
H24B H 0.291139 0.643437 0.307564 0.039 Uiso 1 1 calc GR . . . .
H24C H 0.173110 0.690937 0.294994 0.039 Uiso 1 1 calc GR . . . .
C25 C 0.2482(3) 0.4146(2) 0.03191(16) 0.0192(7) Uani 1 1 d . . . . .
C26 C 0.1284(3) 0.4484(3) 0.01507(18) 0.0281(8) Uani 1 1 d . . . . .
H26A H 0.130792 0.507071 0.016961 0.042 Uiso 1 1 calc GR . . . .
H26B H 0.072797 0.428389 0.047412 0.042 Uiso 1 1 calc GR . . . .
H26C H 0.105084 0.431318 -0.029913 0.042 Uiso 1 1 calc GR . . . .
C27 C 0.3370(3) 0.4501(3) -0.01506(18) 0.0276(8) Uani 1 1 d . . . . .
H27A H 0.413143 0.427868 -0.004317 0.041 Uiso 1 1 calc GR . . . .
H27B H 0.338911 0.508471 -0.009771 0.041 Uiso 1 1 calc GR . . . .
H27C H 0.316007 0.436723 -0.061268 0.041 Uiso 1 1 calc GR . . . .
C28 C 0.2451(4) 0.3230(2) 0.02550(19) 0.0279(8) Uani 1 1 d . . . . .
H28A H 0.188520 0.301134 0.056427 0.042 Uiso 1 1 calc GR . . . .
H28B H 0.321357 0.301066 0.036286 0.042 Uiso 1 1 calc GR . . . .
H28C H 0.223339 0.308308 -0.020316 0.042 Uiso 1 1 calc GR . . . .
Cl2A Cl 0.9776(7) 0.2107(5) 0.3432(3) 0.0402(13) Uani 0.5 1 d . . P C 4
Cl3A Cl 0.8535(6) 0.2360(5) 0.4646(3) 0.100(3) Uani 0.5 1 d . . P C 4
C29A C 0.879(3) 0.1715(19) 0.3960(8) 0.041(4) Uani 0.5 1 d . . P C 4
H29A H 0.907085 0.119134 0.412761 0.049 Uiso 0.5 1 calc R . P C 4
H29B H 0.805853 0.162287 0.371294 0.049 Uiso 0.5 1 calc R . P C 4
Cl2 Cl 0.9891(9) 0.2009(6) 0.3620(4) 0.0458(15) Uani 0.5 1 d . . P D 3
Cl3 Cl 0.8150(4) 0.2613(3) 0.4524(3) 0.0459(9) Uani 0.5 1 d . . P D 3
C29 C 0.874(2) 0.1762(17) 0.4177(8) 0.037(4) Uani 0.5 1 d . . P D 3
H29C H 0.813552 0.146369 0.392938 0.045 Uiso 0.5 1 calc R . P D 3
H29D H 0.904113 0.141058 0.453795 0.045 Uiso 0.5 1 calc R . P D 3
Cl4 Cl 0.9125(9) 0.6517(6) 0.4207(4) 0.057(2) Uani 0.14 1 d . . P . .
Cl5 Cl 0.8492(8) 0.6346(5) 0.2835(4) 0.0446(19) Uani 0.14 1 d . . P . .
C30 C 0.815(3) 0.6415(18) 0.3612(14) 0.033(7) Uani 0.14 1 d . . P . .
H30A H 0.770287 0.592984 0.371975 0.040 Uiso 0.14 1 calc R . P . .
H30B H 0.762269 0.687615 0.364914 0.040 Uiso 0.14 1 calc R . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Br Cu 2.3808(6) . ?
Br Cu 2.4472(6) 3_666 ?
Cu P2 2.1948(9) . ?
Ti Cl1 2.3541(9) . ?
Ti N1 2.029(3) . ?
Ti N2 2.038(3) . ?
Ti N3 1.688(3) . ?
C1 N1 1.434(4) . ?
C1 C2 1.391(5) . ?
C1 C6 1.391(5) . ?
N1 P1 1.632(3) . ?
P1 P2 2.1682(11) . ?
P1 C7 1.833(3) . ?
P1 C10 1.839(4) . ?
C2 C3 1.385(5) . ?
N2 P3 1.637(3) . ?
N2 C13 1.430(9) . ?
N2 C13A 1.443(10) . ?
P2 P3 2.1676(12) . ?
C3 C4 1.389(6) . ?
N3 C25 1.447(4) . ?
P3 C19 1.842(3) . ?
P3 C22 1.844(3) . ?
C4 C5 1.367(6) . ?
C5 C6 1.394(5) . ?
C7 C8 1.536(5) . ?
C7 C9 1.515(5) . ?
C10 C11 1.541(5) . ?
C10 C12 1.530(5) . ?
C13 C14 1.376(13) . ?
C13 C18 1.392(12) . ?
C13A C14A 1.409(13) . ?
C13A C18A 1.366(14) . ?
C14 C15 1.393(11) . ?
C14A C15A 1.422(13) . ?
C15 C16 1.378(11) . ?
C15A C16A 1.362(13) . ?
C16 C17 1.368(12) . ?
C16A C17A 1.381(13) . ?
C17 C18 1.401(12) . ?
C17A C18A 1.379(12) . ?
C19 C20 1.531(5) . ?
C19 C21 1.540(5) . ?
C22 C23 1.529(5) . ?
C22 C24 1.527(5) . ?
C25 C26 1.535(5) . ?
C25 C27 1.526(5) . ?
C25 C28 1.534(5) . ?
Cl2A C29A 1.70(2) . ?
Cl3A C29A 1.77(2) . ?
Cl2 C29 1.80(2) . ?
Cl3 C29 1.73(3) . ?
Cl4 C30 1.64(3) . ?
Cl5 C30 1.62(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
Cu Br Cu 78.977(18) . 3_666 ?
Br Cu Br 101.021(18) . 3_666 ?
P2 Cu Br 122.43(3) . 3_666 ?
P2 Cu Br 135.78(3) . . ?
N1 Ti Cl1 118.11(8) . . ?
N1 Ti N2 104.90(11) . . ?
N2 Ti Cl1 121.47(8) . . ?
N3 Ti Cl1 104.43(10) . . ?
N3 Ti N1 102.32(12) . . ?
N3 Ti N2 102.85(12) . . ?
C2 C1 N1 118.4(3) . . ?
C6 C1 N1 122.7(3) . . ?
C6 C1 C2 118.8(3) . . ?
C1 N1 Ti 121.1(2) . . ?
C1 N1 P1 123.2(2) . . ?
P1 N1 Ti 115.23(14) . . ?
N1 P1 P2 106.33(10) . . ?
N1 P1 C7 112.92(15) . . ?
N1 P1 C10 111.75(16) . . ?
C7 P1 P2 118.55(12) . . ?
C7 P1 C10 105.44(16) . . ?
C10 P1 P2 101.29(11) . . ?
C3 C2 C1 121.1(3) . . ?
P3 N2 Ti 116.49(15) . . ?
C13 N2 Ti 123.9(4) . . ?
C13 N2 P3 119.6(4) . . ?
C13A N2 Ti 118.3(4) . . ?
C13A N2 P3 124.4(4) . . ?
P1 P2 Cu 106.70(4) . . ?
P3 P2 Cu 117.22(5) . . ?
P3 P2 P1 109.39(5) . . ?
C2 C3 C4 119.7(4) . . ?
C25 N3 Ti 174.7(3) . . ?
N2 P3 P2 104.40(11) . . ?
N2 P3 C19 110.38(15) . . ?
N2 P3 C22 110.48(15) . . ?
C19 P3 P2 121.02(12) . . ?
C19 P3 C22 107.02(17) . . ?
C22 P3 P2 103.18(12) . . ?
C5 C4 C3 119.6(4) . . ?
C4 C5 C6 121.3(4) . . ?
C1 C6 C5 119.6(4) . . ?
C8 C7 P1 111.7(2) . . ?
C9 C7 P1 113.5(2) . . ?
C9 C7 C8 111.9(3) . . ?
C11 C10 P1 111.4(2) . . ?
C12 C10 P1 110.9(2) . . ?
C12 C10 C11 111.4(3) . . ?
C14 C13 N2 121.7(8) . . ?
C14 C13 C18 119.6(8) . . ?
C18 C13 N2 118.4(8) . . ?
C14A C13A N2 119.9(8) . . ?
C18A C13A N2 121.2(8) . . ?
C18A C13A C14A 119.0(9) . . ?
C13 C14 C15 118.9(9) . . ?
C13A C14A C15A 120.5(9) . . ?
C16 C15 C14 121.0(8) . . ?
C16A C15A C14A 117.6(8) . . ?
C17 C16 C15 121.1(7) . . ?
C15A C16A C17A 122.2(9) . . ?
C16 C17 C18 118.0(8) . . ?
C18A C17A C16A 119.8(9) . . ?
C13 C18 C17 121.5(9) . . ?
C13A C18A C17A 120.9(10) . . ?
C20 C19 P3 114.1(2) . . ?
C20 C19 C21 110.4(3) . . ?
C21 C19 P3 112.9(2) . . ?
C23 C22 P3 114.6(2) . . ?
C24 C22 P3 111.1(2) . . ?
C24 C22 C23 111.1(3) . . ?
N3 C25 C26 108.8(3) . . ?
N3 C25 C27 109.1(3) . . ?
N3 C25 C28 109.4(3) . . ?
C27 C25 C26 109.9(3) . . ?
C27 C25 C28 110.5(3) . . ?
C28 C25 C26 109.1(3) . . ?
Cl2A C29A Cl3A 111.8(17) . . ?
Cl3 C29 Cl2 111.3(15) . . ?
Cl5 C30 Cl4 122(2) . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'


_vrf_PLAT201_8b                  
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s)
RESPONSE: One phenyl group was found disordered with occupations factors 
equal to 0.52:0.48 and these disordered groups were refined isotropically. 
;
_vrf_PLAT910_8b                  
;
PROBLEM: Missing of FCF Reflections below Theta (Min)
RESPONSE: Most of the missing reflections were excluded by the OMIT 
command in order to avoid problems related to saturation to low 
theta reflections and beamstop.
;
####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 1985143'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne Franche Comte
France
;
_audit_update_record             
;
2020-02-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_audit_creation_date             2020-01-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H38 Cl2 N2 O P3 Ti'
_chemical_formula_sum            'C40 H38 Cl2 N2 O P3 Ti'
_chemical_formula_weight         774.43
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.1219(16)
_cell_length_b                   16.662(3)
_cell_length_c                   22.432(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.270(3)
_cell_angle_gamma                90
_cell_volume                     3733.8(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    115
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.43
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.8014
_exptl_absorpt_correction_T_min  0.7409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0459 before and 0.0427 after correction. The Ratio of minimum to maximum transmission is 0.9245. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            47407
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         2.377
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_orient_matrix_type       'Nonius Collect from scalepack cell'
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7229
_reflns_number_total             8521
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_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     442
_refine_ls_number_reflns         8521
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0316
_refine_ls_restrained_S_all      1.036
_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)+(0.0309P)²+3.2769P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0784
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_special_details      
;
The structure was solved using Patterson Methods, followed by a Tangent Expansion (ShelXS). RE = 0.2, Nqual =  -1, Ralpha = 0.086
;
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
C1 C 0.08443(17) 0.92792(10) 0.84443(7) 0.0152(3) Uani 1 1 d . . . . .
C2 C 0.20285(17) 0.97195(10) 0.86088(7) 0.0166(3) Uani 1 1 d . . . . .
H2 H 0.277485 0.961443 0.841248 0.020 Uiso 1 1 calc R . . . .
C3 C 0.21288(18) 1.03058(10) 0.90534(8) 0.0186(3) Uani 1 1 d . . . . .
H3 H 0.294363 1.059264 0.916011 0.022 Uiso 1 1 calc R . . . .
C4 C 0.10517(19) 1.04766(11) 0.93430(8) 0.0220(4) Uani 1 1 d . . . . .
H4 H 0.112062 1.087868 0.964673 0.026 Uiso 1 1 calc R . . . .
C5 C -0.01314(19) 1.00495(12) 0.91814(8) 0.0238(4) Uani 1 1 d . . . . .
H5 H -0.087934 1.016665 0.937371 0.029 Uiso 1 1 calc R . . . .
C6 C -0.02365(18) 0.94535(11) 0.87428(8) 0.0207(4) Uani 1 1 d . . . . .
H6 H -0.104841 0.916151 0.864439 0.025 Uiso 1 1 calc R . . . .
C7 C 0.33361(16) 0.80064(10) 0.83533(7) 0.0135(3) Uani 1 1 d . . . . .
C8 C 0.46822(17) 0.81794(11) 0.83605(8) 0.0191(3) Uani 1 1 d . . . . .
H8 H 0.494185 0.852544 0.806325 0.023 Uiso 1 1 calc R . . . .
C9 C 0.56481(18) 0.78471(12) 0.88015(8) 0.0240(4) Uani 1 1 d . . . . .
H9 H 0.656756 0.796582 0.880567 0.029 Uiso 1 1 calc R . . . .
C10 C 0.52712(19) 0.73432(12) 0.92347(8) 0.0241(4) Uani 1 1 d . . . . .
H10 H 0.593373 0.710938 0.953211 0.029 Uiso 1 1 calc R . . . .
C11 C 0.3929(2) 0.71786(11) 0.92358(8) 0.0234(4) Uani 1 1 d . . . . .
H11 H 0.367558 0.683751 0.953735 0.028 Uiso 1 1 calc R . . . .
C12 C 0.29549(17) 0.75088(11) 0.87995(8) 0.0186(3) Uani 1 1 d . . . . .
H12 H 0.203545 0.739843 0.880305 0.022 Uiso 1 1 calc R . . . .
C13 C 0.26672(16) 0.90071(10) 0.72532(7) 0.0136(3) Uani 1 1 d . . . . .
C14 C 0.20069(19) 0.97427(10) 0.71396(8) 0.0193(3) Uani 1 1 d . . . . .
H14 H 0.121518 0.984742 0.730344 0.023 Uiso 1 1 calc R . . . .
C15 C 0.2504(2) 1.03191(11) 0.67889(8) 0.0267(4) Uani 1 1 d . . . . .
H15 H 0.204924 1.081586 0.670939 0.032 Uiso 1 1 calc R . . . .
C16 C 0.3667(2) 1.01697(12) 0.65544(8) 0.0293(5) Uani 1 1 d . . . . .
H16 H 0.402548 1.057247 0.632686 0.035 Uiso 1 1 calc R . . . .
C17 C 0.43064(19) 0.94349(13) 0.66506(8) 0.0263(4) Uani 1 1 d . . . . .
H17 H 0.509108 0.933140 0.648114 0.032 Uiso 1 1 calc R . . . .
C18 C 0.38049(17) 0.88487(11) 0.69942(7) 0.0184(3) Uani 1 1 d . . . . .
H18 H 0.423517 0.834159 0.705257 0.022 Uiso 1 1 calc R . . . .
C19 C -0.17472(16) 0.84938(10) 0.62527(7) 0.0147(3) Uani 1 1 d . . . . .
C20 C -0.18949(18) 0.93253(10) 0.63062(8) 0.0190(3) Uani 1 1 d . . . . .
H20 H -0.142978 0.959731 0.664925 0.023 Uiso 1 1 calc R . . . .
C21 C -0.27137(18) 0.97552(11) 0.58630(9) 0.0231(4) Uani 1 1 d . . . . .
H21 H -0.280523 1.031895 0.590464 0.028 Uiso 1 1 calc R . . . .
C22 C -0.34001(18) 0.93673(12) 0.53592(8) 0.0239(4) Uani 1 1 d . . . . .
H22 H -0.394208 0.966604 0.505174 0.029 Uiso 1 1 calc R . . . .
C23 C -0.32916(17) 0.85405(12) 0.53063(8) 0.0218(4) Uani 1 1 d . . . . .
H23 H -0.377346 0.827150 0.496567 0.026 Uiso 1 1 calc R . . . .
C24 C -0.24753(17) 0.81043(11) 0.57530(8) 0.0176(3) Uani 1 1 d . . . . .
H24 H -0.241390 0.753794 0.571710 0.021 Uiso 1 1 calc R . . . .
C25 C -0.02153(16) 0.65448(10) 0.61763(7) 0.0145(3) Uani 1 1 d . . . . .
C26 C -0.04307(18) 0.58774(10) 0.65235(8) 0.0205(4) Uani 1 1 d . . . . .
H26 H -0.023235 0.590565 0.695156 0.025 Uiso 1 1 calc R . . . .
C27 C -0.0935(2) 0.51699(11) 0.62450(9) 0.0269(4) Uani 1 1 d . . . . .
H27 H -0.108391 0.471746 0.648325 0.032 Uiso 1 1 calc R . . . .
C28 C -0.12207(19) 0.51249(11) 0.56226(9) 0.0265(4) Uani 1 1 d . . . . .
H28 H -0.156766 0.464164 0.543419 0.032 Uiso 1 1 calc R . . . .
C29 C -0.10026(19) 0.57826(11) 0.52713(9) 0.0244(4) Uani 1 1 d . . . . .
H29 H -0.119924 0.574951 0.484336 0.029 Uiso 1 1 calc R . . . .
C30 C -0.04965(17) 0.64891(10) 0.55468(8) 0.0181(3) Uani 1 1 d . . . . .
H30 H -0.034022 0.693744 0.530591 0.022 Uiso 1 1 calc R . . . .
C31 C 0.13370(16) 0.79385(10) 0.60215(7) 0.0140(3) Uani 1 1 d . . . . .
C32 C 0.11064(17) 0.87055(10) 0.57805(7) 0.0160(3) Uani 1 1 d . . . . .
H32 H 0.037691 0.901539 0.587174 0.019 Uiso 1 1 calc R . . . .
C33 C 0.19530(18) 0.90167(11) 0.54038(8) 0.0187(3) Uani 1 1 d . . . . .
H33 H 0.179258 0.953758 0.523552 0.022 Uiso 1 1 calc R . . . .
C34 C 0.30251(18) 0.85700(11) 0.52744(8) 0.0202(4) Uani 1 1 d . . . . .
H34 H 0.359588 0.878451 0.501693 0.024 Uiso 1 1 calc R . . . .
C35 C 0.32677(18) 0.78078(11) 0.55206(8) 0.0215(4) Uani 1 1 d . . . . .
H35 H 0.400626 0.750275 0.543336 0.026 Uiso 1 1 calc R . . . .
C36 C 0.24290(17) 0.74941(10) 0.58937(8) 0.0186(3) Uani 1 1 d . . . . .
H36 H 0.259748 0.697445 0.606335 0.022 Uiso 1 1 calc R . . . .
C37 C -0.34520(18) 0.69544(11) 0.68890(8) 0.0223(4) Uani 1 1 d . . . . .
H37A H -0.333495 0.666417 0.651592 0.027 Uiso 1 1 calc R . . . .
H37B H -0.361933 0.752838 0.679050 0.027 Uiso 1 1 calc R . . . .
C38 C -0.45933(19) 0.65991(12) 0.71618(10) 0.0280(4) Uani 1 1 d . . . . .
H38A H -0.525607 0.633861 0.684860 0.034 Uiso 1 1 calc R . . . .
H38B H -0.504975 0.701627 0.736824 0.034 Uiso 1 1 calc R . . . .
C39 C -0.3904(2) 0.59797(15) 0.76148(12) 0.0421(6) Uani 1 1 d . . . . .
H39A H -0.413501 0.607652 0.802120 0.051 Uiso 1 1 calc R . . . .
H39B H -0.418592 0.542912 0.748582 0.051 Uiso 1 1 calc R . . . .
C40 C -0.2459(2) 0.60826(14) 0.76234(13) 0.0458(7) Uani 1 1 d . . . . .
H40A H -0.197541 0.606752 0.804352 0.055 Uiso 1 1 calc R . . . .
H40B H -0.210900 0.564859 0.739085 0.055 Uiso 1 1 calc R . . . .
Cl1 Cl -0.07353(4) 0.72833(3) 0.86244(2) 0.02464(10) Uani 1 1 d . . . . .
Cl2 Cl -0.26867(4) 0.87548(3) 0.76145(2) 0.01904(9) Uani 1 1 d . . . . .
N1 N 0.07042(13) 0.86633(8) 0.79967(6) 0.0140(3) Uani 1 1 d . . . . .
N2 N -0.08422(13) 0.80789(8) 0.67062(6) 0.0134(3) Uani 1 1 d . . . . .
O O -0.22812(13) 0.68605(8) 0.73493(6) 0.0254(3) Uani 1 1 d . . . . .
P2 P 0.14268(4) 0.71332(2) 0.73862(2) 0.01319(9) Uani 1 1 d . . . . .
P1 P 0.20128(4) 0.83031(2) 0.77458(2) 0.01172(9) Uani 1 1 d . . . . .
P3 P 0.03307(4) 0.74946(2) 0.65357(2) 0.01168(9) Uani 1 1 d . . . . .
Ti Ti -0.08560(3) 0.78735(2) 0.76564(2) 0.01342(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
C1 C2 1.403(2) . ?
C1 C6 1.402(2) . ?
C1 N1 1.427(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.388(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.386(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.390(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.390(2) . ?
C7 C12 1.401(2) . ?
C7 P1 1.8186(16) . ?
C8 H8 0.9500 . ?
C8 C9 1.389(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.384(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.386(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.386(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.400(2) . ?
C13 C18 1.396(2) . ?
C13 P1 1.8087(16) . ?
C14 H14 0.9500 . ?
C14 C15 1.387(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.386(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.386(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.390(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.401(2) . ?
C19 C24 1.398(2) . ?
C19 N2 1.432(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.387(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.387(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.388(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.396(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.395(2) . ?
C25 C30 1.398(2) . ?
C25 P3 1.8211(17) . ?
C26 H26 0.9500 . ?
C26 C27 1.392(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.381(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.388(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.388(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.393(2) . ?
C31 C36 1.398(2) . ?
C31 P3 1.8148(17) . ?
C32 H32 0.9500 . ?
C32 C33 1.397(2) . ?
C33 H33 0.9500 . ?
C33 C34 1.385(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.391(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.387(2) . ?
C36 H36 0.9500 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.512(3) . ?
C37 O 1.449(2) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.535(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.470(3) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 O 1.458(2) . ?
Cl1 Ti 2.3688(6) . ?
Cl2 Ti 2.3542(6) . ?
N1 P1 1.6345(14) . ?
N1 Ti 2.1024(14) . ?
N2 P3 1.6278(14) . ?
N2 Ti 2.1611(14) . ?
O Ti 2.2548(13) . ?
P2 P1 2.1558(7) . ?
P2 P3 2.1333(6) . ?
P2 Ti 2.7712(6) . ?
P1 Ti 2.9660(7) . ?
P3 Ti 3.0224(6) . ?

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
C2 C1 N1 123.02(15) . . ?
C6 C1 C2 117.73(15) . . ?
C6 C1 N1 119.24(15) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 C1 121.16(16) . . ?
C3 C2 H2 119.4 . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.63(17) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 118.84(16) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 120.99(17) . . ?
C6 C5 H5 119.5 . . ?
C1 C6 H6 119.7 . . ?
C5 C6 C1 120.63(17) . . ?
C5 C6 H6 119.7 . . ?
C8 C7 C12 119.78(15) . . ?
C8 C7 P1 123.68(13) . . ?
C12 C7 P1 116.22(12) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 C7 120.11(16) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 120.00(17) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 119.9 . . ?
C9 C10 C11 120.17(17) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.40(17) . . ?
C12 C11 H11 119.8 . . ?
C7 C12 H12 120.2 . . ?
C11 C12 C7 119.52(16) . . ?
C11 C12 H12 120.2 . . ?
C14 C13 P1 117.90(13) . . ?
C18 C13 C14 119.43(15) . . ?
C18 C13 P1 122.65(13) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 C13 120.23(17) . . ?
C15 C14 H14 119.9 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 119.92(18) . . ?
C16 C15 H15 120.0 . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.22(17) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.27(18) . . ?
C18 C17 H17 119.9 . . ?
C13 C18 H18 120.1 . . ?
C17 C18 C13 119.83(17) . . ?
C17 C18 H18 120.1 . . ?
C20 C19 N2 118.77(15) . . ?
C24 C19 C20 118.55(15) . . ?
C24 C19 N2 122.67(15) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.61(17) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 119.8 . . ?
C20 C21 C22 120.43(17) . . ?
C22 C21 H21 119.8 . . ?
C21 C22 H22 120.1 . . ?
C21 C22 C23 119.72(16) . . ?
C23 C22 H22 120.1 . . ?
C22 C23 H23 120.0 . . ?
C22 C23 C24 120.07(17) . . ?
C24 C23 H23 120.0 . . ?
C19 C24 H24 119.7 . . ?
C23 C24 C19 120.57(16) . . ?
C23 C24 H24 119.7 . . ?
C26 C25 C30 119.11(16) . . ?
C26 C25 P3 120.61(13) . . ?
C30 C25 P3 120.18(13) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 C25 120.23(17) . . ?
C27 C26 H26 119.9 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.09(18) . . ?
C28 C27 H27 120.0 . . ?
C27 C28 H28 119.9 . . ?
C27 C28 C29 120.30(17) . . ?
C29 C28 H28 119.9 . . ?
C28 C29 H29 120.1 . . ?
C28 C29 C30 119.84(17) . . ?
C30 C29 H29 120.1 . . ?
C25 C30 H30 119.8 . . ?
C29 C30 C25 120.42(17) . . ?
C29 C30 H30 119.8 . . ?
C32 C31 C36 119.67(15) . . ?
C32 C31 P3 123.00(13) . . ?
C36 C31 P3 117.24(12) . . ?
C31 C32 H32 120.2 . . ?
C31 C32 C33 119.66(16) . . ?
C33 C32 H32 120.2 . . ?
C32 C33 H33 119.8 . . ?
C34 C33 C32 120.35(16) . . ?
C34 C33 H33 119.8 . . ?
C33 C34 H34 119.9 . . ?
C33 C34 C35 120.11(16) . . ?
C35 C34 H34 119.9 . . ?
C34 C35 H35 120.1 . . ?
C36 C35 C34 119.85(17) . . ?
C36 C35 H35 120.1 . . ?
C31 C36 H36 119.8 . . ?
C35 C36 C31 120.34(16) . . ?
C35 C36 H36 119.8 . . ?
H37A C37 H37B 108.8 . . ?
C38 C37 H37A 110.7 . . ?
C38 C37 H37B 110.7 . . ?
O C37 H37A 110.7 . . ?
O C37 H37B 110.7 . . ?
O C37 C38 105.05(14) . . ?
C37 C38 H38A 111.0 . . ?
C37 C38 H38B 111.0 . . ?
C37 C38 C39 103.65(16) . . ?
H38A C38 H38B 109.0 . . ?
C39 C38 H38A 111.0 . . ?
C39 C38 H38B 111.0 . . ?
C38 C39 H39A 110.5 . . ?
C38 C39 H39B 110.5 . . ?
H39A C39 H39B 108.7 . . ?
C40 C39 C38 105.98(17) . . ?
C40 C39 H39A 110.5 . . ?
C40 C39 H39B 110.5 . . ?
C39 C40 H40A 110.4 . . ?
C39 C40 H40B 110.4 . . ?
H40A C40 H40B 108.6 . . ?
O C40 C39 106.77(18) . . ?
O C40 H40A 110.4 . . ?
O C40 H40B 110.4 . . ?
C1 N1 P1 120.82(11) . . ?
C1 N1 Ti 133.58(11) . . ?
P1 N1 Ti 104.37(7) . . ?
C19 N2 P3 121.93(11) . . ?
C19 N2 Ti 132.21(11) . . ?
P3 N2 Ti 104.95(7) . . ?
C37 O C40 104.70(14) . . ?
C37 O Ti 123.11(10) . . ?
C40 O Ti 130.77(12) . . ?
P1 P2 Ti 72.816(19) . . ?
P3 P2 P1 98.72(2) . . ?
P3 P2 Ti 74.82(2) . . ?
C7 P1 P2 99.19(6) . . ?
C7 P1 Ti 125.45(6) . . ?
C13 P1 C7 109.63(8) . . ?
C13 P1 P2 117.62(6) . . ?
C13 P1 Ti 124.48(5) . . ?
N1 P1 C7 112.43(7) . . ?
N1 P1 C13 111.66(8) . . ?
N1 P1 P2 105.75(5) . . ?
N1 P1 Ti 43.37(5) . . ?
P2 P1 Ti 63.203(16) . . ?
C25 P3 P2 103.16(6) . . ?
C25 P3 Ti 114.64(6) . . ?
C31 P3 C25 103.54(8) . . ?
C31 P3 P2 114.78(6) . . ?
C31 P3 Ti 141.49(5) . . ?
N2 P3 C25 116.29(7) . . ?
N2 P3 C31 114.26(7) . . ?
N2 P3 P2 104.63(5) . . ?
N2 P3 Ti 43.70(5) . . ?
P2 P3 Ti 62.239(19) . . ?
Cl1 Ti P2 95.395(18) . . ?
Cl1 Ti P1 97.635(17) . . ?
Cl1 Ti P3 134.99(2) . . ?
Cl2 Ti Cl1 102.689(19) . . ?
Cl2 Ti P2 161.358(18) . . ?
Cl2 Ti P1 127.44(2) . . ?
Cl2 Ti P3 120.848(17) . . ?
N1 Ti Cl1 90.13(4) . . ?
N1 Ti Cl2 99.47(4) . . ?
N1 Ti N2 97.77(5) . . ?
N1 Ti O 170.28(5) . . ?
N1 Ti P2 75.76(4) . . ?
N1 Ti P1 32.27(4) . . ?
N1 Ti P3 93.26(4) . . ?
N2 Ti Cl1 164.21(4) . . ?
N2 Ti Cl2 89.54(4) . . ?
N2 Ti O 85.56(5) . . ?
N2 Ti P2 73.53(4) . . ?
N2 Ti P1 82.33(4) . . ?
N2 Ti P3 31.36(4) . . ?
O Ti Cl1 84.57(4) . . ?
O Ti Cl2 89.66(4) . . ?
O Ti P2 96.60(4) . . ?
O Ti P1 140.57(4) . . ?
O Ti P3 84.83(4) . . ?
P2 Ti P1 43.981(15) . . ?
P2 Ti P3 42.939(12) . . ?
P1 Ti P3 65.835(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -0.6(3) . . . . ?
C1 N1 P1 C7 50.49(15) . . . . ?
C1 N1 P1 C13 -73.22(14) . . . . ?
C1 N1 P1 P2 157.71(11) . . . . ?
C1 N1 P1 Ti 168.96(16) . . . . ?
C2 C1 C6 C5 0.7(3) . . . . ?
C2 C1 N1 P1 12.8(2) . . . . ?
C2 C1 N1 Ti 178.00(12) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C3 C4 C5 C6 0.8(3) . . . . ?
C4 C5 C6 C1 -1.2(3) . . . . ?
C6 C1 C2 C3 0.2(2) . . . . ?
C6 C1 N1 P1 -166.37(13) . . . . ?
C6 C1 N1 Ti -1.2(2) . . . . ?
C7 C8 C9 C10 0.0(3) . . . . ?
C8 C7 C12 C11 -1.5(3) . . . . ?
C8 C7 P1 C13 -11.38(17) . . . . ?
C8 C7 P1 N1 -136.21(14) . . . . ?
C8 C7 P1 P2 112.42(14) . . . . ?
C8 C7 P1 Ti 175.97(12) . . . . ?
C8 C9 C10 C11 -1.0(3) . . . . ?
C9 C10 C11 C12 0.8(3) . . . . ?
C10 C11 C12 C7 0.5(3) . . . . ?
C12 C7 C8 C9 1.3(3) . . . . ?
C12 C7 P1 C13 175.19(13) . . . . ?
C12 C7 P1 N1 50.35(15) . . . . ?
C12 C7 P1 P2 -61.02(13) . . . . ?
C12 C7 P1 Ti 2.53(16) . . . . ?
C13 C14 C15 C16 -0.6(3) . . . . ?
C14 C13 C18 C17 3.0(2) . . . . ?
C14 C13 P1 C7 -126.03(13) . . . . ?
C14 C13 P1 N1 -0.75(15) . . . . ?
C14 C13 P1 P2 121.76(12) . . . . ?
C14 C13 P1 Ti 46.71(15) . . . . ?
C14 C15 C16 C17 2.4(3) . . . . ?
C15 C16 C17 C18 -1.4(3) . . . . ?
C16 C17 C18 C13 -1.3(3) . . . . ?
C18 C13 C14 C15 -2.1(3) . . . . ?
C18 C13 P1 C7 52.92(16) . . . . ?
C18 C13 P1 N1 178.20(13) . . . . ?
C18 C13 P1 P2 -59.29(15) . . . . ?
C18 C13 P1 Ti -134.34(12) . . . . ?
C19 C20 C21 C22 0.0(3) . . . . ?
C19 N2 P3 C25 -71.36(14) . . . . ?
C19 N2 P3 C31 49.24(15) . . . . ?
C19 N2 P3 P2 175.59(11) . . . . ?
C19 N2 P3 Ti -170.34(16) . . . . ?
C20 C19 C24 C23 2.4(2) . . . . ?
C20 C19 N2 P3 -127.13(15) . . . . ?
C20 C19 N2 Ti 65.5(2) . . . . ?
C20 C21 C22 C23 1.6(3) . . . . ?
C21 C22 C23 C24 -1.2(3) . . . . ?
C22 C23 C24 C19 -0.8(3) . . . . ?
C24 C19 C20 C21 -2.0(3) . . . . ?
C24 C19 N2 P3 51.9(2) . . . . ?
C24 C19 N2 Ti -115.50(16) . . . . ?
C25 C26 C27 C28 0.2(3) . . . . ?
C26 C25 C30 C29 1.0(3) . . . . ?
C26 C25 P3 C31 148.69(14) . . . . ?
C26 C25 P3 N2 -85.13(15) . . . . ?
C26 C25 P3 P2 28.75(15) . . . . ?
C26 C25 P3 Ti -36.48(15) . . . . ?
C26 C27 C28 C29 0.2(3) . . . . ?
C27 C28 C29 C30 0.0(3) . . . . ?
C28 C29 C30 C25 -0.5(3) . . . . ?
C30 C25 C26 C27 -0.8(3) . . . . ?
C30 C25 P3 C31 -34.94(15) . . . . ?
C30 C25 P3 N2 91.25(15) . . . . ?
C30 C25 P3 P2 -154.87(13) . . . . ?
C30 C25 P3 Ti 139.90(12) . . . . ?
C31 C32 C33 C34 -0.6(3) . . . . ?
C32 C31 C36 C35 -1.1(3) . . . . ?
C32 C31 P3 C25 125.90(14) . . . . ?
C32 C31 P3 N2 -1.57(17) . . . . ?
C32 C31 P3 P2 -122.44(13) . . . . ?
C32 C31 P3 Ti -46.55(18) . . . . ?
C32 C33 C34 C35 -0.2(3) . . . . ?
C33 C34 C35 C36 0.3(3) . . . . ?
C34 C35 C36 C31 0.3(3) . . . . ?
C36 C31 C32 C33 1.3(2) . . . . ?
C36 C31 P3 C25 -57.48(14) . . . . ?
C36 C31 P3 N2 175.05(12) . . . . ?
C36 C31 P3 P2 54.18(14) . . . . ?
C36 C31 P3 Ti 130.07(11) . . . . ?
C37 C38 C39 C40 6.2(3) . . . . ?
C38 C37 O C40 37.7(2) . . . . ?
C38 C37 O Ti -130.03(13) . . . . ?
C38 C39 C40 O 16.5(3) . . . . ?
C39 C40 O C37 -34.0(3) . . . . ?
C39 C40 O Ti 132.43(18) . . . . ?
N1 C1 C2 C3 -179.01(15) . . . . ?
N1 C1 C6 C5 179.93(16) . . . . ?
N2 C19 C20 C21 177.04(15) . . . . ?
N2 C19 C24 C23 -176.60(15) . . . . ?
O C37 C38 C39 -26.8(2) . . . . ?
P1 C7 C8 C9 -171.93(14) . . . . ?
P1 C7 C12 C11 172.19(14) . . . . ?
P1 C13 C14 C15 176.90(13) . . . . ?
P1 C13 C18 C17 -175.91(13) . . . . ?
P3 C25 C26 C27 175.59(14) . . . . ?
P3 C25 C30 C29 -175.46(14) . . . . ?
P3 C31 C32 C33 177.80(13) . . . . ?
P3 C31 C36 C35 -177.84(14) . . . . ?
Ti N1 P1 C7 -118.47(7) . . . . ?
Ti N1 P1 C13 117.82(7) . . . . ?
Ti N1 P1 P2 -11.25(7) . . . . ?
Ti N2 P3 C25 98.97(8) . . . . ?
Ti N2 P3 C31 -140.42(7) . . . . ?
Ti N2 P3 P2 -14.07(7) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_6ap
_database_code_depnum_ccdc_archive 'CCDC 1985138'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne Franche Comte
France
;
_audit_update_record             
;
2020-02-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_audit_creation_date             2020-01-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45 H44 Cl N4 P3 Ti'
_chemical_formula_sum            'C45 H44 Cl N4 P3 Ti'
_chemical_formula_weight         817.10
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.209(3)
_cell_length_b                   12.264(3)
_cell_length_c                   15.876(4)
_cell_angle_alpha                97.041(6)
_cell_angle_beta                 99.249(6)
_cell_angle_gamma                98.343(6)
_cell_volume                     2295.2(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2709
_cell_measurement_temperature    115
_cell_measurement_theta_max      24.81
_cell_measurement_theta_min      2.342
_shelx_estimated_absorpt_T_max   0.990
_shelx_estimated_absorpt_T_min   0.910
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_T_max  0.6461
_exptl_absorpt_correction_T_min  0.4785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0988 before and 0.0732 after correction. The Ratio of minimum to maximum transmission is 0.7164. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1707
_diffrn_reflns_av_unetI/netI     0.2498
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25525
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.055
_diffrn_reflns_theta_max         25.055
_diffrn_reflns_theta_min         2.608
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3504
_reflns_number_total             8107
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         8107
_refine_ls_number_restraints     459
_refine_ls_R_factor_all          0.1959
_refine_ls_R_factor_gt           0.0708
_refine_ls_restrained_S_all      0.897
_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)+(0.0882P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.2049
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C41(H41), C42(H42),
  C43(H43), C44(H44), C45(H45)
3.b Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Ti Ti 0.16105(9) 0.40458(10) 0.72185(8) 0.0250(3) Uani 1 1 d . U . . .
Cl Cl -0.00228(13) 0.30216(16) 0.62092(12) 0.0415(5) Uani 1 1 d . U . . .
P1 P 0.36320(14) 0.56460(14) 0.68241(11) 0.0212(4) Uani 1 1 d . U . . .
P2 P 0.28590(14) 0.44386(14) 0.57171(11) 0.0239(4) Uani 1 1 d . U . . .
P3 P 0.32501(14) 0.29583(14) 0.61954(11) 0.0231(4) Uani 1 1 d . U . . .
N1 N 0.3035(4) 0.5336(4) 0.7626(3) 0.0202(12) Uani 1 1 d . U . . .
N2 N 0.2611(4) 0.2809(4) 0.6998(3) 0.0221(12) Uani 1 1 d . U . . .
N3 N 0.1192(4) 0.3765(4) 0.8142(3) 0.0245(13) Uani 1 1 d . U . . .
N4 N 0.0691(4) 0.5497(5) 0.7066(4) 0.0302(13) Uani 1 1 d . U . . .
C1 C 0.3386(5) 0.5956(5) 0.8468(4) 0.0244(14) Uani 1 1 d . U . . .
C2 C 0.3507(5) 0.7098(6) 0.8658(4) 0.0337(17) Uani 1 1 d . U . . .
H2 H 0.337172 0.751394 0.819604 0.040 Uiso 1 1 calc R . . . .
C3 C 0.3816(6) 0.7667(6) 0.9492(5) 0.047(2) Uani 1 1 d . U . . .
H3 H 0.391213 0.845768 0.959278 0.056 Uiso 1 1 calc R . . . .
C4 C 0.3984(6) 0.7077(7) 1.0173(5) 0.0441(19) Uani 1 1 d . U . . .
H4 H 0.417985 0.745557 1.074917 0.053 Uiso 1 1 calc R . . . .
C5 C 0.3866(6) 0.5948(7) 1.0011(5) 0.047(2) Uani 1 1 d . U . . .
H5 H 0.399513 0.554308 1.048029 0.056 Uiso 1 1 calc R . . . .
C6 C 0.3559(5) 0.5369(6) 0.9172(4) 0.0310(16) Uani 1 1 d . U . . .
H6 H 0.346664 0.457873 0.907638 0.037 Uiso 1 1 calc R . . . .
C7 C 0.3449(5) 0.6970(5) 0.6445(4) 0.0209(14) Uani 1 1 d . U . . .
C8 C 0.4201(6) 0.7943(5) 0.6792(4) 0.0329(17) Uani 1 1 d . U . . .
H8 H 0.482280 0.792499 0.723152 0.039 Uiso 1 1 calc R . . . .
C9 C 0.4050(6) 0.8934(6) 0.6502(5) 0.0403(18) Uani 1 1 d . U . . .
H9 H 0.458607 0.958927 0.672270 0.048 Uiso 1 1 calc R . . . .
C10 C 0.3113(6) 0.8975(6) 0.5888(4) 0.0386(18) Uani 1 1 d . U . . .
H10 H 0.299859 0.966073 0.569600 0.046 Uiso 1 1 calc R . . . .
C11 C 0.2354(6) 0.8015(6) 0.5561(4) 0.0323(16) Uani 1 1 d . U . . .
H11 H 0.171449 0.803703 0.513811 0.039 Uiso 1 1 calc R . . . .
C12 C 0.2515(5) 0.7027(6) 0.5842(4) 0.0284(16) Uani 1 1 d . U . . .
H12 H 0.197705 0.637273 0.561982 0.034 Uiso 1 1 calc R . . . .
C13 C 0.5135(5) 0.5761(5) 0.7102(4) 0.0230(14) Uani 1 1 d . U . . .
C14 C 0.5619(5) 0.5287(6) 0.7798(4) 0.0283(16) Uani 1 1 d . U . . .
H14 H 0.515687 0.493787 0.814963 0.034 Uiso 1 1 calc R . . . .
C15 C 0.6777(5) 0.5329(6) 0.7975(4) 0.0354(18) Uani 1 1 d . U . . .
H15 H 0.710359 0.501631 0.845392 0.042 Uiso 1 1 calc R . . . .
C16 C 0.7457(6) 0.5814(6) 0.7468(4) 0.0346(17) Uani 1 1 d . U . . .
H16 H 0.824796 0.583784 0.759571 0.041 Uiso 1 1 calc R . . . .
C17 C 0.6986(5) 0.6265(6) 0.6774(4) 0.0341(18) Uani 1 1 d . U . . .
H17 H 0.745749 0.660804 0.642536 0.041 Uiso 1 1 calc R . . . .
C18 C 0.5846(5) 0.6225(5) 0.6578(4) 0.0278(16) Uani 1 1 d . U . . .
H18 H 0.553194 0.651435 0.608290 0.033 Uiso 1 1 calc R . . . .
C19 C 0.2731(6) 0.1880(5) 0.5274(4) 0.0274(15) Uani 1 1 d . U . . .
C20 C 0.1584(6) 0.1441(5) 0.5076(4) 0.0315(16) Uani 1 1 d . U . . .
H20 H 0.108571 0.172868 0.541357 0.038 Uiso 1 1 calc R . . . .
C21 C 0.1170(6) 0.0595(6) 0.4396(4) 0.0398(18) Uani 1 1 d . U . . .
H21 H 0.038550 0.031056 0.427069 0.048 Uiso 1 1 calc R . . . .
C22 C 0.1866(6) 0.0151(6) 0.3892(5) 0.0435(19) Uani 1 1 d . U . . .
H22 H 0.157494 -0.045099 0.343744 0.052 Uiso 1 1 calc R . . . .
C23 C 0.3005(7) 0.0607(6) 0.4067(5) 0.046(2) Uani 1 1 d . U . . .
H23 H 0.349393 0.033165 0.371445 0.055 Uiso 1 1 calc R . . . .
C24 C 0.3432(6) 0.1455(6) 0.4746(4) 0.0374(18) Uani 1 1 d . U . . .
H24 H 0.421279 0.175527 0.485623 0.045 Uiso 1 1 calc R . . . .
C25 C 0.4739(5) 0.2875(5) 0.6419(4) 0.0281(15) Uani 1 1 d . U . . .
C26 C 0.5157(6) 0.2174(6) 0.6955(5) 0.0370(18) Uani 1 1 d . U . . .
H26 H 0.466256 0.174315 0.723954 0.044 Uiso 1 1 calc R . . . .
C27 C 0.6298(6) 0.2086(6) 0.7086(5) 0.0420(19) Uani 1 1 d . U . . .
H27 H 0.657974 0.161267 0.746885 0.050 Uiso 1 1 calc R . . . .
C28 C 0.7006(6) 0.2681(6) 0.6662(5) 0.0402(18) Uani 1 1 d . U . . .
H28 H 0.777785 0.260646 0.674266 0.048 Uiso 1 1 calc R . . . .
C29 C 0.6619(6) 0.3388(6) 0.6120(4) 0.0376(18) Uani 1 1 d . U . . .
H29 H 0.712170 0.380132 0.583064 0.045 Uiso 1 1 calc R . . . .
C30 C 0.5482(5) 0.3498(5) 0.5996(4) 0.0319(16) Uani 1 1 d . U . . .
H30 H 0.521165 0.399243 0.562630 0.038 Uiso 1 1 calc R . . . .
C31 C 0.2628(5) 0.1895(6) 0.7479(4) 0.0266(15) Uani 1 1 d . U . . .
C32 C 0.2017(6) 0.0855(6) 0.7151(5) 0.0402(19) Uani 1 1 d . U . . .
H32 H 0.158665 0.072385 0.658312 0.048 Uiso 1 1 calc R . . . .
C33 C 0.2024(7) -0.0005(7) 0.7645(5) 0.058(2) Uani 1 1 d . U . . .
H33 H 0.159714 -0.071991 0.741082 0.069 Uiso 1 1 calc R . . . .
C34 C 0.2633(7) 0.0164(7) 0.8456(5) 0.049(2) Uani 1 1 d . U . . .
H34 H 0.263285 -0.042838 0.878970 0.059 Uiso 1 1 calc R . . . .
C35 C 0.3248(6) 0.1196(7) 0.8792(5) 0.046(2) Uani 1 1 d . U . . .
H35 H 0.367441 0.131753 0.936104 0.056 Uiso 1 1 calc R . . . .
C36 C 0.3252(6) 0.2056(6) 0.8311(4) 0.0366(17) Uani 1 1 d . U . . .
H36 H 0.368544 0.276577 0.854984 0.044 Uiso 1 1 calc R . . . .
C37 C 0.0539(6) 0.3359(6) 0.8774(4) 0.0363(17) Uani 1 1 d . U . . .
C38 C 0.0089(7) 0.2123(6) 0.8490(6) 0.067(3) Uani 1 1 d . U . . .
H38A H -0.033042 0.200600 0.789629 0.101 Uiso 1 1 calc GR . . . .
H38B H -0.041179 0.185876 0.887324 0.101 Uiso 1 1 calc GR . . . .
H38C H 0.071905 0.170875 0.851613 0.101 Uiso 1 1 calc GR . . . .
C39 C 0.1284(7) 0.3562(8) 0.9669(5) 0.059(2) Uani 1 1 d . U . . .
H39A H 0.193328 0.318082 0.964994 0.088 Uiso 1 1 calc GR . . . .
H39B H 0.084847 0.327053 1.008504 0.088 Uiso 1 1 calc GR . . . .
H39C H 0.154571 0.436356 0.984685 0.088 Uiso 1 1 calc GR . . . .
C40 C -0.0456(6) 0.3986(7) 0.8786(5) 0.054(2) Uani 1 1 d . U . . .
H40A H -0.017561 0.477701 0.900397 0.080 Uiso 1 1 calc GR . . . .
H40B H -0.094249 0.367415 0.916257 0.080 Uiso 1 1 calc GR . . . .
H40C H -0.088815 0.390956 0.819944 0.080 Uiso 1 1 calc GR . . . .
C41 C 0.0138(5) 0.5717(6) 0.6304(5) 0.0372(17) Uani 1 1 d . U . . .
H41 H 0.004142 0.517232 0.580677 0.045 Uiso 1 1 calc R . . . .
C42 C -0.0281(6) 0.6672(7) 0.6217(6) 0.048(2) Uani 1 1 d . U . . .
H42 H -0.064413 0.679217 0.566904 0.057 Uiso 1 1 calc R . . . .
C43 C -0.0175(6) 0.7463(7) 0.6932(6) 0.050(2) Uani 1 1 d . U . . .
H43 H -0.046725 0.813452 0.688637 0.060 Uiso 1 1 calc R . . . .
C44 C 0.0371(6) 0.7260(6) 0.7730(5) 0.0451(19) Uani 1 1 d . U . . .
H44 H 0.045246 0.778556 0.823712 0.054 Uiso 1 1 calc R . . . .
C45 C 0.0784(5) 0.6283(6) 0.7758(5) 0.0344(17) Uani 1 1 d . U . . .
H45 H 0.115951 0.615070 0.829898 0.041 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Ti Cl 2.424(2) . ?
Ti N1 2.130(5) . ?
Ti N2 2.112(5) . ?
Ti N3 1.686(5) . ?
Ti N4 2.255(5) . ?
P1 P2 2.144(2) . ?
P1 N1 1.623(5) . ?
P1 C7 1.830(6) . ?
P1 C13 1.798(6) . ?
P2 P3 2.139(2) . ?
P3 N2 1.614(5) . ?
P3 C19 1.810(7) . ?
P3 C25 1.816(6) . ?
N1 C1 1.421(8) . ?
N2 C31 1.432(8) . ?
N3 C37 1.468(7) . ?
N4 C41 1.364(8) . ?
N4 C45 1.349(8) . ?
C1 C2 1.377(9) . ?
C1 C6 1.405(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.385(9) . ?
C3 H3 0.9500 . ?
C3 C4 1.378(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.359(10) . ?
C5 H5 0.9500 . ?
C5 C6 1.397(9) . ?
C6 H6 0.9500 . ?
C7 C8 1.389(8) . ?
C7 C12 1.382(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.377(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.389(9) . ?
C10 H10 0.9500 . ?
C10 C11 1.377(9) . ?
C11 H11 0.9500 . ?
C11 C12 1.371(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.399(8) . ?
C13 C18 1.404(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.389(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.370(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.375(9) . ?
C17 H17 0.9500 . ?
C17 C18 1.369(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.395(9) . ?
C19 C24 1.401(9) . ?
C20 H20 0.9500 . ?
C20 C21 1.377(9) . ?
C21 H21 0.9500 . ?
C21 C22 1.381(9) . ?
C22 H22 0.9500 . ?
C22 C23 1.391(10) . ?
C23 H23 0.9500 . ?
C23 C24 1.379(9) . ?
C24 H24 0.9500 . ?
C25 C26 1.374(9) . ?
C25 C30 1.407(8) . ?
C26 H26 0.9500 . ?
C26 C27 1.397(9) . ?
C27 H27 0.9500 . ?
C27 C28 1.362(9) . ?
C28 H28 0.9500 . ?
C28 C29 1.373(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.399(9) . ?
C30 H30 0.9500 . ?
C31 C32 1.375(9) . ?
C31 C36 1.391(9) . ?
C32 H32 0.9500 . ?
C32 C33 1.389(9) . ?
C33 H33 0.9500 . ?
C33 C34 1.355(10) . ?
C34 H34 0.9500 . ?
C34 C35 1.371(10) . ?
C35 H35 0.9500 . ?
C35 C36 1.376(9) . ?
C36 H36 0.9500 . ?
C37 C38 1.521(10) . ?
C37 C39 1.530(9) . ?
C37 C40 1.531(9) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41 0.9500 . ?
C41 C42 1.357(10) . ?
C42 H42 0.9500 . ?
C42 C43 1.376(11) . ?
C43 H43 0.9500 . ?
C43 C44 1.402(10) . ?
C44 H44 0.9500 . ?
C44 C45 1.368(9) . ?
C45 H45 0.9500 . ?

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
N1 Ti Cl 154.32(15) . . ?
N1 Ti N4 82.77(19) . . ?
N2 Ti Cl 93.77(15) . . ?
N2 Ti N1 93.05(19) . . ?
N2 Ti N4 162.16(19) . . ?
N3 Ti Cl 98.36(18) . . ?
N3 Ti N1 104.4(2) . . ?
N3 Ti N2 101.7(2) . . ?
N3 Ti N4 96.1(2) . . ?
N4 Ti Cl 83.19(16) . . ?
N1 P1 P2 107.72(19) . . ?
N1 P1 C7 117.4(3) . . ?
N1 P1 C13 110.9(3) . . ?
C7 P1 P2 102.9(2) . . ?
C13 P1 P2 114.7(2) . . ?
C13 P1 C7 103.3(3) . . ?
P3 P2 P1 99.46(10) . . ?
N2 P3 P2 107.4(2) . . ?
N2 P3 C19 113.7(3) . . ?
N2 P3 C25 114.5(3) . . ?
C19 P3 P2 103.5(2) . . ?
C19 P3 C25 102.2(3) . . ?
C25 P3 P2 115.1(2) . . ?
P1 N1 Ti 111.7(3) . . ?
C1 N1 Ti 126.1(4) . . ?
C1 N1 P1 121.9(4) . . ?
P3 N2 Ti 112.9(3) . . ?
C31 N2 Ti 122.1(4) . . ?
C31 N2 P3 124.8(4) . . ?
C37 N3 Ti 163.7(5) . . ?
C41 N4 Ti 125.3(5) . . ?
C45 N4 Ti 118.3(5) . . ?
C45 N4 C41 116.0(6) . . ?
C2 C1 N1 124.8(6) . . ?
C2 C1 C6 116.7(6) . . ?
C6 C1 N1 118.4(6) . . ?
C1 C2 H2 118.5 . . ?
C1 C2 C3 123.0(7) . . ?
C3 C2 H2 118.5 . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.5(7) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.2(7) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.6(7) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 H6 120.0 . . ?
C5 C6 C1 120.0(7) . . ?
C5 C6 H6 120.0 . . ?
C8 C7 P1 121.0(5) . . ?
C12 C7 P1 120.1(5) . . ?
C12 C7 C8 118.8(6) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 C7 120.4(6) . . ?
C9 C8 H8 119.8 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.1(7) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 120.3 . . ?
C11 C10 C9 119.4(7) . . ?
C11 C10 H10 120.3 . . ?
C10 C11 H11 119.8 . . ?
C12 C11 C10 120.3(7) . . ?
C12 C11 H11 119.8 . . ?
C7 C12 H12 119.5 . . ?
C11 C12 C7 120.9(6) . . ?
C11 C12 H12 119.5 . . ?
C14 C13 P1 120.5(5) . . ?
C14 C13 C18 118.1(6) . . ?
C18 C13 P1 121.1(5) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 119.8(6) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.0(6) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 H16 120.2 . . ?
C15 C16 C17 119.6(6) . . ?
C17 C16 H16 120.2 . . ?
C16 C17 H17 119.6 . . ?
C18 C17 C16 120.7(6) . . ?
C18 C17 H17 119.6 . . ?
C13 C18 H18 119.6 . . ?
C17 C18 C13 120.8(6) . . ?
C17 C18 H18 119.6 . . ?
C20 C19 P3 119.2(5) . . ?
C20 C19 C24 117.9(6) . . ?
C24 C19 P3 122.9(5) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.5(7) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 119.2 . . ?
C20 C21 C22 121.6(7) . . ?
C22 C21 H21 119.2 . . ?
C21 C22 H22 120.9 . . ?
C21 C22 C23 118.3(7) . . ?
C23 C22 H22 120.9 . . ?
C22 C23 H23 119.6 . . ?
C24 C23 C22 120.7(7) . . ?
C24 C23 H23 119.6 . . ?
C19 C24 H24 119.6 . . ?
C23 C24 C19 120.9(7) . . ?
C23 C24 H24 119.6 . . ?
C26 C25 P3 122.0(5) . . ?
C26 C25 C30 118.7(6) . . ?
C30 C25 P3 119.2(5) . . ?
C25 C26 H26 119.5 . . ?
C25 C26 C27 121.0(6) . . ?
C27 C26 H26 119.5 . . ?
C26 C27 H27 120.1 . . ?
C28 C27 C26 119.8(7) . . ?
C28 C27 H27 120.1 . . ?
C27 C28 H28 119.5 . . ?
C27 C28 C29 120.9(7) . . ?
C29 C28 H28 119.5 . . ?
C28 C29 H29 120.1 . . ?
C28 C29 C30 119.8(7) . . ?
C30 C29 H29 120.1 . . ?
C25 C30 H30 120.1 . . ?
C29 C30 C25 119.8(6) . . ?
C29 C30 H30 120.1 . . ?
C32 C31 N2 121.9(6) . . ?
C32 C31 C36 118.2(6) . . ?
C36 C31 N2 119.9(6) . . ?
C31 C32 H32 119.8 . . ?
C31 C32 C33 120.5(7) . . ?
C33 C32 H32 119.8 . . ?
C32 C33 H33 119.6 . . ?
C34 C33 C32 120.7(8) . . ?
C34 C33 H33 119.6 . . ?
C33 C34 H34 120.2 . . ?
C33 C34 C35 119.6(7) . . ?
C35 C34 H34 120.2 . . ?
C34 C35 H35 119.8 . . ?
C34 C35 C36 120.5(7) . . ?
C36 C35 H35 119.8 . . ?
C31 C36 H36 119.7 . . ?
C35 C36 C31 120.6(7) . . ?
C35 C36 H36 119.7 . . ?
N3 C37 C38 108.6(6) . . ?
N3 C37 C39 109.9(6) . . ?
N3 C37 C40 108.5(6) . . ?
C38 C37 C39 110.8(7) . . ?
C38 C37 C40 108.9(6) . . ?
C39 C37 C40 110.1(6) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N4 C41 H41 118.1 . . ?
C42 C41 N4 123.7(8) . . ?
C42 C41 H41 118.1 . . ?
C41 C42 H42 120.4 . . ?
C41 C42 C43 119.3(8) . . ?
C43 C42 H42 120.4 . . ?
C42 C43 H43 120.6 . . ?
C42 C43 C44 118.8(8) . . ?
C44 C43 H43 120.6 . . ?
C43 C44 H44 120.9 . . ?
C45 C44 C43 118.2(8) . . ?
C45 C44 H44 120.9 . . ?
N4 C45 C44 124.0(7) . . ?
N4 C45 H45 118.0 . . ?
C44 C45 H45 118.0 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.209 0.000 0.000 399.9 145.8 ?

_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_5b
_database_code_depnum_ccdc_archive 'CCDC 1985135'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne Franche Comte
France
;
_audit_update_record             
;
2020-02-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_audit_creation_date             2018-11-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H38 Cl3 N2 P3 Zr'
_chemical_formula_sum            'C24 H38 Cl3 N2 P3 Zr'
_chemical_formula_weight         645.04
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   16.4550(9)
_cell_length_b                   16.2910(8)
_cell_length_c                   22.0025(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5898.2(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9380
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.512
_cell_measurement_theta_min      2.924
_shelx_estimated_absorpt_T_max   0.905
_shelx_estimated_absorpt_T_min   0.814
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2656
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of dichloromethane and pentane  by slow evaporation'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.124
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            103469
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.534
_diffrn_reflns_theta_min         2.774
_diffrn_ambient_temperature      100
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'κ-geometry diffractometer triump Mo'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       "φ and ω scans'"
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-90C'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5843
_reflns_number_total             6784
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         6784
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0220
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0214P)²+5.0382P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0540
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Zr Zr 0.62085(2) 0.75978(2) 0.38462(2) 0.00821(4) Uani 1 1 d . . . . .
C1 C 0.62011(9) 0.65914(10) 0.51280(7) 0.0119(3) Uani 1 1 d . . . . .
Cl1 Cl 0.61201(3) 0.88433(2) 0.44833(2) 0.01807(9) Uani 1 1 d . . . . .
P1 P 0.76777(2) 0.70323(2) 0.46687(2) 0.00957(8) Uani 1 1 d . . . . .
C2 C 0.61063(11) 0.57527(11) 0.51975(9) 0.0213(4) Uani 1 1 d . . . . .
H2 H 0.638888 0.538629 0.493636 0.026 Uiso 1 1 calc R . . . .
Cl2 Cl 0.49358(2) 0.69212(2) 0.40159(2) 0.01497(8) Uani 1 1 d . . . . .
N2 N 0.66168(7) 0.67785(8) 0.31302(6) 0.0089(2) Uani 1 1 d . . . . .
P2 P 0.79293(2) 0.76238(2) 0.38156(2) 0.00941(8) Uani 1 1 d . . . . .
C3 C 0.55969(12) 0.54433(12) 0.56499(10) 0.0286(4) Uani 1 1 d . . . . .
H3 H 0.553248 0.486696 0.569460 0.034 Uiso 1 1 calc R . . . .
Cl3 Cl 0.57548(3) 0.84772(2) 0.30154(2) 0.01923(9) Uani 1 1 d . . . . .
P3 P 0.76112(2) 0.67499(2) 0.31196(2) 0.00874(8) Uani 1 1 d . . . . .
C4 C 0.51865(12) 0.59707(12) 0.60327(9) 0.0257(4) Uani 1 1 d . . . . .
H4 H 0.485037 0.575908 0.634680 0.031 Uiso 1 1 calc R . . . .
C5 C 0.52674(11) 0.68077(12) 0.59563(8) 0.0230(4) Uani 1 1 d . . . . .
H5 H 0.498211 0.717330 0.621632 0.028 Uiso 1 1 calc R . . . .
C6 C 0.57630(10) 0.71161(11) 0.55019(8) 0.0173(3) Uani 1 1 d . . . . .
H6 H 0.580362 0.769281 0.544545 0.021 Uiso 1 1 calc R . . . .
C7 C 0.82483(10) 0.60853(10) 0.48308(8) 0.0151(3) Uani 1 1 d . . . . .
H7 H 0.799435 0.563443 0.458779 0.018 Uiso 1 1 calc R . . . .
C8 C 0.91305(10) 0.61671(11) 0.46205(8) 0.0192(4) Uani 1 1 d . . . . .
H8A H 0.914217 0.631592 0.418899 0.029 Uiso 1 1 calc GR . . . .
H8B H 0.941212 0.564293 0.467886 0.029 Uiso 1 1 calc GR . . . .
H8C H 0.940234 0.659471 0.485874 0.029 Uiso 1 1 calc GR . . . .
C9 C 0.82171(12) 0.58259(12) 0.55050(9) 0.0259(4) Uani 1 1 d . . . . .
H9A H 0.851832 0.622425 0.575123 0.039 Uiso 1 1 calc GR . . . .
H9B H 0.846299 0.528154 0.555096 0.039 Uiso 1 1 calc GR . . . .
H9C H 0.765023 0.580722 0.564079 0.039 Uiso 1 1 calc GR . . . .
C10 C 0.80901(10) 0.77753(10) 0.52219(7) 0.0152(3) Uani 1 1 d . . . . .
H10 H 0.863340 0.755695 0.534561 0.018 Uiso 1 1 calc R . . . .
C11 C 0.82438(12) 0.86408(11) 0.49809(8) 0.0215(4) Uani 1 1 d . . . . .
H11A H 0.865190 0.861959 0.465692 0.032 Uiso 1 1 calc GR . . . .
H11B H 0.844162 0.899031 0.531187 0.032 Uiso 1 1 calc GR . . . .
H11C H 0.773634 0.886792 0.481932 0.032 Uiso 1 1 calc GR . . . .
C12 C 0.75907(13) 0.78253(13) 0.58004(8) 0.0291(4) Uani 1 1 d . . . . .
H12A H 0.708614 0.812569 0.571955 0.044 Uiso 1 1 calc GR . . . .
H12B H 0.790276 0.811266 0.611445 0.044 Uiso 1 1 calc GR . . . .
H12C H 0.746056 0.726974 0.594083 0.044 Uiso 1 1 calc GR . . . .
C13 C 0.61553(9) 0.63402(9) 0.26807(7) 0.0101(3) Uani 1 1 d . . . . .
C14 C 0.61780(10) 0.65488(10) 0.20676(7) 0.0137(3) Uani 1 1 d . . . . .
H14 H 0.647369 0.701890 0.193958 0.016 Uiso 1 1 calc R . . . .
C15 C 0.57684(10) 0.60702(10) 0.16399(8) 0.0159(3) Uani 1 1 d . . . . .
H15 H 0.579266 0.621154 0.122143 0.019 Uiso 1 1 calc R . . . .
C16 C 0.53276(10) 0.53914(10) 0.18226(8) 0.0176(3) Uani 1 1 d . . . . .
H16 H 0.506403 0.505464 0.153037 0.021 Uiso 1 1 calc R . . . .
C17 C 0.52735(10) 0.52059(10) 0.24392(8) 0.0163(3) Uani 1 1 d . . . . .
H17 H 0.495541 0.475194 0.256905 0.020 Uiso 1 1 calc R . . . .
C18 C 0.56793(9) 0.56779(10) 0.28626(7) 0.0130(3) Uani 1 1 d . . . . .
H18 H 0.563334 0.554946 0.328238 0.016 Uiso 1 1 calc R . . . .
C19 C 0.79864(10) 0.56837(10) 0.31245(8) 0.0147(3) Uani 1 1 d . . . . .
H19 H 0.854050 0.568368 0.331120 0.018 Uiso 1 1 calc R . . . .
C20 C 0.80595(11) 0.53272(11) 0.24785(8) 0.0210(4) Uani 1 1 d . . . . .
H20A H 0.753306 0.536666 0.227236 0.032 Uiso 1 1 calc GR . . . .
H20B H 0.822475 0.475014 0.250272 0.032 Uiso 1 1 calc GR . . . .
H20C H 0.846733 0.563780 0.224945 0.032 Uiso 1 1 calc GR . . . .
C21 C 0.74372(11) 0.51284(10) 0.35124(8) 0.0187(4) Uani 1 1 d . . . . .
H21A H 0.720722 0.544771 0.384838 0.028 Uiso 1 1 calc GR . . . .
H21B H 0.775803 0.467230 0.367598 0.028 Uiso 1 1 calc GR . . . .
H21C H 0.699611 0.491110 0.325996 0.028 Uiso 1 1 calc GR . . . .
C22 C 0.80892(10) 0.72436(10) 0.24615(7) 0.0131(3) Uani 1 1 d . . . . .
H22 H 0.794663 0.691269 0.209385 0.016 Uiso 1 1 calc R . . . .
C23 C 0.90161(10) 0.72323(11) 0.25257(8) 0.0198(4) Uani 1 1 d . . . . .
H23A H 0.917973 0.760890 0.285072 0.030 Uiso 1 1 calc GR . . . .
H23B H 0.926508 0.740564 0.214199 0.030 Uiso 1 1 calc GR . . . .
H23C H 0.919641 0.667501 0.262546 0.030 Uiso 1 1 calc GR . . . .
C24 C 0.77859(11) 0.81206(10) 0.23541(8) 0.0173(3) Uani 1 1 d . . . . .
H24A H 0.719230 0.811804 0.231798 0.026 Uiso 1 1 calc GR . . . .
H24B H 0.802499 0.833604 0.197862 0.026 Uiso 1 1 calc GR . . . .
H24C H 0.794634 0.846877 0.269689 0.026 Uiso 1 1 calc GR . . . .
N1 N 0.66885(8) 0.69239(8) 0.46445(6) 0.0099(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Zr Cl1 2.4704(4) . ?
Zr Cl2 2.3958(4) . ?
Zr N2 2.1713(13) . ?
Zr Cl3 2.4397(4) . ?
Zr N1 2.2168(13) . ?
C1 C2 1.384(2) . ?
C1 C6 1.388(2) . ?
C1 N1 1.4381(19) . ?
P1 P2 2.1502(6) . ?
P1 C7 1.8410(16) . ?
P1 C10 1.8458(16) . ?
P1 N1 1.6381(13) . ?
C2 H2 0.9500 . ?
C2 C3 1.396(2) . ?
N2 P3 1.6371(13) . ?
N2 C13 1.4369(19) . ?
P2 P3 2.1553(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.380(3) . ?
P3 C19 1.8434(16) . ?
P3 C22 1.8337(16) . ?
C4 H4 0.9500 . ?
C4 C5 1.380(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.385(2) . ?
C6 H6 0.9500 . ?
C7 H7 1.0000 . ?
C7 C8 1.529(2) . ?
C7 C9 1.543(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.527(2) . ?
C10 C12 1.517(2) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.392(2) . ?
C13 C18 1.392(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.396(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.382(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.393(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.380(2) . ?
C18 H18 0.9500 . ?
C19 H19 1.0000 . ?
C19 C20 1.540(2) . ?
C19 C21 1.537(2) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22 1.0000 . ?
C22 C23 1.532(2) . ?
C22 C24 1.532(2) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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
Cl2 Zr Cl1 103.765(15) . . ?
Cl2 Zr Cl3 96.857(15) . . ?
N2 Zr Cl1 159.19(3) . . ?
N2 Zr Cl2 95.78(3) . . ?
N2 Zr Cl3 84.95(4) . . ?
N2 Zr N1 99.22(5) . . ?
Cl3 Zr Cl1 85.685(15) . . ?
N1 Zr Cl1 88.75(4) . . ?
N1 Zr Cl2 87.72(3) . . ?
N1 Zr Cl3 173.50(4) . . ?
C2 C1 C6 118.95(15) . . ?
C2 C1 N1 121.09(15) . . ?
C6 C1 N1 119.74(14) . . ?
C7 P1 P2 116.51(6) . . ?
C7 P1 C10 103.55(8) . . ?
C10 P1 P2 102.18(6) . . ?
N1 P1 P2 102.20(5) . . ?
N1 P1 C7 115.01(7) . . ?
N1 P1 C10 117.23(7) . . ?
C1 C2 H2 119.9 . . ?
C1 C2 C3 120.20(17) . . ?
C3 C2 H2 119.9 . . ?
P3 N2 Zr 109.70(6) . . ?
C13 N2 Zr 129.89(9) . . ?
C13 N2 P3 120.29(10) . . ?
P1 P2 P3 106.11(2) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.30(17) . . ?
C4 C3 H3 119.8 . . ?
N2 P3 P2 102.35(5) . . ?
N2 P3 C19 111.19(7) . . ?
N2 P3 C22 115.31(7) . . ?
C19 P3 P2 122.47(6) . . ?
C22 P3 P2 99.62(5) . . ?
C22 P3 C19 105.92(8) . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.58(17) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.21(17) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 H6 119.7 . . ?
C5 C6 C1 120.68(16) . . ?
C5 C6 H6 119.7 . . ?
P1 C7 H7 107.4 . . ?
C8 C7 P1 110.64(12) . . ?
C8 C7 H7 107.4 . . ?
C8 C7 C9 110.26(14) . . ?
C9 C7 P1 113.49(12) . . ?
C9 C7 H7 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P1 C10 H10 106.0 . . ?
C11 C10 P1 115.93(12) . . ?
C11 C10 H10 106.0 . . ?
C12 C10 P1 112.90(12) . . ?
C12 C10 H10 106.0 . . ?
C12 C10 C11 109.35(15) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N2 122.12(14) . . ?
C14 C13 C18 118.88(14) . . ?
C18 C13 N2 118.99(14) . . ?
C13 C14 H14 119.9 . . ?
C13 C14 C15 120.28(15) . . ?
C15 C14 H14 119.9 . . ?
C14 C15 H15 119.9 . . ?
C16 C15 C14 120.29(16) . . ?
C16 C15 H15 119.9 . . ?
C15 C16 H16 120.3 . . ?
C15 C16 C17 119.37(15) . . ?
C17 C16 H16 120.3 . . ?
C16 C17 H17 119.8 . . ?
C18 C17 C16 120.38(15) . . ?
C18 C17 H17 119.8 . . ?
C13 C18 H18 119.7 . . ?
C17 C18 C13 120.66(15) . . ?
C17 C18 H18 119.7 . . ?
P3 C19 H19 107.9 . . ?
C20 C19 P3 112.10(11) . . ?
C20 C19 H19 107.9 . . ?
C21 C19 P3 111.15(11) . . ?
C21 C19 H19 107.9 . . ?
C21 C19 C20 109.65(14) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
P3 C22 H22 107.6 . . ?
C23 C22 P3 110.42(12) . . ?
C23 C22 H22 107.6 . . ?
C24 C22 P3 113.03(11) . . ?
C24 C22 H22 107.6 . . ?
C24 C22 C23 110.48(14) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C1 N1 Zr 125.03(10) . . ?
C1 N1 P1 124.79(11) . . ?
P1 N1 Zr 109.05(6) . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_7b
_database_code_depnum_ccdc_archive 'CCDC 1985144'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne Franche Comte
France
;
_audit_update_record             
;
2020-02-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_audit_creation_date             2020-01-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H47 Au Cl2 N3 P3 Ti, 0.5(C2 H4 Cl4)'
_chemical_formula_sum            'C29 H49 Au Cl4 N3 P3 Ti'
_chemical_formula_weight         919.29
_chemical_melting_point          ?
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'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   14.2921(8)
_cell_length_b                   13.7871(7)
_cell_length_c                   18.9179(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3727.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9644
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.564
_cell_measurement_theta_min      2.955
_shelx_estimated_absorpt_T_max   0.632
_shelx_estimated_absorpt_T_min   0.261
_exptl_absorpt_coefficient_mu    4.585
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_correction_T_min  0.2024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0600 before and 0.0411 after correction.
The Ratio of minimum to maximum transmission is 0.7737.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of dichloromethane and pentane  by slow evaporation'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65977
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.583
_diffrn_reflns_theta_min         2.850
_diffrn_ambient_temperature      100.0
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'κ-geometry diffractometer triump Mo'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       "φ and ω scans'"
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-90C'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4161
_reflns_number_total             4478
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.214
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.235
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         4478
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0249
_refine_ls_restrained_S_all      1.259
_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)+(0.0055P)²+11.9888P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0528
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2-C3 = C3-C4 = C4-C2
 2.44353 with sigma of 0.02
 C1-C2 = C1-C3 = C1-C4
 1.4936 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C1(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C3(0.5) H3A(0.5)
 H3B(0.5) H3C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) H17A(0.5) H17B(0.5)
 Fixed U12: C1(0)
 Fixed U23: C1(0)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14)
5.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10)
5.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Au Au 0.45608(2) 0.750000 0.23527(2) 0.01529(5) Uani 1 2 d S T P A .
Ti Ti 0.37570(5) 0.750000 0.50431(3) 0.01264(13) Uani 1 2 d S T P A .
Cl1 Cl 0.53659(7) 0.750000 0.52191(6) 0.0275(2) Uani 1 2 d S T P . .
N2 N 0.3310(2) 0.750000 0.58657(18) 0.0183(7) Uani 1 2 d S T P . .
P2 P 0.41147(7) 0.750000 0.34899(5) 0.01295(18) Uani 1 2 d S T P . .
C1 C 0.3096(3) 0.7471(14) 0.6620(2) 0.0221(10) Uani 0.5 1 d D . . A -1
Cl2 Cl 0.51116(7) 0.750000 0.12140(5) 0.0211(2) Uani 1 2 d S T P . .
N1 N 0.31218(16) 0.63420(17) 0.45767(11) 0.0148(5) Uani 1 1 d . . . . .
P1 P 0.32489(5) 0.62298(5) 0.37206(3) 0.01279(13) Uani 1 1 d . . . . .
C2 C 0.2120(7) 0.7098(8) 0.6740(4) 0.077(3) Uani 0.5 1 d D U . A -1
H2A H 0.167000 0.752428 0.650280 0.115 Uiso 0.5 1 calc GR . . A -1
H2B H 0.198754 0.708625 0.724855 0.115 Uiso 0.5 1 calc GR . . A -1
H2C H 0.206566 0.644021 0.654822 0.115 Uiso 0.5 1 calc GR . . A -1
C3 C 0.3803(9) 0.6879(9) 0.6999(5) 0.081(3) Uani 0.5 1 d D U . A -1
H3A H 0.381595 0.622353 0.679777 0.121 Uiso 0.5 1 calc GR . . A -1
H3B H 0.363839 0.684240 0.750076 0.121 Uiso 0.5 1 calc GR . . A -1
H3C H 0.442076 0.717858 0.694739 0.121 Uiso 0.5 1 calc GR . . A -1
C4 C 0.3131(7) 0.8494(5) 0.6876(4) 0.0405(19) Uani 0.5 1 d D U . A -1
H4A H 0.377539 0.873474 0.684664 0.061 Uiso 0.5 1 calc GR . . A -1
H4B H 0.291779 0.852068 0.736769 0.061 Uiso 0.5 1 calc GR . . A -1
H4C H 0.272395 0.889882 0.658143 0.061 Uiso 0.5 1 calc GR . . A -1
C5 C 0.2561(2) 0.5673(2) 0.49733(14) 0.0216(6) Uani 1 1 d . . . . .
C6 C 0.2928(3) 0.4779(2) 0.51753(16) 0.0329(8) Uani 1 1 d . . . . .
H6 H 0.354189 0.459578 0.503667 0.039 Uiso 1 1 calc R . . . .
C7 C 0.2385(4) 0.4160(3) 0.5581(2) 0.0592(15) Uani 1 1 d . . . . .
H7 H 0.263475 0.355153 0.572337 0.071 Uiso 1 1 calc R . . . .
C8 C 0.1496(5) 0.4408(4) 0.5780(2) 0.074(2) Uani 1 1 d . . . . .
H8 H 0.113131 0.397430 0.605533 0.088 Uiso 1 1 calc R . . . .
C9 C 0.1139(3) 0.5279(5) 0.5581(2) 0.0643(16) Uani 1 1 d . . . . .
H9 H 0.052162 0.544915 0.572001 0.077 Uiso 1 1 calc R . . . .
C10 C 0.1663(2) 0.5929(3) 0.51743(19) 0.0383(9) Uani 1 1 d . . . . .
H10 H 0.140701 0.653699 0.503837 0.046 Uiso 1 1 calc R . . . .
C11 C 0.21211(19) 0.6102(2) 0.32690(15) 0.0192(6) Uani 1 1 d . . . . .
H11 H 0.171143 0.663087 0.345642 0.023 Uiso 1 1 calc R . . . .
C12 C 0.1627(2) 0.5149(3) 0.34440(18) 0.0322(8) Uani 1 1 d . . . . .
H12A H 0.202257 0.460289 0.329953 0.048 Uiso 1 1 calc GR . . . .
H12B H 0.102962 0.511819 0.319068 0.048 Uiso 1 1 calc GR . . . .
H12C H 0.151205 0.511341 0.395407 0.048 Uiso 1 1 calc GR . . . .
C13 C 0.2157(2) 0.6242(2) 0.24671(16) 0.0263(7) Uani 1 1 d . . . . .
H13A H 0.265085 0.670707 0.234857 0.039 Uiso 1 1 calc GR . . . .
H13B H 0.155302 0.648840 0.230035 0.039 Uiso 1 1 calc GR . . . .
H13C H 0.229001 0.561861 0.223882 0.039 Uiso 1 1 calc GR . . . .
C14 C 0.3984(2) 0.5175(2) 0.35248(15) 0.0191(6) Uani 1 1 d . . . . .
H14 H 0.366087 0.460489 0.374249 0.023 Uiso 1 1 calc R . . . .
C15 C 0.4109(2) 0.4926(2) 0.27423(16) 0.0265(7) Uani 1 1 d . . . . .
H15A H 0.350078 0.475719 0.253682 0.040 Uiso 1 1 calc GR . . . .
H15B H 0.453647 0.437390 0.269608 0.040 Uiso 1 1 calc GR . . . .
H15C H 0.436937 0.548722 0.249273 0.040 Uiso 1 1 calc GR . . . .
C16 C 0.4927(2) 0.5263(2) 0.39029(17) 0.0247(6) Uani 1 1 d . . . . .
H16A H 0.533203 0.570838 0.364020 0.037 Uiso 1 1 calc GR . . . .
H16B H 0.522347 0.462305 0.392872 0.037 Uiso 1 1 calc GR . . . .
H16C H 0.482774 0.551315 0.438197 0.037 Uiso 1 1 calc GR . . . .
Cl3 Cl 0.23280(10) 0.250000 0.39665(9) 0.0460(3) Uani 1 2 d S T P . .
Cl4 Cl 0.03094(13) 0.250000 0.38451(13) 0.1039(10) Uani 1 2 d S T P . .
C17 C 0.1253(5) 0.250000 0.4408(4) 0.066(2) Uani 1 2 d S T P . .
H17A H 0.121767 0.191998 0.471543 0.079 Uiso 0.5 1 calc R . . . .
H17B H 0.121767 0.308002 0.471543 0.079 Uiso 0.5 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Au P2 2.2440(10) . ?
Au Cl2 2.2934(10) . ?
Ti Cl1 2.3234(12) . ?
Ti N2 1.682(3) . ?
Ti P2 2.9823(12) . ?
Ti N1 2.037(2) . ?
Ti N1 2.037(2) 7_575 ?
N2 C1 1.459(5) . ?
P2 P1 2.1884(9) 7_575 ?
P2 P1 2.1883(9) . ?
C1 C2 1.505(11) . ?
C1 C3 1.484(13) . ?
C1 C4 1.492(18) . ?
N1 P1 1.637(2) . ?
N1 C5 1.434(4) . ?
P1 C11 1.833(3) . ?
P1 C14 1.832(3) . ?
C5 C6 1.393(5) . ?
C5 C10 1.385(5) . ?
C6 C7 1.385(5) . ?
C7 C8 1.369(8) . ?
C8 C9 1.357(9) . ?
C9 C10 1.399(6) . ?
C11 C12 1.529(4) . ?
C11 C13 1.530(4) . ?
C14 C15 1.530(4) . ?
C14 C16 1.530(4) . ?
Cl3 C17 1.749(7) . ?
Cl4 C17 1.718(7) . ?

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 Au Cl2 176.43(4) . . ?
Cl1 Ti P2 88.37(4) . . ?
N2 Ti Cl1 104.08(13) . . ?
N2 Ti P2 167.55(13) . . ?
N2 Ti N1 103.38(10) . 7_575 ?
N2 Ti N1 103.38(10) . . ?
N1 Ti Cl1 120.20(7) 7_575 . ?
N1 Ti Cl1 120.20(7) . . ?
N1 Ti P2 69.50(6) . . ?
N1 Ti P2 69.50(6) 7_575 . ?
N1 Ti N1 103.18(13) . 7_575 ?
C1 N2 Ti 169.7(3) . . ?
Au P2 Ti 173.36(5) . . ?
P1 P2 Au 110.60(3) . . ?
P1 P2 Au 110.60(3) 7_575 . ?
P1 P2 Ti 72.94(3) 7_575 . ?
P1 P2 Ti 72.94(3) . . ?
P1 P2 P1 106.31(5) . 7_575 ?
N2 C1 C2 110.6(6) . . ?
N2 C1 C3 110.2(7) . . ?
N2 C1 C4 106.6(10) . . ?
C3 C1 C2 111.7(12) . . ?
C3 C1 C4 109.9(8) . . ?
C4 C1 C2 107.8(9) . . ?
P1 N1 Ti 116.94(13) . . ?
C5 N1 Ti 121.77(17) . . ?
C5 N1 P1 121.25(19) . . ?
N1 P1 P2 100.62(9) . . ?
N1 P1 C11 111.89(13) . . ?
N1 P1 C14 109.80(13) . . ?
C11 P1 P2 118.76(10) . . ?
C14 P1 P2 105.71(10) . . ?
C14 P1 C11 109.49(13) . . ?
C6 C5 N1 120.2(3) . . ?
C10 C5 N1 119.8(3) . . ?
C10 C5 C6 119.9(3) . . ?
C7 C6 C5 119.1(4) . . ?
C8 C7 C6 121.2(5) . . ?
C9 C8 C7 119.7(4) . . ?
C8 C9 C10 121.2(5) . . ?
C5 C10 C9 119.0(4) . . ?
C12 C11 P1 112.8(2) . . ?
C12 C11 C13 109.8(2) . . ?
C13 C11 P1 114.9(2) . . ?
C15 C14 P1 116.2(2) . . ?
C15 C14 C16 111.5(3) . . ?
C16 C14 P1 110.3(2) . . ?
Cl4 C17 Cl3 113.2(4) . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_5a
_database_code_depnum_ccdc_archive 'CCDC 1985141'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne Franche Comte
France
;
_audit_update_record             
;
2020-02-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_audit_creation_date             2018-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C36 H30 Cl3 N2 P3 Zr), 3(C H2 Cl2)'
_chemical_formula_sum            'C147 H126 Cl18 N8 P12 Zr4'
_chemical_formula_weight         3379.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.8938(12)
_cell_length_b                   12.0699(11)
_cell_length_c                   27.548(3)
_cell_angle_alpha                82.319(4)
_cell_angle_beta                 80.357(5)
_cell_angle_gamma                70.217(4)
_cell_volume                     3656.1(6)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9592
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.522
_cell_measurement_theta_min      2.961
_shelx_estimated_absorpt_T_max   0.864
_shelx_estimated_absorpt_T_min   0.743
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0525 before and 0.0415 after correction.
The Ratio of minimum to maximum transmission is 0.9233.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1710
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of dichloromethane and pentane  by slow evaporation'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.19
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            106171
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_min         2.958
_diffrn_ambient_temperature      100
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'κ-geometry diffractometer triump Mo'
_diffrn_measurement_device_type  'Bruker D8 Venture triumph Mo'
_diffrn_measurement_method       "φ and ω scans'"
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-90C'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14964
_reflns_number_total             16785
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_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     865
_refine_ls_number_reflns         16785
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0277
_refine_ls_restrained_S_all      1.037
_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)+(0.0265P)²+4.1469P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0681
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl9-Cl10
 2.916 with sigma of 0.03
 Cl9-C74 = Cl10-C74
 1.771 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl9 \\sim Cl10 \\sim C74: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 Cl9, Cl10, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl9(0.5) Cl10(0.5) C74(0.5) H74A(0.5) H74B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C74(H74A,H74B)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C38(H38), C46(H46), C18(H18), C68(H68), C20(H20), C6(H6),
 C48(H48), C47(H47), C8(H8), C11(H11), C35(H35), C39(H39), C36(H36), C72(H72),
 C54(H54), C24(H24), C44(H44), C15(H15), C45(H45), C21(H21), C16(H16), C32(H32),
  C34(H34), C66(H66), C62(H62), C10(H10), C42(H42), C64(H64), C33(H33),
 C53(H53), C5(H5), C40(H40), C17(H17), C9(H9), C50(H50), C69(H69), C63(H63),
 C65(H65), C56(H56), C60(H60), C22(H22), C30(H30), C51(H51), C52(H52), C41(H41),
  C2(H2), C26(H26), C59(H59), C23(H23), C58(H58), C70(H70), C71(H71), C57(H57),
 C4(H4), C27(H27), C29(H29), C28(H28), C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Zr2 Zr 0.68094(2) 0.08197(2) 0.83597(2) 0.01485(4) Uani 1 1 d . . . . .
Zr1 Zr 0.39289(2) 0.33606(2) 0.34878(2) 0.01701(4) Uani 1 1 d . . . . .
P1 P 0.28631(4) 0.15435(4) 0.41692(2) 0.01049(8) Uani 1 1 d . . . . .
P2 P 0.44372(4) 0.17857(4) 0.43688(2) 0.01318(8) Uani 1 1 d . . . . .
Cl4 Cl 0.65989(5) 0.08059(4) 0.75191(2) 0.02561(10) Uani 1 1 d . . . . .
P6 P 0.82194(4) 0.21431(4) 0.88044(2) 0.01544(9) Uani 1 1 d . . . . .
P4 P 0.52316(4) 0.28881(4) 0.90065(2) 0.01443(9) Uani 1 1 d . . . . .
Cl2 Cl 0.35030(5) 0.40553(4) 0.26694(2) 0.02622(10) Uani 1 1 d . . . . .
P3 P 0.57632(4) 0.09111(4) 0.37839(2) 0.01382(9) Uani 1 1 d . . . . .
P5 P 0.68204(4) 0.16619(4) 0.92947(2) 0.01496(9) Uani 1 1 d . . . . .
Cl5 Cl 0.85107(5) -0.10084(4) 0.84591(2) 0.02733(10) Uani 1 1 d . . . . .
Cl6 Cl 0.54552(5) -0.02385(4) 0.87928(2) 0.02674(10) Uani 1 1 d . . . . .
Cl3 Cl 0.24839(6) 0.49793(4) 0.39490(2) 0.03567(13) Uani 1 1 d . . . . .
Cl1 Cl 0.54819(6) 0.41847(5) 0.35809(2) 0.03649(13) Uani 1 1 d . . . . .
Cl8 Cl 0.10578(5) 0.62388(5) 0.94997(2) 0.03692(13) Uani 1 1 d . . . . .
Cl7 Cl 0.13795(7) 0.57770(6) 0.84626(3) 0.05465(19) Uani 1 1 d . . . . .
N1 N 0.25948(13) 0.24300(12) 0.36734(5) 0.0134(3) Uani 1 1 d . . . . .
N3 N 0.53279(14) 0.24914(13) 0.84528(5) 0.0156(3) Uani 1 1 d . . . . .
N4 N 0.80805(14) 0.18101(13) 0.82682(5) 0.0162(3) Uani 1 1 d . . . . .
N2 N 0.53299(13) 0.17171(13) 0.32812(5) 0.0154(3) Uani 1 1 d . . . . .
C7 C 0.17144(15) 0.19763(15) 0.46958(6) 0.0142(3) Uani 1 1 d . . . . .
C12 C 0.14713(17) 0.30797(16) 0.48731(7) 0.0200(4) Uani 1 1 d . . . . .
H12 H 0.191964 0.358344 0.472364 0.024 Uiso 1 1 calc R . . . .
C13 C 0.29935(15) 0.00340(14) 0.41152(6) 0.0123(3) Uani 1 1 d . . . . .
C14 C 0.35440(16) -0.08276(15) 0.44711(6) 0.0164(3) Uani 1 1 d . . . . .
H14 H 0.387488 -0.061730 0.472192 0.020 Uiso 1 1 calc R . . . .
C38 C 0.42751(17) 0.38544(16) 0.77980(7) 0.0201(4) Uani 1 1 d . . . . .
H38 H 0.489124 0.421035 0.773589 0.024 Uiso 1 1 calc R . . . .
C67 C 0.88781(17) 0.19479(16) 0.78255(6) 0.0186(4) Uani 1 1 d . . . . .
C46 C 0.20204(19) 0.22935(18) 1.00600(7) 0.0244(4) Uani 1 1 d . . . . .
H46 H 0.134825 0.218196 1.027565 0.029 Uiso 1 1 calc R . . . .
C18 C 0.25178(16) -0.02834(16) 0.37458(6) 0.0161(3) Uani 1 1 d . . . . .
H18 H 0.215110 0.029653 0.350050 0.019 Uiso 1 1 calc R . . . .
C68 C 0.8402(2) 0.27286(18) 0.74349(7) 0.0258(4) Uani 1 1 d . . . . .
H68 H 0.755810 0.312264 0.745368 0.031 Uiso 1 1 calc R . . . .
C20 C 0.55288(16) -0.09988(16) 0.33962(7) 0.0173(3) Uani 1 1 d . . . . .
H20 H 0.507712 -0.043013 0.316823 0.021 Uiso 1 1 calc R . . . .
C6 C 0.15483(18) 0.23322(17) 0.29952(7) 0.0206(4) Uani 1 1 d . . . . .
H6 H 0.228187 0.180729 0.284829 0.025 Uiso 1 1 calc R . . . .
C1 C 0.15052(16) 0.27688(16) 0.34461(7) 0.0183(4) Uani 1 1 d . . . . .
C61 C 0.95834(17) 0.12100(17) 0.90565(6) 0.0187(4) Uani 1 1 d . . . . .
C48 C 0.41606(18) 0.17579(17) 0.98274(7) 0.0211(4) Uani 1 1 d . . . . .
H48 H 0.495216 0.127344 0.988225 0.025 Uiso 1 1 calc R . . . .
C31 C 0.60773(16) 0.15546(16) 0.28094(6) 0.0168(3) Uani 1 1 d . . . . .
C47 C 0.31726(19) 0.15991(18) 1.01385(7) 0.0248(4) Uani 1 1 d . . . . .
H47 H 0.329052 0.100825 1.040735 0.030 Uiso 1 1 calc R . . . .
C37 C 0.43299(16) 0.29341(16) 0.81664(6) 0.0165(3) Uani 1 1 d . . . . .
C8 C 0.10557(17) 0.12465(17) 0.49220(7) 0.0210(4) Uani 1 1 d . . . . .
H8 H 0.122363 0.049004 0.480891 0.025 Uiso 1 1 calc R . . . .
C43 C 0.39926(17) 0.26279(16) 0.94343(6) 0.0172(3) Uani 1 1 d . . . . .
C19 C 0.60148(15) -0.06355(16) 0.37497(6) 0.0160(3) Uani 1 1 d . . . . .
C11 C 0.05725(18) 0.34383(17) 0.52684(7) 0.0236(4) Uani 1 1 d . . . . .
H11 H 0.041013 0.418664 0.538825 0.028 Uiso 1 1 calc R . . . .
C35 C 0.64846(18) 0.09075(18) 0.19877(7) 0.0234(4) Uani 1 1 d . . . . .
H35 H 0.626554 0.057874 0.173774 0.028 Uiso 1 1 calc R . . . .
C39 C 0.33188(18) 0.42503(18) 0.75218(7) 0.0249(4) Uani 1 1 d . . . . .
H39 H 0.327951 0.488456 0.727355 0.030 Uiso 1 1 calc R . . . .
C36 C 0.57535(17) 0.10835(16) 0.24399(7) 0.0189(4) Uani 1 1 d . . . . .
H36 H 0.503342 0.088254 0.249683 0.023 Uiso 1 1 calc R . . . .
C72 C 1.01008(18) 0.1332(2) 0.77853(7) 0.0260(4) Uani 1 1 d . . . . .
H72 H 1.042277 0.076574 0.804329 0.031 Uiso 1 1 calc R . . . .
C54 C 0.44326(17) 0.50265(16) 0.94417(7) 0.0193(4) Uani 1 1 d . . . . .
H54 H 0.415464 0.460728 0.972689 0.023 Uiso 1 1 calc R . . . .
C24 C 0.66665(17) -0.14714(18) 0.40888(7) 0.0228(4) Uani 1 1 d . . . . .
H24 H 0.699748 -0.122973 0.433087 0.027 Uiso 1 1 calc R . . . .
C44 C 0.28242(17) 0.33267(16) 0.93549(7) 0.0201(4) Uani 1 1 d . . . . .
H44 H 0.270211 0.392025 0.908722 0.024 Uiso 1 1 calc R . . . .
C15 C 0.36052(18) -0.19898(16) 0.44565(7) 0.0213(4) Uani 1 1 d . . . . .
H15 H 0.397902 -0.257696 0.469803 0.026 Uiso 1 1 calc R . . . .
C45 C 0.18395(18) 0.31557(17) 0.96667(7) 0.0236(4) Uani 1 1 d . . . . .
H45 H 0.104464 0.362742 0.961090 0.028 Uiso 1 1 calc R . . . .
C49 C 0.49860(17) 0.44475(15) 0.90146(7) 0.0172(3) Uani 1 1 d . . . . .
C55 C 0.82190(17) 0.36318(16) 0.88153(7) 0.0198(4) Uani 1 1 d . . . . .
C21 C 0.57049(17) -0.21898(17) 0.33777(7) 0.0226(4) Uani 1 1 d . . . . .
H21 H 0.538311 -0.243724 0.313417 0.027 Uiso 1 1 calc R . . . .
C16 C 0.31230(18) -0.22998(17) 0.40906(7) 0.0232(4) Uani 1 1 d . . . . .
H16 H 0.316577 -0.309785 0.408319 0.028 Uiso 1 1 calc R . . . .
C32 C 0.71087(19) 0.1898(2) 0.27131(7) 0.0267(4) Uani 1 1 d . . . . .
H32 H 0.731338 0.225874 0.295637 0.032 Uiso 1 1 calc R . . . .
C34 C 0.75246(19) 0.1207(2) 0.19002(7) 0.0288(5) Uani 1 1 d . . . . .
H34 H 0.802956 0.107022 0.159345 0.035 Uiso 1 1 calc R . . . .
C66 C 0.96485(18) 0.00942(17) 0.92923(7) 0.0220(4) Uani 1 1 d . . . . .
H66 H 0.896992 -0.017058 0.932871 0.026 Uiso 1 1 calc R . . . .
C62 C 1.05950(18) 0.15715(19) 0.90017(7) 0.0244(4) Uani 1 1 d . . . . .
H62 H 1.056273 0.233135 0.884643 0.029 Uiso 1 1 calc R . . . .
C10 C -0.00832(18) 0.27126(19) 0.54867(7) 0.0257(4) Uani 1 1 d . . . . .
H10 H -0.069638 0.296160 0.575596 0.031 Uiso 1 1 calc R . . . .
C25 C 0.71801(17) 0.09648(19) 0.39146(7) 0.0211(4) Uani 1 1 d . . . . .
C42 C 0.34410(19) 0.23991(18) 0.82395(7) 0.0234(4) Uani 1 1 d . . . . .
H42 H 0.348379 0.175491 0.848308 0.028 Uiso 1 1 calc R . . . .
C64 C 1.17049(19) -0.02650(19) 0.94092(7) 0.0266(4) Uani 1 1 d . . . . .
H64 H 1.242828 -0.076717 0.952782 0.032 Uiso 1 1 calc R . . . .
C33 C 0.7833(2) 0.1711(2) 0.22618(8) 0.0325(5) Uani 1 1 d . . . . .
H33 H 0.854397 0.192816 0.219953 0.039 Uiso 1 1 calc R . . . .
C53 C 0.42896(18) 0.62157(17) 0.94484(7) 0.0233(4) Uani 1 1 d . . . . .
H53 H 0.391834 0.660814 0.973925 0.028 Uiso 1 1 calc R . . . .
C5 C 0.0520(2) 0.2665(2) 0.27619(8) 0.0297(5) Uani 1 1 d . . . . .
H5 H 0.054774 0.235788 0.245846 0.036 Uiso 1 1 calc R . . . .
C40 C 0.24213(18) 0.37314(19) 0.76041(7) 0.0255(4) Uani 1 1 d . . . . .
H40 H 0.176240 0.401513 0.741732 0.031 Uiso 1 1 calc R . . . .
C17 C 0.25837(18) -0.14573(17) 0.37388(7) 0.0217(4) Uani 1 1 d . . . . .
H17 H 0.225419 -0.167533 0.348955 0.026 Uiso 1 1 calc R . . . .
C9 C 0.01526(18) 0.1620(2) 0.53131(8) 0.0285(4) Uani 1 1 d . . . . .
H9 H -0.030486 0.112464 0.546197 0.034 Uiso 1 1 calc R . . . .
C50 C 0.5397(2) 0.50703(17) 0.85993(7) 0.0240(4) Uani 1 1 d . . . . .
H50 H 0.578435 0.467971 0.830944 0.029 Uiso 1 1 calc R . . . .
C69 C 0.9167(2) 0.2929(2) 0.70174(8) 0.0352(5) Uani 1 1 d . . . . .
H69 H 0.884334 0.346798 0.675207 0.042 Uiso 1 1 calc R . . . .
C63 C 1.16511(19) 0.0827(2) 0.91729(8) 0.0281(4) Uani 1 1 d . . . . .
H63 H 1.234262 0.107429 0.912639 0.034 Uiso 1 1 calc R . . . .
C65 C 1.06986(19) -0.06289(19) 0.94734(7) 0.0261(4) Uani 1 1 d . . . . .
H65 H 1.072793 -0.137603 0.964209 0.031 Uiso 1 1 calc R . . . .
C56 C 0.8462(2) 0.43217(19) 0.83897(8) 0.0316(5) Uani 1 1 d . . . . .
H56 H 0.864856 0.400868 0.807653 0.038 Uiso 1 1 calc R . . . .
C60 C 0.7956(2) 0.41007(18) 0.92736(7) 0.0255(4) Uani 1 1 d . . . . .
H60 H 0.779875 0.363109 0.956550 0.031 Uiso 1 1 calc R . . . .
C22 C 0.63484(19) -0.30163(18) 0.37135(8) 0.0276(4) Uani 1 1 d . . . . .
H22 H 0.646485 -0.383117 0.370165 0.033 Uiso 1 1 calc R . . . .
C30 C 0.72490(19) 0.1742(2) 0.42304(7) 0.0278(4) Uani 1 1 d . . . . .
H30 H 0.653931 0.221171 0.441513 0.033 Uiso 1 1 calc R . . . .
C51 C 0.5240(2) 0.62611(18) 0.86090(8) 0.0296(5) Uani 1 1 d . . . . .
H51 H 0.551261 0.668676 0.832473 0.036 Uiso 1 1 calc R . . . .
C52 C 0.4686(2) 0.68283(17) 0.90332(8) 0.0274(4) Uani 1 1 d . . . . .
H52 H 0.457857 0.764340 0.903852 0.033 Uiso 1 1 calc R . . . .
C41 C 0.24927(19) 0.2797(2) 0.79600(8) 0.0276(4) Uani 1 1 d . . . . .
H41 H 0.188900 0.242642 0.801362 0.033 Uiso 1 1 calc R . . . .
C2 C 0.0444(2) 0.3567(2) 0.36507(8) 0.0327(5) Uani 1 1 d . . . . .
H2 H 0.041455 0.388766 0.395112 0.039 Uiso 1 1 calc R . . . .
C26 C 0.82248(18) 0.0291(2) 0.36415(7) 0.0284(5) Uani 1 1 d . . . . .
H26 H 0.818265 -0.025403 0.343200 0.034 Uiso 1 1 calc R . . . .
C59 C 0.7923(2) 0.5248(2) 0.93042(8) 0.0319(5) Uani 1 1 d . . . . .
H59 H 0.773944 0.556449 0.961651 0.038 Uiso 1 1 calc R . . . .
C23 C 0.68252(19) -0.26573(19) 0.40681(8) 0.0284(4) Uani 1 1 d . . . . .
H23 H 0.726407 -0.322941 0.429869 0.034 Uiso 1 1 calc R . . . .
C58 C 0.8158(2) 0.5933(2) 0.88798(9) 0.0356(5) Uani 1 1 d . . . . .
H58 H 0.813194 0.672096 0.890106 0.043 Uiso 1 1 calc R . . . .
C70 C 1.0390(2) 0.2352(2) 0.69861(8) 0.0385(6) Uani 1 1 d . . . . .
H70 H 1.091180 0.250838 0.670433 0.046 Uiso 1 1 calc R . . . .
C71 C 1.0854(2) 0.1542(2) 0.73676(8) 0.0355(5) Uani 1 1 d . . . . .
H71 H 1.169541 0.112869 0.734281 0.043 Uiso 1 1 calc R . . . .
C57 C 0.8429(3) 0.5472(2) 0.84253(8) 0.0398(6) Uani 1 1 d . . . . .
H57 H 0.859491 0.594389 0.813528 0.048 Uiso 1 1 calc R . . . .
C4 C -0.0538(2) 0.3438(2) 0.29701(9) 0.0408(6) Uani 1 1 d . . . . .
H4 H -0.124159 0.365942 0.281142 0.049 Uiso 1 1 calc R . . . .
C27 C 0.9327(2) 0.0414(3) 0.36742(8) 0.0394(6) Uani 1 1 d . . . . .
H27 H 1.003632 -0.002681 0.347984 0.047 Uiso 1 1 calc R . . . .
C29 C 0.8364(2) 0.1823(3) 0.42730(9) 0.0405(6) Uani 1 1 d . . . . .
H29 H 0.842314 0.232561 0.449839 0.049 Uiso 1 1 calc R . . . .
C28 C 0.9384(2) 0.1178(3) 0.39902(9) 0.0448(7) Uani 1 1 d . . . . .
H28 H 1.013915 0.126233 0.401343 0.054 Uiso 1 1 calc R . . . .
C3 C -0.0582(2) 0.3897(2) 0.34114(10) 0.0480(7) Uani 1 1 d . . . . .
H3 H -0.131327 0.443804 0.355145 0.058 Uiso 1 1 calc R . . . .
C73 C 0.1368(2) 0.6764(2) 0.88767(8) 0.0362(5) Uani 1 1 d . . . . .
H73A H 0.075004 0.753506 0.880687 0.043 Uiso 1 1 calc R . . . .
H73B H 0.216166 0.688885 0.882633 0.043 Uiso 1 1 calc R . . . .
Cl9 Cl 0.46699(18) 0.49267(12) 0.49191(7) 0.0575(5) Uani 0.5 1 d D U P A -1
Cl10 Cl 0.72569(15) 0.45141(10) 0.47819(5) 0.0504(3) Uani 0.5 1 d D U P A -1
C74 C 0.5869(5) 0.5213(5) 0.5115(2) 0.0438(14) Uani 0.5 1 d D U P A -1
H74A H 0.572039 0.607614 0.507818 0.053 Uiso 0.5 1 calc R . P A -1
H74B H 0.589681 0.494415 0.546927 0.053 Uiso 0.5 1 calc R . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Zr2 Cl4 2.3734(5) . ?
Zr2 P5 2.8961(6) . ?
Zr2 Cl5 2.4577(5) . ?
Zr2 Cl6 2.4475(5) . ?
Zr2 N3 2.1960(15) . ?
Zr2 N4 2.1893(15) . ?
Zr1 P2 2.8896(5) . ?
Zr1 Cl2 2.3734(5) . ?
Zr1 Cl3 2.4584(5) . ?
Zr1 Cl1 2.4367(6) . ?
Zr1 N1 2.1960(15) . ?
Zr1 N2 2.1868(15) . ?
P1 P2 2.1566(6) . ?
P1 N1 1.6236(14) . ?
P1 C7 1.8165(17) . ?
P1 C13 1.7998(17) . ?
P2 P3 2.1621(6) . ?
P6 P5 2.1499(7) . ?
P6 N4 1.6299(15) . ?
P6 C61 1.820(2) . ?
P6 C55 1.8009(19) . ?
P4 P5 2.1649(7) . ?
P4 N3 1.6336(15) . ?
P4 C43 1.8142(18) . ?
P4 C49 1.8070(18) . ?
P3 N2 1.6337(15) . ?
P3 C19 1.8008(19) . ?
P3 C25 1.8048(18) . ?
Cl8 C73 1.772(2) . ?
Cl7 C73 1.751(3) . ?
N1 C1 1.444(2) . ?
N3 C37 1.445(2) . ?
N4 C67 1.442(2) . ?
N2 C31 1.443(2) . ?
C7 C12 1.401(2) . ?
C7 C8 1.391(3) . ?
C12 C11 1.392(3) . ?
C13 C14 1.398(2) . ?
C13 C18 1.395(2) . ?
C14 C15 1.386(2) . ?
C38 C37 1.393(2) . ?
C38 C39 1.388(3) . ?
C67 C68 1.392(3) . ?
C67 C72 1.384(3) . ?
C46 C47 1.379(3) . ?
C46 C45 1.389(3) . ?
C18 C17 1.395(3) . ?
C68 C69 1.390(3) . ?
C20 C19 1.396(2) . ?
C20 C21 1.388(3) . ?
C6 C1 1.399(3) . ?
C6 C5 1.390(3) . ?
C1 C2 1.387(3) . ?
C61 C66 1.398(3) . ?
C61 C62 1.392(3) . ?
C48 C47 1.387(3) . ?
C48 C43 1.394(3) . ?
C31 C36 1.393(2) . ?
C31 C32 1.397(3) . ?
C37 C42 1.390(3) . ?
C8 C9 1.390(3) . ?
C43 C44 1.396(3) . ?
C19 C24 1.397(3) . ?
C11 C10 1.379(3) . ?
C35 C36 1.392(3) . ?
C35 C34 1.378(3) . ?
C39 C40 1.384(3) . ?
C72 C71 1.387(3) . ?
C54 C49 1.398(3) . ?
C54 C53 1.389(3) . ?
C24 C23 1.387(3) . ?
C44 C45 1.390(3) . ?
C15 C16 1.387(3) . ?
C49 C50 1.394(3) . ?
C55 C56 1.393(3) . ?
C55 C60 1.397(3) . ?
C21 C22 1.382(3) . ?
C16 C17 1.374(3) . ?
C32 C33 1.387(3) . ?
C34 C33 1.390(3) . ?
C66 C65 1.387(3) . ?
C62 C63 1.389(3) . ?
C10 C9 1.385(3) . ?
C25 C30 1.392(3) . ?
C25 C26 1.392(3) . ?
C42 C41 1.386(3) . ?
C64 C63 1.376(3) . ?
C64 C65 1.386(3) . ?
C53 C52 1.381(3) . ?
C5 C4 1.374(3) . ?
C40 C41 1.381(3) . ?
C50 C51 1.389(3) . ?
C69 C70 1.377(4) . ?
C56 C57 1.393(3) . ?
C60 C59 1.385(3) . ?
C22 C23 1.389(3) . ?
C30 C29 1.388(3) . ?
C51 C52 1.385(3) . ?
C2 C3 1.397(3) . ?
C26 C27 1.386(3) . ?
C59 C58 1.385(3) . ?
C58 C57 1.382(3) . ?
C70 C71 1.386(4) . ?
C4 C3 1.388(4) . ?
C27 C28 1.376(4) . ?
C29 C28 1.375(4) . ?
Cl9 C74 1.756(6) . ?
Cl10 C74 1.742(6) . ?

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
Cl4 Zr2 P5 161.135(17) . . ?
Cl4 Zr2 Cl5 100.296(19) . . ?
Cl4 Zr2 Cl6 102.462(19) . . ?
Cl5 Zr2 P5 95.430(17) . . ?
Cl6 Zr2 P5 88.190(17) . . ?
Cl6 Zr2 Cl5 88.61(2) . . ?
N3 Zr2 Cl4 93.30(4) . . ?
N3 Zr2 P5 71.09(4) . . ?
N3 Zr2 Cl5 166.39(4) . . ?
N3 Zr2 Cl6 89.09(4) . . ?
N4 Zr2 Cl4 99.63(4) . . ?
N4 Zr2 P5 70.28(4) . . ?
N4 Zr2 Cl5 88.47(4) . . ?
N4 Zr2 Cl6 157.88(4) . . ?
N4 Zr2 N3 88.63(6) . . ?
Cl2 Zr1 P2 160.485(16) . . ?
Cl2 Zr1 Cl3 100.70(2) . . ?
Cl2 Zr1 Cl1 103.16(2) . . ?
Cl3 Zr1 P2 93.417(18) . . ?
Cl1 Zr1 P2 90.834(18) . . ?
Cl1 Zr1 Cl3 87.20(2) . . ?
N1 Zr1 P2 70.48(4) . . ?
N1 Zr1 Cl2 96.58(4) . . ?
N1 Zr1 Cl3 87.41(4) . . ?
N1 Zr1 Cl1 160.18(4) . . ?
N2 Zr1 P2 71.17(4) . . ?
N2 Zr1 Cl2 95.07(4) . . ?
N2 Zr1 Cl3 164.23(4) . . ?
N2 Zr1 Cl1 89.66(4) . . ?
N2 Zr1 N1 90.37(5) . . ?
N1 P1 P2 103.57(6) . . ?
N1 P1 C7 113.81(8) . . ?
N1 P1 C13 115.52(8) . . ?
C7 P1 P2 104.60(6) . . ?
C13 P1 P2 114.92(6) . . ?
C13 P1 C7 104.19(8) . . ?
P1 P2 Zr1 75.714(18) . . ?
P1 P2 P3 99.19(2) . . ?
P3 P2 Zr1 74.815(19) . . ?
N4 P6 P5 103.39(6) . . ?
N4 P6 C61 114.58(8) . . ?
N4 P6 C55 114.65(8) . . ?
C61 P6 P5 102.93(6) . . ?
C55 P6 P5 116.05(7) . . ?
C55 P6 C61 104.96(9) . . ?
N3 P4 P5 104.17(6) . . ?
N3 P4 C43 113.92(8) . . ?
N3 P4 C49 113.11(8) . . ?
C43 P4 P5 103.79(6) . . ?
C49 P4 P5 117.50(6) . . ?
C49 P4 C43 104.30(8) . . ?
N2 P3 P2 103.99(6) . . ?
N2 P3 C19 112.88(8) . . ?
N2 P3 C25 112.91(8) . . ?
C19 P3 P2 117.54(6) . . ?
C19 P3 C25 104.39(9) . . ?
C25 P3 P2 105.11(6) . . ?
P6 P5 Zr2 75.490(19) . . ?
P6 P5 P4 100.81(3) . . ?
P4 P5 Zr2 74.990(18) . . ?
P1 N1 Zr1 110.24(7) . . ?
C1 N1 Zr1 123.01(11) . . ?
C1 N1 P1 125.44(12) . . ?
P4 N3 Zr2 109.00(8) . . ?
C37 N3 Zr2 125.11(11) . . ?
C37 N3 P4 122.10(12) . . ?
P6 N4 Zr2 109.99(8) . . ?
C67 N4 Zr2 126.10(11) . . ?
C67 N4 P6 122.74(12) . . ?
P3 N2 Zr1 108.78(7) . . ?
C31 N2 Zr1 125.12(11) . . ?
C31 N2 P3 122.06(12) . . ?
C12 C7 P1 119.23(14) . . ?
C8 C7 P1 121.57(14) . . ?
C8 C7 C12 119.19(16) . . ?
C11 C12 C7 119.99(18) . . ?
C14 C13 P1 118.06(13) . . ?
C18 C13 P1 122.09(13) . . ?
C18 C13 C14 119.79(16) . . ?
C15 C14 C13 119.72(17) . . ?
C39 C38 C37 119.88(18) . . ?
C68 C67 N4 118.88(17) . . ?
C72 C67 N4 121.33(17) . . ?
C72 C67 C68 119.79(18) . . ?
C47 C46 C45 120.19(18) . . ?
C17 C18 C13 119.61(17) . . ?
C69 C68 C67 119.7(2) . . ?
C21 C20 C19 120.06(17) . . ?
C5 C6 C1 120.13(19) . . ?
C6 C1 N1 118.85(16) . . ?
C2 C1 N1 121.29(17) . . ?
C2 C1 C6 119.75(18) . . ?
C66 C61 P6 120.39(14) . . ?
C62 C61 P6 120.84(15) . . ?
C62 C61 C66 118.73(18) . . ?
C47 C48 C43 120.02(18) . . ?
C36 C31 N2 119.97(16) . . ?
C36 C31 C32 119.41(17) . . ?
C32 C31 N2 120.59(16) . . ?
C46 C47 C48 120.39(18) . . ?
C38 C37 N3 120.92(16) . . ?
C42 C37 N3 119.90(16) . . ?
C42 C37 C38 119.09(17) . . ?
C9 C8 C7 120.22(18) . . ?
C48 C43 P4 122.96(15) . . ?
C48 C43 C44 119.42(17) . . ?
C44 C43 P4 117.61(14) . . ?
C20 C19 P3 120.26(14) . . ?
C20 C19 C24 119.93(17) . . ?
C24 C19 P3 119.78(14) . . ?
C10 C11 C12 120.33(18) . . ?
C34 C35 C36 120.37(18) . . ?
C40 C39 C38 120.73(18) . . ?
C35 C36 C31 120.02(17) . . ?
C67 C72 C71 119.8(2) . . ?
C53 C54 C49 119.91(17) . . ?
C23 C24 C19 119.31(18) . . ?
C45 C44 C43 120.14(18) . . ?
C14 C15 C16 120.28(18) . . ?
C46 C45 C44 119.83(19) . . ?
C54 C49 P4 120.53(13) . . ?
C50 C49 P4 119.89(14) . . ?
C50 C49 C54 119.52(16) . . ?
C56 C55 P6 122.82(15) . . ?
C56 C55 C60 119.49(17) . . ?
C60 C55 P6 117.69(14) . . ?
C22 C21 C20 120.00(18) . . ?
C17 C16 C15 120.27(17) . . ?
C33 C32 C31 119.89(18) . . ?
C35 C34 C33 119.86(18) . . ?
C65 C66 C61 120.38(18) . . ?
C63 C62 C61 120.35(19) . . ?
C11 C10 C9 119.96(18) . . ?
C30 C25 P3 122.56(15) . . ?
C30 C25 C26 119.75(18) . . ?
C26 C25 P3 117.27(14) . . ?
C41 C42 C37 120.54(18) . . ?
C63 C64 C65 119.7(2) . . ?
C32 C33 C34 120.35(19) . . ?
C52 C53 C54 120.12(18) . . ?
C4 C5 C6 120.0(2) . . ?
C41 C40 C39 119.40(18) . . ?
C16 C17 C18 120.32(17) . . ?
C10 C9 C8 120.30(19) . . ?
C51 C50 C49 120.06(18) . . ?
C70 C69 C68 120.4(2) . . ?
C64 C63 C62 120.60(19) . . ?
C64 C65 C66 120.2(2) . . ?
C57 C56 C55 119.70(19) . . ?
C59 C60 C55 120.28(18) . . ?
C21 C22 C23 120.11(19) . . ?
C29 C30 C25 119.4(2) . . ?
C52 C51 C50 120.00(18) . . ?
C53 C52 C51 120.38(18) . . ?
C40 C41 C42 120.31(19) . . ?
C1 C2 C3 119.5(2) . . ?
C27 C26 C25 120.2(2) . . ?
C58 C59 C60 120.05(19) . . ?
C24 C23 C22 120.60(19) . . ?
C57 C58 C59 120.0(2) . . ?
C69 C70 C71 119.7(2) . . ?
C70 C71 C72 120.5(2) . . ?
C58 C57 C56 120.4(2) . . ?
C5 C4 C3 120.2(2) . . ?
C28 C27 C26 119.5(2) . . ?
C28 C29 C30 120.2(2) . . ?
C29 C28 C27 120.9(2) . . ?
C4 C3 C2 120.4(2) . . ?
Cl7 C73 Cl8 112.05(14) . . ?
Cl10 C74 Cl9 112.7(3) . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'


_vrf_PLAT910_5a                  
;
PROBLEM: Missing of FCF Reflections below Theta (Min)
RESPONSE: Most of the missing reflections were excluded by the OMIT command in 
order to avoid problems related to saturation to low theta reflections 
and beamstop.
;
####################################################################### 
# 
# 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_4a
_database_code_depnum_ccdc_archive 'CCDC 1985140'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne Franche Comte
France
;
_audit_update_record             
;
2020-02-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_audit_creation_date             2020-01-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H20 B, C52 H48 N2 O2 P3 Ti, C H2 Cl2'
_chemical_formula_sum            'C77 H70 B Cl2 N2 O2 P3 Ti'
_chemical_formula_weight         1277.87
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7665(19)
_cell_length_b                   13.781(2)
_cell_length_c                   20.643(3)
_cell_angle_alpha                82.299(4)
_cell_angle_beta                 86.711(4)
_cell_angle_gamma                80.965(4)
_cell_volume                     3273.8(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6600
_cell_measurement_temperature    115
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.24
_shelx_estimated_absorpt_T_max   0.974
_shelx_estimated_absorpt_T_min   0.878
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.9420
_exptl_absorpt_correction_T_min  0.8781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0649 before and 0.0561 after correction. The Ratio of minimum to maximum transmission is 0.9322. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       blade
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_unetI/netI     0.0943
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39257
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.042
_diffrn_reflns_theta_max         25.042
_diffrn_reflns_theta_min         2.605
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7230
_reflns_number_total             11547
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.342
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         11547
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0594
_refine_ls_restrained_S_all      1.024
_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)+(0.0745P)²+3.4435P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1675
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C78(H78A,H78B)
2.b Aromatic/amide H refined with riding coordinates:
 C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61),
 C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C69(H69), C70(H70), C71(H71),
  C73(H73), C74(H74), C75(H75), C76(H76), C77(H77), C2(H2), C3(H3), C4(H4),
 C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C39(H39), C40(H40), C41(H41), C47(H47),
  C48(H48), C49(H49)
2.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
B B 0.9339(4) 0.7918(3) 0.6720(2) 0.0222(10) Uani 1 1 d . . . . .
C53 C 1.0319(3) 0.8595(3) 0.64022(19) 0.0220(9) Uani 1 1 d . . . . .
C54 C 1.1454(3) 0.8355(3) 0.6614(2) 0.0269(10) Uani 1 1 d . . . . .
H54 H 1.164317 0.777510 0.691515 0.032 Uiso 1 1 calc R . . . .
C55 C 1.2308(4) 0.8920(3) 0.6407(2) 0.0314(10) Uani 1 1 d . . . . .
H55 H 1.306201 0.872356 0.656595 0.038 Uiso 1 1 calc R . . . .
C56 C 1.2067(4) 0.9771(3) 0.5970(2) 0.0282(10) Uani 1 1 d . . . . .
H56 H 1.264308 1.017571 0.583559 0.034 Uiso 1 1 calc R . . . .
C57 C 1.0972(4) 1.0020(3) 0.5732(2) 0.0294(10) Uani 1 1 d . . . . .
H57 H 1.079765 1.059349 0.542285 0.035 Uiso 1 1 calc R . . . .
C58 C 1.0126(3) 0.9442(3) 0.59401(19) 0.0222(9) Uani 1 1 d . . . . .
H58 H 0.938391 0.962734 0.576272 0.027 Uiso 1 1 calc R . . . .
C59 C 0.9444(3) 0.7800(3) 0.75191(19) 0.0217(9) Uani 1 1 d . . . . .
C60 C 0.9638(4) 0.8610(3) 0.7827(2) 0.0387(12) Uani 1 1 d . . . . .
H60 H 0.968356 0.922491 0.756457 0.046 Uiso 1 1 calc R . . . .
C61 C 0.9766(4) 0.8552(3) 0.8496(2) 0.0410(12) Uani 1 1 d . . . . .
H61 H 0.990258 0.911686 0.867979 0.049 Uiso 1 1 calc R . . . .
C62 C 0.9694(4) 0.7673(3) 0.8894(2) 0.0321(11) Uani 1 1 d . . . . .
H62 H 0.975791 0.763241 0.935417 0.038 Uiso 1 1 calc R . . . .
C63 C 0.9530(4) 0.6860(3) 0.8613(2) 0.0317(11) Uani 1 1 d . . . . .
H63 H 0.949984 0.624576 0.887884 0.038 Uiso 1 1 calc R . . . .
C64 C 0.9407(3) 0.6931(3) 0.7942(2) 0.0254(10) Uani 1 1 d . . . . .
H64 H 0.929195 0.635529 0.776378 0.030 Uiso 1 1 calc R . . . .
C65 C 0.9548(3) 0.6832(3) 0.64474(18) 0.0190(9) Uani 1 1 d . . . . .
C66 C 0.8731(3) 0.6184(3) 0.65891(19) 0.0232(9) Uani 1 1 d . . . . .
H66 H 0.807738 0.636865 0.686295 0.028 Uiso 1 1 calc R . . . .
C67 C 0.8844(3) 0.5281(3) 0.6343(2) 0.0267(10) Uani 1 1 d . . . . .
H67 H 0.827426 0.486216 0.644930 0.032 Uiso 1 1 calc R . . . .
C69 C 0.9787(3) 0.4992(3) 0.5942(2) 0.0282(10) Uani 1 1 d . . . . .
H69 H 0.986791 0.437686 0.577198 0.034 Uiso 1 1 calc R . . . .
C70 C 1.0602(3) 0.5605(3) 0.5795(2) 0.0265(10) Uani 1 1 d . . . . .
H70 H 1.125057 0.541310 0.551965 0.032 Uiso 1 1 calc R . . . .
C71 C 1.0487(3) 0.6508(3) 0.60457(18) 0.0217(9) Uani 1 1 d . . . . .
H71 H 1.106831 0.691567 0.593950 0.026 Uiso 1 1 calc R . . . .
C72 C 0.8031(3) 0.8434(3) 0.65036(19) 0.0202(9) Uani 1 1 d . . . . .
C73 C 0.7128(3) 0.8745(3) 0.6933(2) 0.0263(10) Uani 1 1 d . . . . .
H73 H 0.727141 0.869320 0.738553 0.032 Uiso 1 1 calc R . . . .
C74 C 0.6027(4) 0.9128(3) 0.6724(2) 0.0335(11) Uani 1 1 d . . . . .
H74 H 0.544453 0.934239 0.703344 0.040 Uiso 1 1 calc R . . . .
C75 C 0.5768(4) 0.9200(3) 0.6081(2) 0.0326(11) Uani 1 1 d . . . . .
H75 H 0.501140 0.945485 0.594180 0.039 Uiso 1 1 calc R . . . .
C76 C 0.6631(4) 0.8894(3) 0.5637(2) 0.0318(11) Uani 1 1 d . . . . .
H76 H 0.647282 0.893911 0.518714 0.038 Uiso 1 1 calc R . . . .
C77 C 0.7726(3) 0.8523(3) 0.5851(2) 0.0259(10) Uani 1 1 d . . . . .
H77 H 0.830397 0.831783 0.553589 0.031 Uiso 1 1 calc R . . . .
C1 C 0.5344(3) 0.5034(3) 0.33033(18) 0.0183(9) Uani 1 1 d . . . . .
C2 C 0.6291(3) 0.4588(3) 0.36591(19) 0.0225(9) Uani 1 1 d . . . . .
H2 H 0.692968 0.492739 0.367502 0.027 Uiso 1 1 calc R . . . .
C3 C 0.6303(4) 0.3642(3) 0.3993(2) 0.0294(10) Uani 1 1 d . . . . .
H3 H 0.693453 0.334881 0.425491 0.035 Uiso 1 1 calc R . . . .
C4 C 0.5408(3) 0.3128(3) 0.3946(2) 0.0266(10) Uani 1 1 d . . . . .
H4 H 0.542864 0.247708 0.417084 0.032 Uiso 1 1 calc R . . . .
C5 C 0.4476(3) 0.3556(3) 0.3573(2) 0.0234(9) Uani 1 1 d . . . . .
H5 H 0.386289 0.319633 0.353435 0.028 Uiso 1 1 calc R . . . .
C6 C 0.4442(3) 0.4510(3) 0.32562(19) 0.0199(9) Uani 1 1 d . . . . .
H6 H 0.379820 0.480825 0.300507 0.024 Uiso 1 1 calc R . . . .
C7 C 0.6377(3) 0.6984(3) 0.38637(19) 0.0225(9) Uani 1 1 d . . . . .
C8 C 0.6255(4) 0.6439(3) 0.4479(2) 0.0287(10) Uani 1 1 d . . . . .
H8 H 0.558393 0.613959 0.458938 0.034 Uiso 1 1 calc R . . . .
C9 C 0.7107(4) 0.6337(3) 0.4924(2) 0.0318(11) Uani 1 1 d . . . . .
H9 H 0.702967 0.595305 0.533756 0.038 Uiso 1 1 calc R . . . .
C10 C 0.8069(4) 0.6787(3) 0.4772(2) 0.0324(11) Uani 1 1 d . . . . .
H10 H 0.865873 0.670978 0.507861 0.039 Uiso 1 1 calc R . . . .
C11 C 0.8174(4) 0.7348(3) 0.4177(2) 0.0327(11) Uani 1 1 d . . . . .
H11 H 0.883004 0.767275 0.408006 0.039 Uiso 1 1 calc R . . . .
C12 C 0.7343(4) 0.7449(3) 0.3716(2) 0.0280(10) Uani 1 1 d . . . . .
H12 H 0.743081 0.783128 0.330242 0.034 Uiso 1 1 calc R . . . .
C13 C 0.3963(3) 0.7331(3) 0.37807(18) 0.0193(9) Uani 1 1 d . . . . .
C14 C 0.3880(4) 0.8188(3) 0.4089(2) 0.0271(10) Uani 1 1 d . . . . .
H14 H 0.447914 0.858360 0.402459 0.033 Uiso 1 1 calc R . . . .
C15 C 0.2928(4) 0.8459(3) 0.4487(2) 0.0298(10) Uani 1 1 d . . . . .
H15 H 0.286000 0.905274 0.468169 0.036 Uiso 1 1 calc R . . . .
C16 C 0.2087(4) 0.7871(3) 0.4599(2) 0.0313(11) Uani 1 1 d . . . . .
H16 H 0.144523 0.805010 0.488155 0.038 Uiso 1 1 calc R . . . .
C17 C 0.2161(4) 0.7017(3) 0.4304(2) 0.0359(11) Uani 1 1 d . . . . .
H17 H 0.156974 0.661459 0.438363 0.043 Uiso 1 1 calc R . . . .
C18 C 0.3107(4) 0.6748(3) 0.3888(2) 0.0288(10) Uani 1 1 d . . . . .
H18 H 0.315677 0.616591 0.368063 0.035 Uiso 1 1 calc R . . . .
C19 C 0.4234(4) 0.9351(3) 0.1362(2) 0.0244(9) Uani 1 1 d . . . . .
C20 C 0.5294(4) 0.9487(3) 0.1052(2) 0.0291(10) Uani 1 1 d . . . . .
H20 H 0.593512 0.897315 0.110481 0.035 Uiso 1 1 calc R . . . .
C21 C 0.5406(4) 1.0373(3) 0.0669(2) 0.0365(11) Uani 1 1 d . . . . .
H21 H 0.612813 1.047109 0.046116 0.044 Uiso 1 1 calc R . . . .
C22 C 0.4467(4) 1.1120(3) 0.0587(2) 0.0370(12) Uani 1 1 d . . . . .
H22 H 0.454725 1.172869 0.032461 0.044 Uiso 1 1 calc R . . . .
C23 C 0.3421(4) 1.0980(3) 0.0885(2) 0.0347(11) Uani 1 1 d . . . . .
H23 H 0.277805 1.148947 0.082225 0.042 Uiso 1 1 calc R . . . .
C24 C 0.3297(4) 1.0099(3) 0.1277(2) 0.0291(10) Uani 1 1 d . . . . .
H24 H 0.257408 1.000874 0.148593 0.035 Uiso 1 1 calc R . . . .
C25 C 0.2795(3) 0.8222(3) 0.23062(19) 0.0223(9) Uani 1 1 d . . . . .
C26 C 0.2439(4) 0.8958(3) 0.27048(19) 0.0284(10) Uani 1 1 d . . . . .
H26 H 0.292602 0.943079 0.275154 0.034 Uiso 1 1 calc R . . . .
C27 C 0.1383(4) 0.9005(4) 0.3032(2) 0.0403(12) Uani 1 1 d . . . . .
H27 H 0.113853 0.950906 0.330379 0.048 Uiso 1 1 calc R . . . .
C28 C 0.0687(4) 0.8318(5) 0.2963(2) 0.0520(15) Uani 1 1 d . . . . .
H28 H -0.005350 0.836386 0.317582 0.062 Uiso 1 1 calc R . . . .
C29 C 0.1044(4) 0.7564(5) 0.2589(3) 0.0552(15) Uani 1 1 d . . . . .
H29 H 0.056354 0.707906 0.256030 0.066 Uiso 1 1 calc R . . . .
C30 C 0.2102(4) 0.7511(3) 0.2256(2) 0.0343(11) Uani 1 1 d . . . . .
H30 H 0.235111 0.699356 0.199586 0.041 Uiso 1 1 calc R . . . .
C31 C 0.3925(3) 0.7178(3) 0.08814(18) 0.0202(9) Uani 1 1 d . . . . .
C32 C 0.4412(4) 0.6479(3) 0.0478(2) 0.0290(10) Uani 1 1 d . . . . .
H32 H 0.510334 0.605327 0.059924 0.035 Uiso 1 1 calc R . . . .
C33 C 0.3904(4) 0.6393(3) -0.0096(2) 0.0344(11) Uani 1 1 d . . . . .
H33 H 0.424603 0.590715 -0.036265 0.041 Uiso 1 1 calc R . . . .
C34 C 0.2900(4) 0.7012(4) -0.0282(2) 0.0389(12) Uani 1 1 d . . . . .
H34 H 0.254734 0.694807 -0.067363 0.047 Uiso 1 1 calc R . . . .
C35 C 0.2419(4) 0.7721(4) 0.0105(2) 0.0352(11) Uani 1 1 d . . . . .
H35 H 0.173662 0.815393 -0.002434 0.042 Uiso 1 1 calc R . . . .
C36 C 0.2920(3) 0.7809(3) 0.0680(2) 0.0277(10) Uani 1 1 d . . . . .
H36 H 0.257810 0.830157 0.094224 0.033 Uiso 1 1 calc R . . . .
C37 C 0.8229(3) 0.6187(3) 0.1406(2) 0.0230(9) Uani 1 1 d . . . . .
C38 C 0.9083(3) 0.5933(3) 0.1866(2) 0.0239(9) Uani 1 1 d . . . . .
C39 C 1.0218(4) 0.5791(3) 0.1634(2) 0.0298(10) Uani 1 1 d . . . . .
H39 H 1.081815 0.562525 0.193662 0.036 Uiso 1 1 calc R . . . .
C40 C 1.0493(4) 0.5886(3) 0.0972(2) 0.0367(12) Uani 1 1 d . . . . .
H40 H 1.127645 0.579394 0.082255 0.044 Uiso 1 1 calc R . . . .
C41 C 0.9640(4) 0.6111(3) 0.0534(2) 0.0410(13) Uani 1 1 d . . . . .
H41 H 0.984002 0.616428 0.007925 0.049 Uiso 1 1 calc R . . . .
C42 C 0.8476(4) 0.6266(3) 0.0734(2) 0.0309(11) Uani 1 1 d . . . . .
C43 C 0.8779(4) 0.5807(4) 0.2586(2) 0.0362(11) Uani 1 1 d . . . . .
H43A H 0.845049 0.645029 0.272155 0.054 Uiso 1 1 calc GR . . . .
H43B H 0.947395 0.553791 0.282976 0.054 Uiso 1 1 calc GR . . . .
H43C H 0.821384 0.534910 0.267773 0.054 Uiso 1 1 calc GR . . . .
C44 C 0.7517(4) 0.6494(4) 0.0253(2) 0.0474(14) Uani 1 1 d . . . . .
H44A H 0.710862 0.592202 0.027597 0.071 Uiso 1 1 calc GR . . . .
H44B H 0.784337 0.663561 -0.019100 0.071 Uiso 1 1 calc GR . . . .
H44C H 0.697751 0.707165 0.036214 0.071 Uiso 1 1 calc GR . . . .
C45 C 0.5334(3) 0.4141(3) 0.18135(19) 0.0217(9) Uani 1 1 d . . . . .
C46 C 0.4258(4) 0.3863(3) 0.1730(2) 0.0271(10) Uani 1 1 d . . . . .
C47 C 0.4211(4) 0.2861(3) 0.1757(2) 0.0348(11) Uani 1 1 d . . . . .
H47 H 0.349970 0.264588 0.169933 0.042 Uiso 1 1 calc R . . . .
C48 C 0.5188(4) 0.2171(3) 0.1867(2) 0.0395(12) Uani 1 1 d . . . . .
H48 H 0.513813 0.148516 0.189270 0.047 Uiso 1 1 calc R . . . .
C49 C 0.6235(4) 0.2467(3) 0.1941(2) 0.0332(11) Uani 1 1 d . . . . .
H49 H 0.689976 0.198247 0.201256 0.040 Uiso 1 1 calc R . . . .
C50 C 0.6330(4) 0.3463(3) 0.19130(19) 0.0249(10) Uani 1 1 d . . . . .
C51 C 0.3210(4) 0.4617(3) 0.1609(2) 0.0333(11) Uani 1 1 d . . . . .
H51A H 0.313788 0.508021 0.193511 0.050 Uiso 1 1 calc GR . . . .
H51B H 0.252721 0.428464 0.164153 0.050 Uiso 1 1 calc GR . . . .
H51C H 0.327598 0.498089 0.117003 0.050 Uiso 1 1 calc GR . . . .
C52 C 0.7465(4) 0.3795(3) 0.1985(2) 0.0321(11) Uani 1 1 d . . . . .
H52A H 0.761077 0.428820 0.161367 0.048 Uiso 1 1 calc GR . . . .
H52B H 0.807989 0.322471 0.199586 0.048 Uiso 1 1 calc GR . . . .
H52C H 0.744672 0.409011 0.239267 0.048 Uiso 1 1 calc GR . . . .
N1 N 0.5323(3) 0.6023(2) 0.29427(15) 0.0175(7) Uani 1 1 d . . . . .
N2 N 0.4462(3) 0.7241(2) 0.14743(15) 0.0194(7) Uani 1 1 d . . . . .
O1 O 0.7100(2) 0.6357(2) 0.16243(13) 0.0250(6) Uani 1 1 d . . . . .
O2 O 0.5392(2) 0.51356(18) 0.18020(12) 0.0218(6) Uani 1 1 d . . . . .
P1 P 0.52568(9) 0.70340(7) 0.32903(5) 0.0186(2) Uani 1 1 d . . . . .
P2 P 0.56308(9) 0.80952(7) 0.24811(5) 0.0208(2) Uani 1 1 d . . . . .
P3 P 0.41679(9) 0.81983(7) 0.18871(5) 0.0197(2) Uani 1 1 d . . . . .
Ti Ti 0.56877(6) 0.62941(5) 0.19716(3) 0.01810(18) Uani 1 1 d . . . . .
C78 C -0.0648(7) 0.8655(6) 0.1196(4) 0.101(3) Uani 1 1 d . . . . .
H78A H -0.047396 0.792322 0.123432 0.122 Uiso 1 1 calc R . . . .
H78B H 0.007119 0.891395 0.125696 0.122 Uiso 1 1 calc R . . . .
Cl1 Cl -0.16811(19) 0.9006(3) 0.17947(15) 0.1791(15) Uani 1 1 d . . . . .
Cl2 Cl -0.1168(4) 0.9123(2) 0.04219(16) 0.1968(17) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
B C53 1.648(6) . ?
B C59 1.646(6) . ?
B C65 1.647(6) . ?
B C72 1.651(6) . ?
C53 C54 1.404(6) . ?
C53 C58 1.403(5) . ?
C54 H54 0.9500 . ?
C54 C55 1.380(6) . ?
C55 H55 0.9500 . ?
C55 C56 1.383(6) . ?
C56 H56 0.9500 . ?
C56 C57 1.381(6) . ?
C57 H57 0.9500 . ?
C57 C58 1.385(6) . ?
C58 H58 0.9500 . ?
C59 C60 1.411(6) . ?
C59 C64 1.389(5) . ?
C60 H60 0.9500 . ?
C60 C61 1.387(6) . ?
C61 H61 0.9500 . ?
C61 C62 1.380(6) . ?
C62 H62 0.9500 . ?
C62 C63 1.373(6) . ?
C63 H63 0.9500 . ?
C63 C64 1.389(6) . ?
C64 H64 0.9500 . ?
C65 C66 1.405(5) . ?
C65 C71 1.396(5) . ?
C66 H66 0.9500 . ?
C66 C67 1.390(5) . ?
C67 H67 0.9500 . ?
C67 C69 1.384(6) . ?
C69 H69 0.9500 . ?
C69 C70 1.370(6) . ?
C70 H70 0.9500 . ?
C70 C71 1.395(5) . ?
C71 H71 0.9500 . ?
C72 C73 1.397(5) . ?
C72 C77 1.399(6) . ?
C73 H73 0.9500 . ?
C73 C74 1.389(6) . ?
C74 H74 0.9500 . ?
C74 C75 1.366(6) . ?
C75 H75 0.9500 . ?
C75 C76 1.382(6) . ?
C76 H76 0.9500 . ?
C76 C77 1.383(6) . ?
C77 H77 0.9500 . ?
C1 C2 1.384(5) . ?
C1 C6 1.388(5) . ?
C1 N1 1.460(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.389(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.372(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.385(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.383(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.398(6) . ?
C7 C12 1.389(6) . ?
C7 P1 1.809(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.377(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.376(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.371(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.383(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.402(5) . ?
C13 C18 1.375(6) . ?
C13 P1 1.803(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.383(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.365(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.384(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.400(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.396(6) . ?
C19 C24 1.387(6) . ?
C19 P3 1.810(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.385(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.388(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.373(6) . ?
C23 H23 0.9500 . ?
C23 C24 1.389(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.390(6) . ?
C25 C30 1.387(6) . ?
C25 P3 1.786(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.376(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.372(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.375(7) . ?
C29 H29 0.9500 . ?
C29 C30 1.385(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.392(5) . ?
C31 C36 1.401(6) . ?
C31 N2 1.428(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.384(6) . ?
C33 H33 0.9500 . ?
C33 C34 1.386(6) . ?
C34 H34 0.9500 . ?
C34 C35 1.378(6) . ?
C35 H35 0.9500 . ?
C35 C36 1.384(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.395(6) . ?
C37 C42 1.394(6) . ?
C37 O1 1.373(4) . ?
C38 C39 1.386(6) . ?
C38 C43 1.503(6) . ?
C39 H39 0.9500 . ?
C39 C40 1.380(6) . ?
C40 H40 0.9500 . ?
C40 C41 1.362(6) . ?
C41 H41 0.9500 . ?
C41 C42 1.399(6) . ?
C42 C44 1.514(6) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.405(6) . ?
C45 C50 1.386(5) . ?
C45 O2 1.380(4) . ?
C46 C47 1.385(6) . ?
C46 C51 1.492(6) . ?
C47 H47 0.9500 . ?
C47 C48 1.380(6) . ?
C48 H48 0.9500 . ?
C48 C49 1.380(6) . ?
C49 H49 0.9500 . ?
C49 C50 1.387(6) . ?
C50 C52 1.500(6) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
N1 P1 1.640(3) . ?
N1 Ti 2.023(3) . ?
N2 P3 1.646(3) . ?
N2 Ti 2.014(3) . ?
O1 Ti 1.782(3) . ?
O2 Ti 1.770(3) . ?
P1 P2 2.1415(14) . ?
P1 Ti 3.0215(13) . ?
P2 P3 2.1460(15) . ?
P2 Ti 2.8125(13) . ?
P3 Ti 2.9246(13) . ?
C78 H78A 0.9900 . ?
C78 H78B 0.9900 . ?
C78 Cl1 1.745(8) . ?
C78 Cl2 1.747(9) . ?

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
C53 B C72 111.7(3) . . ?
C59 B C53 106.7(3) . . ?
C59 B C65 111.4(3) . . ?
C59 B C72 111.0(3) . . ?
C65 B C53 110.8(3) . . ?
C65 B C72 105.4(3) . . ?
C54 C53 B 119.6(3) . . ?
C58 C53 B 125.8(4) . . ?
C58 C53 C54 114.5(4) . . ?
C53 C54 H54 118.3 . . ?
C55 C54 C53 123.4(4) . . ?
C55 C54 H54 118.3 . . ?
C54 C55 H55 119.9 . . ?
C54 C55 C56 120.1(4) . . ?
C56 C55 H55 119.9 . . ?
C55 C56 H56 120.7 . . ?
C57 C56 C55 118.6(4) . . ?
C57 C56 H56 120.7 . . ?
C56 C57 H57 119.7 . . ?
C56 C57 C58 120.6(4) . . ?
C58 C57 H57 119.7 . . ?
C53 C58 H58 118.7 . . ?
C57 C58 C53 122.7(4) . . ?
C57 C58 H58 118.7 . . ?
C60 C59 B 120.3(3) . . ?
C64 C59 B 125.5(4) . . ?
C64 C59 C60 114.2(4) . . ?
C59 C60 H60 118.4 . . ?
C61 C60 C59 123.1(4) . . ?
C61 C60 H60 118.4 . . ?
C60 C61 H61 119.9 . . ?
C62 C61 C60 120.1(4) . . ?
C62 C61 H61 119.9 . . ?
C61 C62 H62 120.6 . . ?
C63 C62 C61 118.7(4) . . ?
C63 C62 H62 120.6 . . ?
C62 C63 H63 119.8 . . ?
C62 C63 C64 120.4(4) . . ?
C64 C63 H63 119.8 . . ?
C59 C64 C63 123.5(4) . . ?
C59 C64 H64 118.3 . . ?
C63 C64 H64 118.3 . . ?
C66 C65 B 120.4(3) . . ?
C71 C65 B 123.9(3) . . ?
C71 C65 C66 115.6(4) . . ?
C65 C66 H66 118.8 . . ?
C67 C66 C65 122.3(4) . . ?
C67 C66 H66 118.8 . . ?
C66 C67 H67 119.9 . . ?
C69 C67 C66 120.1(4) . . ?
C69 C67 H67 119.9 . . ?
C67 C69 H69 120.4 . . ?
C70 C69 C67 119.2(4) . . ?
C70 C69 H69 120.4 . . ?
C69 C70 H70 119.7 . . ?
C69 C70 C71 120.6(4) . . ?
C71 C70 H70 119.7 . . ?
C65 C71 H71 118.9 . . ?
C70 C71 C65 122.2(4) . . ?
C70 C71 H71 118.9 . . ?
C73 C72 B 125.2(4) . . ?
C73 C72 C77 114.3(4) . . ?
C77 C72 B 120.3(3) . . ?
C72 C73 H73 118.7 . . ?
C74 C73 C72 122.5(4) . . ?
C74 C73 H73 118.7 . . ?
C73 C74 H74 119.4 . . ?
C75 C74 C73 121.1(4) . . ?
C75 C74 H74 119.4 . . ?
C74 C75 H75 120.7 . . ?
C74 C75 C76 118.5(4) . . ?
C76 C75 H75 120.7 . . ?
C75 C76 H76 120.1 . . ?
C75 C76 C77 119.8(4) . . ?
C77 C76 H76 120.1 . . ?
C72 C77 H77 118.1 . . ?
C76 C77 C72 123.7(4) . . ?
C76 C77 H77 118.1 . . ?
C2 C1 C6 119.6(3) . . ?
C2 C1 N1 120.4(3) . . ?
C6 C1 N1 119.9(3) . . ?
C1 C2 H2 120.2 . . ?
C1 C2 C3 119.7(4) . . ?
C3 C2 H2 120.2 . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.1(4) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.7(4) . . ?
C6 C5 H5 120.1 . . ?
C1 C6 H6 119.8 . . ?
C5 C6 C1 120.4(4) . . ?
C5 C6 H6 119.8 . . ?
C8 C7 P1 117.4(3) . . ?
C12 C7 C8 119.5(4) . . ?
C12 C7 P1 123.0(3) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 120.0(4) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.3(4) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 120.1 . . ?
C11 C10 C9 119.8(4) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 119.4 . . ?
C10 C11 C12 121.2(4) . . ?
C12 C11 H11 119.4 . . ?
C7 C12 H12 120.4 . . ?
C11 C12 C7 119.2(4) . . ?
C11 C12 H12 120.4 . . ?
C14 C13 P1 116.3(3) . . ?
C18 C13 C14 119.8(4) . . ?
C18 C13 P1 123.8(3) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 C13 120.2(4) . . ?
C15 C14 H14 119.9 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 119.9(4) . . ?
C16 C15 H15 120.0 . . ?
C15 C16 H16 119.7 . . ?
C15 C16 C17 120.7(4) . . ?
C17 C16 H16 119.7 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.0(4) . . ?
C18 C17 H17 120.0 . . ?
C13 C18 C17 119.5(4) . . ?
C13 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C20 C19 P3 117.2(3) . . ?
C24 C19 C20 119.9(4) . . ?
C24 C19 P3 122.8(3) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 C19 119.6(4) . . ?
C21 C20 H20 120.2 . . ?
C20 C21 H21 119.9 . . ?
C20 C21 C22 120.2(4) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 120.0(4) . . ?
C23 C22 H22 120.0 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.5(4) . . ?
C24 C23 H23 119.8 . . ?
C19 C24 C23 119.7(4) . . ?
C19 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C26 C25 P3 118.6(3) . . ?
C30 C25 C26 119.9(4) . . ?
C30 C25 P3 121.5(3) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 C25 120.3(4) . . ?
C27 C26 H26 119.9 . . ?
C26 C27 H27 120.3 . . ?
C28 C27 C26 119.4(5) . . ?
C28 C27 H27 120.3 . . ?
C27 C28 H28 119.5 . . ?
C27 C28 C29 121.0(5) . . ?
C29 C28 H28 119.5 . . ?
C28 C29 H29 120.0 . . ?
C28 C29 C30 120.0(5) . . ?
C30 C29 H29 120.0 . . ?
C25 C30 H30 120.4 . . ?
C29 C30 C25 119.3(4) . . ?
C29 C30 H30 120.4 . . ?
C32 C31 C36 117.9(4) . . ?
C32 C31 N2 119.7(4) . . ?
C36 C31 N2 122.4(3) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 C31 121.1(4) . . ?
C33 C32 H32 119.5 . . ?
C32 C33 H33 119.9 . . ?
C32 C33 C34 120.3(4) . . ?
C34 C33 H33 119.9 . . ?
C33 C34 H34 120.3 . . ?
C35 C34 C33 119.4(4) . . ?
C35 C34 H34 120.3 . . ?
C34 C35 H35 119.7 . . ?
C34 C35 C36 120.6(4) . . ?
C36 C35 H35 119.7 . . ?
C31 C36 H36 119.6 . . ?
C35 C36 C31 120.7(4) . . ?
C35 C36 H36 119.6 . . ?
C42 C37 C38 122.6(4) . . ?
O1 C37 C38 118.5(3) . . ?
O1 C37 C42 118.8(4) . . ?
C37 C38 C43 121.1(4) . . ?
C39 C38 C37 117.5(4) . . ?
C39 C38 C43 121.4(4) . . ?
C38 C39 H39 119.4 . . ?
C40 C39 C38 121.3(4) . . ?
C40 C39 H39 119.4 . . ?
C39 C40 H40 120.0 . . ?
C41 C40 C39 119.9(4) . . ?
C41 C40 H40 120.0 . . ?
C40 C41 H41 119.1 . . ?
C40 C41 C42 121.8(4) . . ?
C42 C41 H41 119.1 . . ?
C37 C42 C41 116.8(4) . . ?
C37 C42 C44 120.8(4) . . ?
C41 C42 C44 122.4(4) . . ?
C38 C43 H43A 109.5 . . ?
C38 C43 H43B 109.5 . . ?
C38 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C50 C45 C46 123.0(4) . . ?
O2 C45 C46 118.1(3) . . ?
O2 C45 C50 118.9(4) . . ?
C45 C46 C51 121.5(4) . . ?
C47 C46 C45 117.3(4) . . ?
C47 C46 C51 121.3(4) . . ?
C46 C47 H47 119.6 . . ?
C48 C47 C46 120.7(4) . . ?
C48 C47 H47 119.6 . . ?
C47 C48 H48 119.7 . . ?
C47 C48 C49 120.6(4) . . ?
C49 C48 H48 119.7 . . ?
C48 C49 H49 119.6 . . ?
C48 C49 C50 120.9(4) . . ?
C50 C49 H49 119.6 . . ?
C45 C50 C49 117.4(4) . . ?
C45 C50 C52 121.1(4) . . ?
C49 C50 C52 121.4(4) . . ?
C46 C51 H51A 109.5 . . ?
C46 C51 H51B 109.5 . . ?
C46 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C1 N1 P1 124.0(3) . . ?
C1 N1 Ti 124.3(2) . . ?
P1 N1 Ti 110.70(16) . . ?
C31 N2 P3 123.5(3) . . ?
C31 N2 Ti 130.9(2) . . ?
P3 N2 Ti 105.62(17) . . ?
C37 O1 Ti 167.4(3) . . ?
C45 O2 Ti 164.7(3) . . ?
C7 P1 P2 105.70(14) . . ?
C7 P1 Ti 123.39(13) . . ?
C13 P1 C7 102.52(18) . . ?
C13 P1 P2 117.88(13) . . ?
C13 P1 Ti 132.64(13) . . ?
N1 P1 C7 113.92(17) . . ?
N1 P1 C13 114.79(17) . . ?
N1 P1 P2 102.12(12) . . ?
N1 P1 Ti 38.78(11) . . ?
P2 P1 Ti 63.35(4) . . ?
P1 P2 P3 102.25(6) . . ?
P1 P2 Ti 73.77(4) . . ?
P3 P2 Ti 70.84(4) . . ?
C19 P3 P2 102.11(14) . . ?
C19 P3 Ti 131.37(14) . . ?
C25 P3 C19 110.46(19) . . ?
C25 P3 P2 116.65(14) . . ?
C25 P3 Ti 117.11(13) . . ?
N2 P3 C19 111.46(17) . . ?
N2 P3 C25 111.20(18) . . ?
N2 P3 P2 104.54(12) . . ?
N2 P3 Ti 41.55(11) . . ?
P2 P3 Ti 65.28(4) . . ?
N1 Ti P1 30.52(9) . . ?
N1 Ti P2 73.40(9) . . ?
N1 Ti P3 91.21(9) . . ?
N2 Ti N1 114.19(13) . . ?
N2 Ti P1 98.77(9) . . ?
N2 Ti P2 75.29(9) . . ?
N2 Ti P3 32.83(9) . . ?
O1 Ti N1 124.02(13) . . ?
O1 Ti N2 113.01(13) . . ?
O1 Ti P1 114.49(9) . . ?
O1 Ti P2 91.43(9) . . ?
O1 Ti P3 114.43(9) . . ?
O2 Ti N1 94.33(12) . . ?
O2 Ti N2 101.70(13) . . ?
O2 Ti O1 103.91(12) . . ?
O2 Ti P1 124.23(9) . . ?
O2 Ti P2 164.15(9) . . ?
O2 Ti P3 128.86(9) . . ?
P2 Ti P1 42.88(3) . . ?
P2 Ti P3 43.88(3) . . ?
P3 Ti P1 68.27(3) . . ?
H78A C78 H78B 108.2 . . ?
Cl1 C78 H78A 109.8 . . ?
Cl1 C78 H78B 109.8 . . ?
Cl1 C78 Cl2 109.5(4) . . ?
Cl2 C78 H78A 109.8 . . ?
Cl2 C78 H78B 109.8 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT910_4a                  
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 13 Note
RESPONSE: a set of poorly measured low-order reflections
(too intense or affected by the beamstop) have been
 omitted from the final least-squares refinement.
;
_vrf_PLAT919_4a                  
;
PROBLEM: Reflection # Likely Affected by the Beamstop ... 1 Check
RESPONSE: a set of poorly measured low-order reflections
(too intense or affected by the beamstop) have been
 omitted from the final least-squares refinement.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_9b
_database_code_depnum_ccdc_archive 'CCDC 1985139'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne Franche Comte
France
;
_audit_update_record             
;
2020-02-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_audit_creation_date             2019-05-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H76 Cu2 N4 P6'
_chemical_formula_sum            'C48 H76 Cu2 N4 P6'
_chemical_formula_weight         1022.02
_chemical_melting_point          ?
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'
Cu Cu 0.3201 1.2651 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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                   31.2123(12)
_cell_length_b                   11.3573(4)
_cell_length_c                   16.6578(7)
_cell_angle_alpha                90
_cell_angle_beta                 111.6900(10)
_cell_angle_gamma                90
_cell_volume                     5486.9(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      3.06
_shelx_estimated_absorpt_T_max   0.879
_shelx_estimated_absorpt_T_min   0.679
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0580 before and 0.0465 after correction. The Ratio of minimum to maximum transmission is 0.8392. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2160
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of pentane and toluene  by slow evaporation'
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.134
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31836
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.590
_diffrn_reflns_theta_min         3.045
_diffrn_ambient_temperature      99.99
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'κ-geometry diffractometer triump Mo'
_diffrn_measurement_device_type  'Bruker D8 Venture triumph Mo'
_diffrn_measurement_method       "φ and ω scans'"
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-90C'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5155
_reflns_number_total             6346
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         6346
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0302
_refine_ls_restrained_S_all      1.021
_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)+(0.0250P)²+10.0856P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0711
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Cu Cu 0.77105(2) 0.65311(2) 0.53103(2) 0.01564(6) Uani 1 1 d . . . . .
C1 C 0.73857(6) 0.47014(16) 0.60974(12) 0.0155(4) Uani 1 1 d . . . . .
N1 N 0.72416(5) 0.56025(13) 0.54672(10) 0.0167(3) Uani 1 1 d . . . . .
P1 P 0.67153(2) 0.59321(4) 0.48440(3) 0.01325(10) Uani 1 1 d . . . . .
C2 C 0.76754(6) 0.50080(17) 0.69370(12) 0.0198(4) Uani 1 1 d . . . . .
H2 H 0.775411 0.581126 0.707258 0.024 Uiso 1 1 calc R . . . .
N2 N 0.57673(5) 0.78899(14) 0.31963(10) 0.0189(3) Uani 1 1 d . . . . .
P2 P 0.67154(2) 0.78207(4) 0.50118(3) 0.01395(10) Uani 1 1 d . . . . .
C3 C 0.78497(7) 0.41596(19) 0.75743(13) 0.0260(4) Uani 1 1 d . . . . .
H3 H 0.804784 0.438486 0.813891 0.031 Uiso 1 1 calc R . . . .
P3 P 0.60861(2) 0.86008(4) 0.40155(3) 0.01524(10) Uani 1 1 d . . . . .
C4 C 0.77361(7) 0.2989(2) 0.73910(14) 0.0294(5) Uani 1 1 d . . . . .
H4 H 0.785278 0.240843 0.782838 0.035 Uiso 1 1 calc R . . . .
C5 C 0.74519(7) 0.26717(18) 0.65678(15) 0.0282(5) Uani 1 1 d . . . . .
H5 H 0.737355 0.186677 0.643965 0.034 Uiso 1 1 calc R . . . .
C6 C 0.72782(6) 0.35137(17) 0.59215(13) 0.0209(4) Uani 1 1 d . . . . .
H6 H 0.708497 0.327781 0.535614 0.025 Uiso 1 1 calc R . . . .
C7 C 0.62984(6) 0.52366(16) 0.52284(12) 0.0167(4) Uani 1 1 d . . . . .
H7 H 0.635359 0.436795 0.524594 0.020 Uiso 1 1 calc R . . . .
C8 C 0.63717(7) 0.56311(18) 0.61473(13) 0.0230(4) Uani 1 1 d . . . . .
H8A H 0.669531 0.551424 0.652067 0.034 Uiso 1 1 calc GR . . . .
H8B H 0.617410 0.516521 0.636675 0.034 Uiso 1 1 calc GR . . . .
H8C H 0.629256 0.646662 0.614362 0.034 Uiso 1 1 calc GR . . . .
C9 C 0.58002(7) 0.54541(18) 0.46112(14) 0.0264(4) Uani 1 1 d . . . . .
H9A H 0.573784 0.630210 0.456549 0.040 Uiso 1 1 calc GR . . . .
H9B H 0.558754 0.506166 0.483453 0.040 Uiso 1 1 calc GR . . . .
H9C H 0.575713 0.513736 0.403922 0.040 Uiso 1 1 calc GR . . . .
C10 C 0.65779(6) 0.54563(16) 0.37241(11) 0.0171(4) Uani 1 1 d . . . . .
H10 H 0.628924 0.586770 0.335359 0.020 Uiso 1 1 calc R . . . .
C11 C 0.64942(8) 0.41240(17) 0.36038(13) 0.0276(5) Uani 1 1 d . . . . .
H11A H 0.677977 0.370222 0.392913 0.041 Uiso 1 1 calc GR . . . .
H11B H 0.639700 0.392697 0.298926 0.041 Uiso 1 1 calc GR . . . .
H11C H 0.625257 0.389269 0.381616 0.041 Uiso 1 1 calc GR . . . .
C12 C 0.69628(7) 0.58087(18) 0.34099(13) 0.0226(4) Uani 1 1 d . . . . .
H12A H 0.703687 0.664357 0.353543 0.034 Uiso 1 1 calc GR . . . .
H12B H 0.686032 0.567649 0.278568 0.034 Uiso 1 1 calc GR . . . .
H12C H 0.723755 0.533188 0.370752 0.034 Uiso 1 1 calc GR . . . .
C13 C 0.58087(6) 0.77025(16) 0.24087(12) 0.0182(4) Uani 1 1 d . . . . .
C14 C 0.54171(7) 0.7283(2) 0.17300(14) 0.0316(5) Uani 1 1 d . . . . .
H14 H 0.514446 0.711812 0.183678 0.038 Uiso 1 1 calc R . . . .
C15 C 0.54198(8) 0.7105(2) 0.09119(14) 0.0341(5) Uani 1 1 d . . . . .
H15 H 0.514851 0.683177 0.046412 0.041 Uiso 1 1 calc R . . . .
C16 C 0.58138(7) 0.73193(18) 0.07359(13) 0.0240(4) Uani 1 1 d . . . . .
H16 H 0.581318 0.721039 0.017001 0.029 Uiso 1 1 calc R . . . .
C17 C 0.62060(7) 0.76934(17) 0.13980(13) 0.0229(4) Uani 1 1 d . . . . .
H17 H 0.648034 0.782519 0.128965 0.028 Uiso 1 1 calc R . . . .
C18 C 0.62057(7) 0.78802(17) 0.22203(13) 0.0210(4) Uani 1 1 d . . . . .
H18 H 0.648120 0.813448 0.266638 0.025 Uiso 1 1 calc R . . . .
C19 C 0.63326(7) 0.99854(16) 0.37776(13) 0.0213(4) Uani 1 1 d . . . . .
H19 H 0.659411 0.973668 0.360610 0.026 Uiso 1 1 calc R . . . .
C20 C 0.65455(8) 1.08054(18) 0.45547(15) 0.0308(5) Uani 1 1 d . . . . .
H20A H 0.629952 1.117341 0.470023 0.046 Uiso 1 1 calc GR . . . .
H20B H 0.672647 1.141759 0.441049 0.046 Uiso 1 1 calc GR . . . .
H20C H 0.674662 1.034971 0.505025 0.046 Uiso 1 1 calc GR . . . .
C21 C 0.59973(8) 1.06529(19) 0.29938(15) 0.0318(5) Uani 1 1 d . . . . .
H21A H 0.584159 1.009300 0.252975 0.048 Uiso 1 1 calc GR . . . .
H21B H 0.616908 1.122599 0.279038 0.048 Uiso 1 1 calc GR . . . .
H21C H 0.576746 1.106504 0.316185 0.048 Uiso 1 1 calc GR . . . .
C22 C 0.56894(6) 0.89009(17) 0.45799(12) 0.0206(4) Uani 1 1 d . . . . .
H22 H 0.552582 0.814007 0.456768 0.025 Uiso 1 1 calc R . . . .
C23 C 0.53113(7) 0.9772(2) 0.40659(15) 0.0342(5) Uani 1 1 d . . . . .
H23A H 0.543811 1.057156 0.414470 0.051 Uiso 1 1 calc GR . . . .
H23B H 0.505592 0.973482 0.427342 0.051 Uiso 1 1 calc GR . . . .
H23C H 0.519861 0.956504 0.345144 0.051 Uiso 1 1 calc GR . . . .
C24 C 0.59020(7) 0.92441(19) 0.55329(13) 0.0267(4) Uani 1 1 d . . . . .
H24A H 0.613106 0.865301 0.584855 0.040 Uiso 1 1 calc GR . . . .
H24B H 0.565963 0.928515 0.577406 0.040 Uiso 1 1 calc GR . . . .
H24C H 0.605172 1.001431 0.558757 0.040 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Cu Cu 2.5759(4) 7_666 ?
Cu N1 1.8989(15) . ?
Cu P2 2.1798(5) 7_666 ?
C1 N1 1.415(2) . ?
C1 C2 1.400(3) . ?
C1 C6 1.395(3) . ?
N1 P1 1.6296(15) . ?
P1 P2 2.1631(6) . ?
P1 C7 1.8283(18) . ?
P1 C10 1.8343(18) . ?
C2 H2 0.9500 . ?
C2 C3 1.387(3) . ?
N2 P3 1.5814(16) . ?
N2 C13 1.382(2) . ?
P2 P3 2.2332(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.380(3) . ?
P3 C19 1.8566(19) . ?
P3 C22 1.8424(18) . ?
C4 H4 0.9500 . ?
C4 C5 1.378(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.391(3) . ?
C6 H6 0.9500 . ?
C7 H7 1.0000 . ?
C7 C8 1.529(3) . ?
C7 C9 1.534(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.536(3) . ?
C10 C12 1.530(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.406(3) . ?
C13 C18 1.401(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.381(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.387(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.377(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.387(3) . ?
C18 H18 0.9500 . ?
C19 H19 1.0000 . ?
C19 C20 1.533(3) . ?
C19 C21 1.538(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22 1.0000 . ?
C22 C23 1.535(3) . ?
C22 C24 1.528(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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
N1 Cu Cu 102.99(5) . 7_666 ?
N1 Cu P2 165.25(5) . 7_666 ?
P2 Cu Cu 87.510(16) 7_666 7_666 ?
C2 C1 N1 118.17(16) . . ?
C6 C1 N1 123.89(17) . . ?
C6 C1 C2 117.83(17) . . ?
C1 N1 Cu 116.99(11) . . ?
C1 N1 P1 127.44(12) . . ?
P1 N1 Cu 115.57(8) . . ?
N1 P1 P2 101.16(6) . . ?
N1 P1 C7 110.98(8) . . ?
N1 P1 C10 112.45(8) . . ?
C7 P1 P2 110.44(6) . . ?
C7 P1 C10 107.44(8) . . ?
C10 P1 P2 114.35(6) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 C1 121.16(19) . . ?
C3 C2 H2 119.4 . . ?
C13 N2 P3 130.40(13) . . ?
Cu P2 P3 105.08(2) 7_666 . ?
P1 P2 Cu 105.30(2) . 7_666 ?
P1 P2 P3 109.84(3) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.2(2) . . ?
C4 C3 H3 119.9 . . ?
N2 P3 P2 122.61(6) . . ?
N2 P3 C19 115.25(9) . . ?
N2 P3 C22 101.97(9) . . ?
C19 P3 P2 100.06(6) . . ?
C22 P3 P2 105.46(6) . . ?
C22 P3 C19 111.22(9) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.37(19) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 120.9(2) . . ?
C6 C5 H5 119.5 . . ?
C1 C6 H6 119.8 . . ?
C5 C6 C1 120.49(19) . . ?
C5 C6 H6 119.8 . . ?
P1 C7 H7 107.4 . . ?
C8 C7 P1 111.20(13) . . ?
C8 C7 H7 107.4 . . ?
C8 C7 C9 111.30(16) . . ?
C9 C7 P1 111.84(13) . . ?
C9 C7 H7 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P1 C10 H10 108.0 . . ?
C11 C10 P1 112.80(13) . . ?
C11 C10 H10 108.0 . . ?
C12 C10 P1 110.66(13) . . ?
C12 C10 H10 108.0 . . ?
C12 C10 C11 109.27(16) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 C14 117.20(17) . . ?
N2 C13 C18 126.26(17) . . ?
C18 C13 C14 116.53(18) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 C13 121.5(2) . . ?
C15 C14 H14 119.2 . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.8(2) . . ?
C16 C15 H15 119.6 . . ?
C15 C16 H16 120.7 . . ?
C17 C16 C15 118.68(19) . . ?
C17 C16 H16 120.7 . . ?
C16 C17 H17 119.6 . . ?
C16 C17 C18 120.89(18) . . ?
C18 C17 H17 119.6 . . ?
C13 C18 H18 119.2 . . ?
C17 C18 C13 121.52(18) . . ?
C17 C18 H18 119.2 . . ?
P3 C19 H19 105.5 . . ?
C20 C19 P3 114.76(14) . . ?
C20 C19 H19 105.5 . . ?
C20 C19 C21 111.35(17) . . ?
C21 C19 P3 113.15(14) . . ?
C21 C19 H19 105.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
P3 C22 H22 105.3 . . ?
C23 C22 P3 110.95(14) . . ?
C23 C22 H22 105.3 . . ?
C24 C22 P3 117.49(14) . . ?
C24 C22 H22 105.3 . . ?
C24 C22 C23 111.37(17) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu Cu N1 C1 -155.28(12) 7_666 . . . ?
Cu Cu N1 P1 25.46(10) 7_666 . . . ?
Cu N1 P1 P2 -49.08(9) . . . . ?
Cu N1 P1 C7 -166.26(9) . . . . ?
Cu N1 P1 C10 73.35(11) . . . . ?
C1 N1 P1 P2 131.76(15) . . . . ?
C1 N1 P1 C7 14.57(18) . . . . ?
C1 N1 P1 C10 -105.81(16) . . . . ?
C1 C2 C3 C4 -0.5(3) . . . . ?
N1 C1 C2 C3 -176.49(17) . . . . ?
N1 C1 C6 C5 176.80(17) . . . . ?
N1 P1 C7 C8 59.45(15) . . . . ?
N1 P1 C7 C9 -175.44(13) . . . . ?
N1 P1 C10 C11 75.84(16) . . . . ?
N1 P1 C10 C12 -46.92(15) . . . . ?
C2 C1 N1 Cu 54.1(2) . . . . ?
C2 C1 N1 P1 -126.78(16) . . . . ?
C2 C1 C6 C5 0.6(3) . . . . ?
C2 C3 C4 C5 0.6(3) . . . . ?
N2 P3 C19 C20 166.50(14) . . . . ?
N2 P3 C19 C21 37.20(17) . . . . ?
N2 P3 C22 C23 -68.46(16) . . . . ?
N2 P3 C22 C24 161.81(15) . . . . ?
N2 C13 C14 C15 177.9(2) . . . . ?
N2 C13 C18 C17 -178.26(18) . . . . ?
P2 Cu N1 C1 70.2(2) 7_666 . . . ?
P2 Cu N1 P1 -109.08(17) 7_666 . . . ?
P2 P1 C7 C8 -51.90(14) . . . . ?
P2 P1 C7 C9 73.21(14) . . . . ?
P2 P1 C10 C11 -169.52(12) . . . . ?
P2 P1 C10 C12 67.72(14) . . . . ?
P2 P3 C19 C20 -59.97(15) . . . . ?
P2 P3 C19 C21 170.73(13) . . . . ?
P2 P3 C22 C23 162.47(14) . . . . ?
P2 P3 C22 C24 32.75(16) . . . . ?
C3 C4 C5 C6 -0.1(3) . . . . ?
P3 N2 C13 C14 -164.70(16) . . . . ?
P3 N2 C13 C18 15.9(3) . . . . ?
C4 C5 C6 C1 -0.6(3) . . . . ?
C6 C1 N1 Cu -122.09(16) . . . . ?
C6 C1 N1 P1 57.1(2) . . . . ?
C6 C1 C2 C3 -0.1(3) . . . . ?
C7 P1 C10 C11 -46.56(16) . . . . ?
C7 P1 C10 C12 -169.32(13) . . . . ?
C10 P1 C7 C8 -177.23(13) . . . . ?
C10 P1 C7 C9 -52.13(16) . . . . ?
C13 N2 P3 P2 -83.74(18) . . . . ?
C13 N2 P3 C19 38.3(2) . . . . ?
C13 N2 P3 C22 158.93(17) . . . . ?
C13 C14 C15 C16 1.0(4) . . . . ?
C14 C13 C18 C17 2.4(3) . . . . ?
C14 C15 C16 C17 1.2(3) . . . . ?
C15 C16 C17 C18 -1.5(3) . . . . ?
C16 C17 C18 C13 -0.3(3) . . . . ?
C18 C13 C14 C15 -2.7(3) . . . . ?
C19 P3 C22 C23 54.90(17) . . . . ?
C19 P3 C22 C24 -74.82(17) . . . . ?
C22 P3 C19 C20 51.09(17) . . . . ?
C22 P3 C19 C21 -78.21(16) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.158 0.250 180.0 42.6 ' '
2 0.000 0.158 0.750 180.0 42.6 ' '
3 0.500 0.342 0.250 180.0 42.6 ' '
4 0.500 0.658 0.750 180.0 42.6 ' '

_vrf_PLAT868_9b                  
;
PROBLEM: ALERTS Due to the Use of _smtbx_masks Suppressed 
RESPONSE: During the refinement, atoms of solvent were 
observed (recrystallisation solvents were pentane, THF 
and tetrahydrofuran), but any attempt to modelise these 
disordered molecules were unsatisfactory and we decided 
to use the bypass procedure (Spek, A.L. (2003), J. Appl. 
Cryst. 36, 7-13).
;

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_6b
_database_code_depnum_ccdc_archive 'CCDC 1985136'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne Franche Comte
France
;
_audit_update_record             
;
2020-02-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_audit_creation_date             2020-01-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H47 Cl N3 P3 Ti'
_chemical_formula_sum            'C28 H47 Cl N3 P3 Ti'
_chemical_formula_weight         601.94
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   19.7139(8)
_cell_length_b                   17.7743(9)
_cell_length_c                   20.2496(9)
_cell_angle_alpha                90
_cell_angle_beta                 112.4110(10)
_cell_angle_gamma                90
_cell_volume                     6559.6(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9068
_cell_measurement_temperature    115
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.29
_shelx_estimated_absorpt_T_max   0.941
_shelx_estimated_absorpt_T_min   0.785
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_T_max  0.8014
_exptl_absorpt_correction_T_min  0.7516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0444 before and 0.0393 after correction. The Ratio of minimum to maximum transmission is 0.9379. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            82653
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.709
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12430
_reflns_number_total             14979
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         14979
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0300
_refine_ls_restrained_S_all      1.059
_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)+(0.0268P)²+5.0800P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0759
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C23(H23), C26(H26), C11A(H11A), C14A(H14A), C23A(H23A),
 C26A(H26A)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22), C6A(H6A), C7A(H7A), C8A(H8A), C9A(H9A), C10A(H10A),
 C18A(H18A), C19A(H19A), C20A(H20A), C21A(H21A), C22A(H22A)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C2A(H2AA,
 H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC), C12A(H12D,H12E,H12F),
 C13A(H13D,H13E,H13F), C15A(H15D,H15E,H15F), C16A(H16D,H16E,H16F), C24A(H24D,
 H24E,H24F), C25A(H25D,H25E,H25F), C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Ti Ti 0.65857(2) 0.33434(2) 0.39231(2) 0.01321(6) Uani 1 1 d . . . . .
Cl Cl 0.60758(2) 0.45345(2) 0.38972(3) 0.02777(10) Uani 1 1 d . . . . .
P1 P 0.55946(2) 0.22110(2) 0.42520(2) 0.01199(8) Uani 1 1 d . . . . .
P2 P 0.60938(2) 0.29235(2) 0.51615(2) 0.01530(8) Uani 1 1 d . . . . .
P3 P 0.72670(2) 0.28833(2) 0.54773(2) 0.01365(8) Uani 1 1 d . . . . .
N1 N 0.59897(7) 0.23739(7) 0.36839(7) 0.0140(3) Uani 1 1 d . . . . .
N2 N 0.74926(7) 0.31644(7) 0.48163(7) 0.0137(3) Uani 1 1 d . . . . .
N3 N 0.69266(7) 0.33736(8) 0.32733(7) 0.0179(3) Uani 1 1 d . . . . .
C1 C 0.71745(9) 0.34566(10) 0.26895(9) 0.0216(3) Uani 1 1 d . . . . .
C2 C 0.65114(13) 0.33815(16) 0.19890(10) 0.0483(6) Uani 1 1 d . . . . .
H2A H 0.628182 0.290212 0.197438 0.073 Uiso 1 1 calc GR . . . .
H2B H 0.666780 0.341930 0.159553 0.073 Uiso 1 1 calc GR . . . .
H2C H 0.616724 0.377581 0.195606 0.073 Uiso 1 1 calc GR . . . .
C3 C 0.75100(13) 0.42391(12) 0.27274(11) 0.0387(5) Uani 1 1 d . . . . .
H3A H 0.715434 0.461430 0.271309 0.058 Uiso 1 1 calc GR . . . .
H3B H 0.765376 0.430736 0.232862 0.058 Uiso 1 1 calc GR . . . .
H3C H 0.793242 0.428692 0.316426 0.058 Uiso 1 1 calc GR . . . .
C4 C 0.77454(16) 0.28604(15) 0.27520(16) 0.0592(8) Uani 1 1 d . . . . .
H4A H 0.814746 0.290904 0.320455 0.089 Uiso 1 1 calc GR . . . .
H4B H 0.792110 0.292395 0.237376 0.089 Uiso 1 1 calc GR . . . .
H4C H 0.752936 0.237055 0.271733 0.089 Uiso 1 1 calc GR . . . .
C5 C 0.59299(9) 0.18711(9) 0.31121(8) 0.0162(3) Uani 1 1 d . . . . .
C6 C 0.53289(9) 0.18903(11) 0.24655(9) 0.0254(4) Uani 1 1 d . . . . .
H6 H 0.494314 0.221933 0.240552 0.030 Uiso 1 1 calc R . . . .
C7 C 0.53039(11) 0.14176(13) 0.19077(10) 0.0355(5) Uani 1 1 d . . . . .
H7 H 0.490065 0.143379 0.147688 0.043 Uiso 1 1 calc R . . . .
C8 C 0.58688(12) 0.09281(12) 0.19879(11) 0.0364(5) Uani 1 1 d . . . . .
H8 H 0.584939 0.061537 0.161286 0.044 Uiso 1 1 calc R . . . .
C9 C 0.64640(13) 0.09030(11) 0.26267(11) 0.0372(5) Uani 1 1 d . . . . .
H9 H 0.684606 0.056988 0.268387 0.045 Uiso 1 1 calc R . . . .
C10 C 0.64969(10) 0.13736(10) 0.31874(10) 0.0269(4) Uani 1 1 d . . . . .
H10 H 0.690252 0.135448 0.361612 0.032 Uiso 1 1 calc R . . . .
C11 C 0.46309(8) 0.25323(9) 0.38967(8) 0.0168(3) Uani 1 1 d . . . . .
H11 H 0.434941 0.216938 0.353030 0.020 Uiso 1 1 calc R . . . .
C12 C 0.45361(10) 0.32999(11) 0.35329(11) 0.0290(4) Uani 1 1 d . . . . .
H12A H 0.477830 0.367731 0.388262 0.043 Uiso 1 1 calc GR . . . .
H12B H 0.402319 0.341710 0.331030 0.043 Uiso 1 1 calc GR . . . .
H12C H 0.474744 0.328771 0.317718 0.043 Uiso 1 1 calc GR . . . .
C13 C 0.42980(9) 0.25365(11) 0.44678(9) 0.0239(4) Uani 1 1 d . . . . .
H13A H 0.437447 0.205532 0.470023 0.036 Uiso 1 1 calc GR . . . .
H13B H 0.378131 0.263631 0.424711 0.036 Uiso 1 1 calc GR . . . .
H13C H 0.452959 0.292048 0.481395 0.036 Uiso 1 1 calc GR . . . .
C14 C 0.55632(8) 0.11874(8) 0.44061(8) 0.0153(3) Uani 1 1 d . . . . .
H14 H 0.601287 0.097597 0.438330 0.018 Uiso 1 1 calc R . . . .
C15 C 0.49205(9) 0.07827(9) 0.38244(9) 0.0219(3) Uani 1 1 d . . . . .
H15A H 0.446571 0.094502 0.384786 0.033 Uiso 1 1 calc GR . . . .
H15B H 0.497206 0.024903 0.389998 0.033 Uiso 1 1 calc GR . . . .
H15C H 0.492299 0.090175 0.336297 0.033 Uiso 1 1 calc GR . . . .
C16 C 0.55808(9) 0.09965(9) 0.51529(9) 0.0201(3) Uani 1 1 d . . . . .
H16A H 0.597008 0.127146 0.550658 0.030 Uiso 1 1 calc GR . . . .
H16B H 0.566262 0.046665 0.523844 0.030 Uiso 1 1 calc GR . . . .
H16C H 0.512080 0.113210 0.518003 0.030 Uiso 1 1 calc GR . . . .
C17 C 0.82223(8) 0.33281(9) 0.48699(8) 0.0142(3) Uani 1 1 d . . . . .
C18 C 0.87609(9) 0.27793(9) 0.49930(9) 0.0187(3) Uani 1 1 d . . . . .
H18 H 0.865805 0.228222 0.506447 0.022 Uiso 1 1 calc R . . . .
C19 C 0.94526(9) 0.29699(10) 0.50098(9) 0.0227(4) Uani 1 1 d . . . . .
H19 H 0.981028 0.259980 0.510045 0.027 Uiso 1 1 calc R . . . .
C20 C 0.96141(9) 0.37054(10) 0.48928(9) 0.0208(3) Uani 1 1 d . . . . .
H20 H 1.007714 0.383030 0.490590 0.025 Uiso 1 1 calc R . . . .
C21 C 0.90759(9) 0.42519(10) 0.47561(9) 0.0205(3) Uani 1 1 d . . . . .
H21 H 0.917646 0.474519 0.466994 0.025 Uiso 1 1 calc R . . . .
C22 C 0.83886(9) 0.40684(9) 0.47470(9) 0.0186(3) Uani 1 1 d . . . . .
H22 H 0.803384 0.444131 0.465819 0.022 Uiso 1 1 calc R . . . .
C23 C 0.75278(9) 0.35772(10) 0.62113(9) 0.0213(3) Uani 1 1 d . . . . .
H23 H 0.729996 0.342000 0.654280 0.026 Uiso 1 1 calc R . . . .
C24 C 0.72253(10) 0.43586(10) 0.59268(10) 0.0293(4) Uani 1 1 d . . . . .
H24A H 0.748171 0.455406 0.564510 0.044 Uiso 1 1 calc GR . . . .
H24B H 0.729310 0.469059 0.632086 0.044 Uiso 1 1 calc GR . . . .
H24C H 0.671168 0.431987 0.563641 0.044 Uiso 1 1 calc GR . . . .
C25 C 0.83597(10) 0.36147(12) 0.66343(10) 0.0311(4) Uani 1 1 d . . . . .
H25A H 0.853864 0.312454 0.681781 0.047 Uiso 1 1 calc GR . . . .
H25B H 0.846300 0.396161 0.702396 0.047 Uiso 1 1 calc GR . . . .
H25C H 0.859763 0.378143 0.632583 0.047 Uiso 1 1 calc GR . . . .
C26 C 0.77601(9) 0.20163(9) 0.58762(8) 0.0183(3) Uani 1 1 d . . . . .
H26 H 0.828507 0.212276 0.602353 0.022 Uiso 1 1 calc R . . . .
C27 C 0.75813(9) 0.13702(9) 0.53395(9) 0.0220(3) Uani 1 1 d . . . . .
H27A H 0.708849 0.120107 0.523403 0.033 Uiso 1 1 calc GR . . . .
H27B H 0.791661 0.096254 0.553876 0.033 Uiso 1 1 calc GR . . . .
H27C H 0.762629 0.154099 0.490825 0.033 Uiso 1 1 calc GR . . . .
C28 C 0.76326(10) 0.17900(12) 0.65499(10) 0.0302(4) Uani 1 1 d . . . . .
H28A H 0.781722 0.217704 0.690429 0.045 Uiso 1 1 calc GR . . . .
H28B H 0.788399 0.132656 0.673299 0.045 Uiso 1 1 calc GR . . . .
H28C H 0.711656 0.172465 0.643444 0.045 Uiso 1 1 calc GR . . . .
TiA Ti 0.69321(2) 0.32779(2) 0.87639(2) 0.01289(6) Uani 1 1 d . . . . .
ClA Cl 0.77533(2) 0.34662(2) 0.81845(2) 0.02317(9) Uani 1 1 d . . . . .
P1A P 0.61390(2) 0.17706(2) 0.82722(2) 0.01313(8) Uani 1 1 d . . . . .
P2A P 0.58749(2) 0.25253(2) 0.73929(2) 0.01751(9) Uani 1 1 d . . . . .
P3A P 0.53926(2) 0.35034(2) 0.76623(2) 0.01524(8) Uani 1 1 d . . . . .
N1A N 0.66498(7) 0.22314(7) 0.89958(7) 0.0138(2) Uani 1 1 d . . . . .
N2A N 0.60091(7) 0.39226(7) 0.83606(7) 0.0163(3) Uani 1 1 d . . . . .
N3A N 0.74016(7) 0.36046(7) 0.96049(7) 0.0161(3) Uani 1 1 d . . . . .
C1A C 0.79336(9) 0.38356(9) 1.02959(9) 0.0203(3) Uani 1 1 d . . . . .
C2A C 0.83021(11) 0.31336(11) 1.07253(10) 0.0321(4) Uani 1 1 d . . . . .
H2AA H 0.794271 0.283783 1.082156 0.048 Uiso 1 1 calc GR . . . .
H2AB H 0.868011 0.328429 1.116816 0.048 Uiso 1 1 calc GR . . . .
H2AC H 0.851389 0.283986 1.045471 0.048 Uiso 1 1 calc GR . . . .
C3A C 0.85040(10) 0.43321(11) 1.01689(10) 0.0290(4) Uani 1 1 d . . . . .
H3AA H 0.872201 0.406120 0.988964 0.044 Uiso 1 1 calc GR . . . .
H3AB H 0.887749 0.446861 1.061957 0.044 Uiso 1 1 calc GR . . . .
H3AC H 0.827118 0.477865 0.991755 0.044 Uiso 1 1 calc GR . . . .
C4A C 0.75590(12) 0.42902(13) 1.07029(11) 0.0367(5) Uani 1 1 d . . . . .
H4AA H 0.791880 0.444828 1.115368 0.055 Uiso 1 1 calc GR . . . .
H4AB H 0.719686 0.398329 1.078285 0.055 Uiso 1 1 calc GR . . . .
H4AC H 0.732631 0.472430 1.042752 0.055 Uiso 1 1 calc GR . . . .
C5A C 0.68201(8) 0.18997(8) 0.96856(8) 0.0138(3) Uani 1 1 d . . . . .
C6A C 0.73544(9) 0.13445(9) 0.99485(8) 0.0182(3) Uani 1 1 d . . . . .
H6A H 0.761451 0.118646 0.967511 0.022 Uiso 1 1 calc R . . . .
C7A C 0.75031(9) 0.10235(9) 1.06162(9) 0.0222(3) Uani 1 1 d . . . . .
H7A H 0.786155 0.065359 1.078697 0.027 Uiso 1 1 calc R . . . .
C8A C 0.71180(10) 0.12545(10) 1.10262(9) 0.0256(4) Uani 1 1 d . . . . .
H8A H 0.721207 0.103540 1.146950 0.031 Uiso 1 1 calc R . . . .
C9A C 0.65914(10) 0.18136(11) 1.07738(9) 0.0256(4) Uani 1 1 d . . . . .
H9A H 0.633471 0.197199 1.105028 0.031 Uiso 1 1 calc R . . . .
C10A C 0.64455(9) 0.21387(9) 1.01087(9) 0.0188(3) Uani 1 1 d . . . . .
H10A H 0.609582 0.251788 0.994545 0.023 Uiso 1 1 calc R . . . .
C11A C 0.66736(9) 0.10322(9) 0.80506(8) 0.0163(3) Uani 1 1 d . . . . .
H11A H 0.676961 0.063865 0.841404 0.020 Uiso 1 1 calc R . . . .
C12A C 0.74197(9) 0.13327(10) 0.81050(9) 0.0213(3) Uani 1 1 d . . . . .
H12D H 0.734886 0.174479 0.777900 0.032 Uiso 1 1 calc GR . . . .
H12E H 0.768749 0.093939 0.798642 0.032 Uiso 1 1 calc GR . . . .
H12F H 0.769123 0.150246 0.858368 0.032 Uiso 1 1 calc GR . . . .
C13A C 0.62561(11) 0.06599(10) 0.73263(9) 0.0264(4) Uani 1 1 d . . . . .
H13D H 0.580800 0.044603 0.732394 0.040 Uiso 1 1 calc GR . . . .
H13E H 0.655338 0.027040 0.724628 0.040 Uiso 1 1 calc GR . . . .
H13F H 0.614509 0.103011 0.695462 0.040 Uiso 1 1 calc GR . . . .
C14A C 0.53879(8) 0.12703(9) 0.84300(9) 0.0180(3) Uani 1 1 d . . . . .
H14A H 0.526553 0.158122 0.876882 0.022 Uiso 1 1 calc R . . . .
C15A C 0.56146(9) 0.05007(9) 0.87892(9) 0.0223(3) Uani 1 1 d . . . . .
H15D H 0.568894 0.015562 0.845834 0.033 Uiso 1 1 calc GR . . . .
H15E H 0.523481 0.031318 0.893256 0.033 Uiso 1 1 calc GR . . . .
H15F H 0.606187 0.055169 0.920160 0.033 Uiso 1 1 calc GR . . . .
C16A C 0.46804(9) 0.12051(11) 0.77626(10) 0.0280(4) Uani 1 1 d . . . . .
H16D H 0.455543 0.168869 0.753762 0.042 Uiso 1 1 calc GR . . . .
H16E H 0.428969 0.103175 0.789685 0.042 Uiso 1 1 calc GR . . . .
H16F H 0.475272 0.085385 0.743523 0.042 Uiso 1 1 calc GR . . . .
C17A C 0.58323(8) 0.46039(9) 0.86407(9) 0.0207(3) Uani 1 1 d . . . . .
C18A C 0.58583(10) 0.46107(11) 0.93384(10) 0.0275(4) Uani 1 1 d . . . . .
H18A H 0.600289 0.418202 0.962093 0.033 Uiso 1 1 calc R . . . .
C19A C 0.56671(11) 0.52621(13) 0.96126(13) 0.0405(5) Uani 1 1 d . . . . .
H19A H 0.568566 0.526568 1.007848 0.049 Uiso 1 1 calc R . . . .
C20A C 0.54499(11) 0.59032(12) 0.91949(15) 0.0467(6) Uani 1 1 d . . . . .
H20A H 0.530828 0.633059 0.937463 0.056 Uiso 1 1 calc R . . . .
C21A C 0.54445(11) 0.59050(11) 0.85157(14) 0.0424(6) Uani 1 1 d . . . . .
H21A H 0.530636 0.633823 0.823884 0.051 Uiso 1 1 calc R . . . .
C22A C 0.56436(10) 0.52653(10) 0.82368(11) 0.0305(4) Uani 1 1 d . . . . .
H22A H 0.565130 0.527728 0.778057 0.037 Uiso 1 1 calc R . . . .
C23A C 0.51616(9) 0.40462(9) 0.68358(8) 0.0207(3) Uani 1 1 d . . . . .
H23A H 0.492269 0.451027 0.689555 0.025 Uiso 1 1 calc R . . . .
C24A C 0.58470(11) 0.42769(11) 0.67031(11) 0.0316(4) Uani 1 1 d . . . . .
H24D H 0.619445 0.450530 0.712662 0.047 Uiso 1 1 calc GR . . . .
H24E H 0.571348 0.463019 0.631569 0.047 Uiso 1 1 calc GR . . . .
H24F H 0.606296 0.383983 0.658371 0.047 Uiso 1 1 calc GR . . . .
C25A C 0.46096(11) 0.36286(11) 0.61882(9) 0.0310(4) Uani 1 1 d . . . . .
H25D H 0.483413 0.318161 0.609833 0.046 Uiso 1 1 calc GR . . . .
H25E H 0.446466 0.394970 0.577620 0.046 Uiso 1 1 calc GR . . . .
H25F H 0.418547 0.349383 0.628584 0.046 Uiso 1 1 calc GR . . . .
C26A C 0.45182(9) 0.33826(10) 0.77897(9) 0.0208(3) Uani 1 1 d . . . . .
H26A H 0.424322 0.298387 0.746291 0.025 Uiso 1 1 calc R . . . .
C27A C 0.46568(10) 0.31152(10) 0.85492(10) 0.0248(4) Uani 1 1 d . . . . .
H27D H 0.504046 0.274512 0.869195 0.037 Uiso 1 1 calc GR . . . .
H27E H 0.421582 0.289743 0.856092 0.037 Uiso 1 1 calc GR . . . .
H27F H 0.480084 0.353531 0.887091 0.037 Uiso 1 1 calc GR . . . .
C28A C 0.40246(10) 0.40849(11) 0.76180(10) 0.0279(4) Uani 1 1 d . . . . .
H28D H 0.427554 0.448755 0.793204 0.042 Uiso 1 1 calc GR . . . .
H28E H 0.357783 0.397181 0.768284 0.042 Uiso 1 1 calc GR . . . .
H28F H 0.391250 0.423339 0.713185 0.042 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Ti Cl 2.3357(5) . ?
Ti P3 3.0256(5) . ?
Ti N1 2.0372(13) . ?
Ti N2 2.0257(13) . ?
Ti N3 1.6912(13) . ?
P1 P2 2.1404(5) . ?
P1 N1 1.6422(13) . ?
P1 C11 1.8470(15) . ?
P1 C14 1.8510(16) . ?
P2 P3 2.1531(5) . ?
P3 N2 1.6409(13) . ?
P3 C23 1.8472(16) . ?
P3 C26 1.8366(17) . ?
N1 C5 1.4316(19) . ?
N2 C17 1.4307(18) . ?
N3 C1 1.449(2) . ?
C1 C2 1.525(3) . ?
C1 C3 1.529(3) . ?
C1 C4 1.516(3) . ?
C5 C6 1.392(2) . ?
C5 C10 1.387(2) . ?
C6 C7 1.393(3) . ?
C7 C8 1.373(3) . ?
C8 C9 1.376(3) . ?
C9 C10 1.392(3) . ?
C11 C12 1.528(2) . ?
C11 C13 1.532(2) . ?
C14 C15 1.540(2) . ?
C14 C16 1.537(2) . ?
C17 C18 1.393(2) . ?
C17 C22 1.401(2) . ?
C18 C19 1.393(2) . ?
C19 C20 1.387(2) . ?
C20 C21 1.386(2) . ?
C21 C22 1.387(2) . ?
C23 C24 1.534(3) . ?
C23 C25 1.535(2) . ?
C26 C27 1.527(2) . ?
C26 C28 1.532(2) . ?
TiA ClA 2.3575(5) . ?
TiA P3A 3.0308(5) . ?
TiA N1A 2.0470(13) . ?
TiA N2A 2.0391(13) . ?
TiA N3A 1.7007(13) . ?
P1A P2A 2.1293(6) . ?
P1A N1A 1.6453(13) . ?
P1A C11A 1.8427(16) . ?
P1A C14A 1.8563(16) . ?
P2A P3A 2.1494(6) . ?
P3A N2A 1.6496(13) . ?
P3A C23A 1.8325(16) . ?
P3A C26A 1.8502(17) . ?
N1A C5A 1.4331(19) . ?
N2A C17A 1.435(2) . ?
N3A C1A 1.452(2) . ?
C1A C2A 1.536(2) . ?
C1A C3A 1.526(2) . ?
C1A C4A 1.530(2) . ?
C5A C6A 1.393(2) . ?
C5A C10A 1.394(2) . ?
C6A C7A 1.392(2) . ?
C7A C8A 1.384(3) . ?
C8A C9A 1.386(3) . ?
C9A C10A 1.391(2) . ?
C11A C12A 1.529(2) . ?
C11A C13A 1.532(2) . ?
C14A C15A 1.534(2) . ?
C14A C16A 1.532(2) . ?
C17A C18A 1.394(3) . ?
C17A C22A 1.399(3) . ?
C18A C19A 1.397(3) . ?
C19A C20A 1.386(4) . ?
C20A C21A 1.371(4) . ?
C21A C22A 1.391(3) . ?
C23A C24A 1.531(2) . ?
C23A C25A 1.539(2) . ?
C26A C27A 1.532(2) . ?
C26A C28A 1.539(2) . ?

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
Cl Ti P3 106.556(17) . . ?
N1 Ti Cl 123.85(4) . . ?
N1 Ti P3 90.33(4) . . ?
N2 Ti Cl 112.84(4) . . ?
N2 Ti P3 30.47(4) . . ?
N2 Ti N1 108.19(5) . . ?
N3 Ti Cl 104.42(5) . . ?
N3 Ti P3 131.86(5) . . ?
N3 Ti N1 101.90(6) . . ?
N3 Ti N2 102.85(6) . . ?
N1 P1 P2 108.25(5) . . ?
N1 P1 C11 111.39(7) . . ?
N1 P1 C14 110.28(7) . . ?
C11 P1 P2 102.68(5) . . ?
C11 P1 C14 105.90(7) . . ?
C14 P1 P2 118.07(5) . . ?
P1 P2 P3 108.98(2) . . ?
P2 P3 Ti 71.424(16) . . ?
N2 P3 Ti 38.75(4) . . ?
N2 P3 P2 110.00(5) . . ?
N2 P3 C23 111.97(7) . . ?
N2 P3 C26 110.59(7) . . ?
C23 P3 Ti 122.24(6) . . ?
C23 P3 P2 98.90(5) . . ?
C26 P3 Ti 129.41(5) . . ?
C26 P3 P2 119.15(5) . . ?
C26 P3 C23 105.55(8) . . ?
P1 N1 Ti 111.54(7) . . ?
C5 N1 Ti 125.63(10) . . ?
C5 N1 P1 122.80(10) . . ?
P3 N2 Ti 110.78(6) . . ?
C17 N2 Ti 123.74(10) . . ?
C17 N2 P3 125.27(10) . . ?
C1 N3 Ti 174.81(12) . . ?
N3 C1 C2 108.30(14) . . ?
N3 C1 C3 108.99(14) . . ?
N3 C1 C4 109.36(15) . . ?
C2 C1 C3 109.10(17) . . ?
C4 C1 C2 111.3(2) . . ?
C4 C1 C3 109.79(18) . . ?
C6 C5 N1 121.59(15) . . ?
C10 C5 N1 119.65(14) . . ?
C10 C5 C6 118.70(15) . . ?
C5 C6 C7 120.16(18) . . ?
C8 C7 C6 120.64(18) . . ?
C7 C8 C9 119.60(17) . . ?
C8 C9 C10 120.35(19) . . ?
C5 C10 C9 120.56(18) . . ?
C12 C11 P1 112.48(11) . . ?
C12 C11 C13 110.54(14) . . ?
C13 C11 P1 112.37(11) . . ?
C15 C14 P1 113.63(11) . . ?
C16 C14 P1 113.15(11) . . ?
C16 C14 C15 110.65(13) . . ?
C18 C17 N2 123.16(14) . . ?
C18 C17 C22 118.40(14) . . ?
C22 C17 N2 118.31(14) . . ?
C17 C18 C19 120.43(15) . . ?
C20 C19 C18 120.75(16) . . ?
C21 C20 C19 119.11(15) . . ?
C20 C21 C22 120.49(15) . . ?
C21 C22 C17 120.80(15) . . ?
C24 C23 P3 110.68(12) . . ?
C24 C23 C25 110.48(15) . . ?
C25 C23 P3 112.86(12) . . ?
C27 C26 P3 112.21(11) . . ?
C27 C26 C28 111.38(14) . . ?
C28 C26 P3 111.89(12) . . ?
ClA TiA P3A 107.450(16) . . ?
N1A TiA ClA 122.79(4) . . ?
N1A TiA P3A 90.31(4) . . ?
N2A TiA ClA 113.46(4) . . ?
N2A TiA P3A 30.75(4) . . ?
N2A TiA N1A 108.87(5) . . ?
N3A TiA ClA 103.60(5) . . ?
N3A TiA P3A 134.58(5) . . ?
N3A TiA N1A 99.92(6) . . ?
N3A TiA N2A 105.73(6) . . ?
N1A P1A P2A 107.62(5) . . ?
N1A P1A C11A 111.02(7) . . ?
N1A P1A C14A 110.04(7) . . ?
C11A P1A P2A 103.02(5) . . ?
C11A P1A C14A 105.58(7) . . ?
C14A P1A P2A 119.27(5) . . ?
P1A P2A P3A 106.74(2) . . ?
P2A P3A TiA 70.374(16) . . ?
N2A P3A TiA 39.20(5) . . ?
N2A P3A P2A 109.29(5) . . ?
N2A P3A C23A 112.97(8) . . ?
N2A P3A C26A 110.74(7) . . ?
C23A P3A TiA 124.90(6) . . ?
C23A P3A P2A 100.01(6) . . ?
C23A P3A C26A 105.56(8) . . ?
C26A P3A TiA 127.36(6) . . ?
C26A P3A P2A 117.86(6) . . ?
P1A N1A TiA 112.06(7) . . ?
C5A N1A TiA 127.90(10) . . ?
C5A N1A P1A 119.98(10) . . ?
P3A N2A TiA 110.05(7) . . ?
C17A N2A TiA 129.04(10) . . ?
C17A N2A P3A 120.61(11) . . ?
C1A N3A TiA 168.28(12) . . ?
N3A C1A C2A 109.14(13) . . ?
N3A C1A C3A 108.00(14) . . ?
N3A C1A C4A 110.42(14) . . ?
C3A C1A C2A 110.19(15) . . ?
C3A C1A C4A 108.86(15) . . ?
C4A C1A C2A 110.20(16) . . ?
C6A C5A N1A 121.74(14) . . ?
C6A C5A C10A 118.81(14) . . ?
C10A C5A N1A 119.45(14) . . ?
C7A C6A C5A 120.68(15) . . ?
C8A C7A C6A 120.04(16) . . ?
C7A C8A C9A 119.77(16) . . ?
C8A C9A C10A 120.28(16) . . ?
C9A C10A C5A 120.40(15) . . ?
C12A C11A P1A 110.95(11) . . ?
C12A C11A C13A 111.77(14) . . ?
C13A C11A P1A 113.10(11) . . ?
C15A C14A P1A 113.68(11) . . ?
C16A C14A P1A 113.70(12) . . ?
C16A C14A C15A 110.70(14) . . ?
C18A C17A N2A 119.16(15) . . ?
C18A C17A C22A 118.95(17) . . ?
C22A C17A N2A 121.89(16) . . ?
C17A C18A C19A 119.9(2) . . ?
C20A C19A C18A 120.4(2) . . ?
C21A C20A C19A 119.77(19) . . ?
C20A C21A C22A 120.6(2) . . ?
C21A C22A C17A 120.2(2) . . ?
C24A C23A P3A 111.89(12) . . ?
C24A C23A C25A 111.37(15) . . ?
C25A C23A P3A 111.91(12) . . ?
C27A C26A P3A 110.92(11) . . ?
C27A C26A C28A 109.51(14) . . ?
C28A C26A P3A 114.63(12) . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT910_6b                  
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         17 Note  
RESPONSE: a set of poorly measured low-order reflections (too
intense or affected by the beamstop) have been omitted from the final
least-squares refinement
;
# end Validation Reply Form
####################################################################### 
# 
# 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_3b
_database_code_depnum_ccdc_archive 'CCDC 1985146'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne Franche Comte
France
;
_audit_update_record             
;
2020-02-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_audit_creation_date             2020-01-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H38 Cl2 N2 P3 Ti'
_chemical_formula_sum            'C24 H38 Cl2 N2 P3 Ti'
_chemical_formula_weight         566.27
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.1686(13)
_cell_length_b                   15.390(2)
_cell_length_c                   16.608(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.796(6)
_cell_angle_gamma                90
_cell_volume                     2813.1(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2721
_cell_measurement_temperature    100.
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.93
_shelx_estimated_absorpt_T_max   0.951
_shelx_estimated_absorpt_T_min   0.812
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0720 before and 0.0629 after correction. The Ratio of minimum to maximum transmission is 0.9026. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.075
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            50555
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.583
_diffrn_reflns_theta_min         3.132
_diffrn_ambient_temperature      100.
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Mo'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-90C'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5542
_reflns_number_total             6479
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         6479
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0295
_refine_ls_restrained_S_all      1.086
_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)+(0.0187P)²+3.0018P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0685
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C 0.32328(17) 0.11757(11) 0.60948(10) 0.0189(4) Uani 1 1 d . . . . .
C2 C 0.4071(2) 0.06023(12) 0.58606(11) 0.0317(5) Uani 1 1 d . . . A 1
H2 H 0.490390 0.075946 0.592176 0.038 Uiso 1 1 calc R . . A 1
C3 C 0.3683(3) -0.02051(14) 0.55353(13) 0.0546(8) Uani 1 1 d . . . A 1
H3 H 0.425625 -0.059947 0.537913 0.066 Uiso 1 1 calc R . . A 1
C4 C 0.2476(4) -0.04356(16) 0.54384(14) 0.0684(11) Uani 1 1 d . . . A 1
H4 H 0.221692 -0.098430 0.521111 0.082 Uiso 1 1 calc R . . A 1
C5 C 0.1653(3) 0.01284(19) 0.56707(13) 0.0588(9) Uani 1 1 d . . . A 1
H5 H 0.082275 -0.003600 0.561217 0.071 Uiso 1 1 calc R . . A 1
C6 C 0.2015(2) 0.09374(15) 0.59906(11) 0.0343(5) Uani 1 1 d . . . A 1
H6 H 0.143110 0.132876 0.613855 0.041 Uiso 1 1 calc R . . A 1
C7 C 0.21713(15) 0.22726(11) 0.76855(10) 0.0166(3) Uani 1 1 d . . . . .
H7 H 0.183734 0.167213 0.758433 0.020 Uiso 1 1 calc R . . . .
C8 C 0.12781(16) 0.29000(13) 0.71912(12) 0.0264(4) Uani 1 1 d . . . . .
H8A H 0.045323 0.277070 0.728407 0.040 Uiso 1 1 calc GR . . . .
H8B H 0.131515 0.283519 0.660895 0.040 Uiso 1 1 calc GR . . . .
H8C H 0.149144 0.349749 0.736273 0.040 Uiso 1 1 calc GR . . . .
C9 C 0.22835(17) 0.24572(13) 0.85999(11) 0.0238(4) Uani 1 1 d . . . . .
H9A H 0.273932 0.198674 0.891066 0.036 Uiso 1 1 calc GR . . . .
H9B H 0.147079 0.249458 0.874553 0.036 Uiso 1 1 calc GR . . . .
H9C H 0.271216 0.300851 0.872943 0.036 Uiso 1 1 calc GR . . . .
C10 C 0.46288(16) 0.15640(11) 0.80683(10) 0.0176(3) Uani 1 1 d . . . . .
H10 H 0.478725 0.184888 0.861734 0.021 Uiso 1 1 calc R . . . .
C11 C 0.58576(16) 0.14148(12) 0.77997(12) 0.0234(4) Uani 1 1 d . . . . .
H11A H 0.575521 0.101183 0.733611 0.035 Uiso 1 1 calc GR . . . .
H11B H 0.643016 0.116724 0.825457 0.035 Uiso 1 1 calc GR . . . .
H11C H 0.617407 0.196967 0.763638 0.035 Uiso 1 1 calc GR . . . .
C12 C 0.40105(18) 0.06845(12) 0.81649(12) 0.0254(4) Uani 1 1 d . . . . .
H12A H 0.326993 0.077916 0.839588 0.038 Uiso 1 1 calc GR . . . .
H12B H 0.456729 0.030977 0.853109 0.038 Uiso 1 1 calc GR . . . .
H12C H 0.380085 0.040494 0.762932 0.038 Uiso 1 1 calc GR . . . .
C13 C 0.69951(14) 0.33287(11) 0.59728(9) 0.0141(3) Uani 1 1 d . . . . .
C14 C 0.74984(16) 0.40453(12) 0.56430(10) 0.0187(3) Uani 1 1 d . . . . .
H14 H 0.708043 0.458542 0.559892 0.022 Uiso 1 1 calc R . . . .
C15 C 0.86107(16) 0.39745(13) 0.53777(10) 0.0229(4) Uani 1 1 d . . . . .
H15 H 0.895340 0.446850 0.515980 0.027 Uiso 1 1 calc R . . . .
C16 C 0.92206(16) 0.31886(14) 0.54296(11) 0.0242(4) Uani 1 1 d . . . . .
H16 H 0.998540 0.314325 0.525522 0.029 Uiso 1 1 calc R . . . .
C17 C 0.87084(16) 0.24697(13) 0.57371(10) 0.0219(4) Uani 1 1 d . . . . .
H17 H 0.911734 0.192651 0.576272 0.026 Uiso 1 1 calc R . . . .
C18 C 0.75995(15) 0.25333(11) 0.60095(10) 0.0168(3) Uani 1 1 d . . . . .
H18 H 0.725542 0.203557 0.622010 0.020 Uiso 1 1 calc R . . . .
C19 C 0.58296(16) 0.50862(10) 0.70039(11) 0.0175(3) Uani 1 1 d . . . . .
H19 H 0.664898 0.523889 0.687932 0.021 Uiso 1 1 calc R . . . .
C20 C 0.56744(19) 0.55920(12) 0.77762(12) 0.0261(4) Uani 1 1 d . . . . .
H20A H 0.487609 0.546264 0.791720 0.039 Uiso 1 1 calc GR . . . .
H20B H 0.573610 0.621650 0.767541 0.039 Uiso 1 1 calc GR . . . .
H20C H 0.631179 0.541971 0.822893 0.039 Uiso 1 1 calc GR . . . .
C21 C 0.48938(17) 0.53804(12) 0.62717(12) 0.0233(4) Uani 1 1 d . . . . .
H21A H 0.499483 0.503972 0.578926 0.035 Uiso 1 1 calc GR . . . .
H21B H 0.501457 0.599790 0.616566 0.035 Uiso 1 1 calc GR . . . .
H21C H 0.407311 0.529186 0.639148 0.035 Uiso 1 1 calc GR . . . .
C22 C 0.70994(15) 0.36063(11) 0.79399(10) 0.0169(3) Uani 1 1 d . . . . .
H22 H 0.732839 0.299708 0.782157 0.020 Uiso 1 1 calc R . . . .
C23 C 0.82370(16) 0.41621(13) 0.79260(12) 0.0246(4) Uani 1 1 d . . . . .
H23A H 0.842837 0.416891 0.737166 0.037 Uiso 1 1 calc GR . . . .
H23B H 0.892287 0.391542 0.830340 0.037 Uiso 1 1 calc GR . . . .
H23C H 0.808607 0.475697 0.809412 0.037 Uiso 1 1 calc GR . . . .
C24 C 0.67449(17) 0.35886(13) 0.87921(11) 0.0245(4) Uani 1 1 d . . . . .
H24A H 0.652097 0.417554 0.894078 0.037 Uiso 1 1 calc GR . . . .
H24B H 0.743482 0.338217 0.919125 0.037 Uiso 1 1 calc GR . . . .
H24C H 0.605229 0.319690 0.878883 0.037 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.24293(4) 0.37957(3) 0.51509(3) 0.02193(10) Uani 1 1 d . . . . .
Cl2 Cl 0.47043(4) 0.23724(3) 0.46741(2) 0.01954(9) Uani 1 1 d . . . . .
N1 N 0.36167(12) 0.20152(9) 0.64082(8) 0.0127(3) Uani 1 1 d . . . . .
N2 N 0.58681(12) 0.33958(9) 0.62760(8) 0.0130(3) Uani 1 1 d . . . . .
P1 P 0.36633(4) 0.22998(3) 0.73645(2) 0.01150(9) Uani 1 1 d . . . . .
P2 P 0.39918(4) 0.36845(3) 0.73579(3) 0.01293(9) Uani 1 1 d . . . . .
P3 P 0.58046(4) 0.38957(3) 0.71380(2) 0.01162(9) Uani 1 1 d . . . . .
Ti Ti 0.41160(3) 0.30510(2) 0.58047(2) 0.01134(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
C1 C2 1.389(3) . ?
C1 C6 1.391(3) . ?
C1 N1 1.431(2) . ?
C2 C3 1.394(3) . ?
C3 C4 1.376(5) . ?
C4 C5 1.367(5) . ?
C5 C6 1.387(3) . ?
C7 C8 1.524(2) . ?
C7 C9 1.529(2) . ?
C7 P1 1.8343(16) . ?
C10 C11 1.531(2) . ?
C10 C12 1.540(2) . ?
C10 P1 1.8392(17) . ?
C13 C14 1.392(2) . ?
C13 C18 1.394(2) . ?
C13 N2 1.437(2) . ?
C14 C15 1.391(2) . ?
C15 C16 1.384(3) . ?
C16 C17 1.383(3) . ?
C17 C18 1.392(2) . ?
C19 C20 1.535(2) . ?
C19 C21 1.531(2) . ?
C19 P3 1.8465(17) . ?
C22 C23 1.535(2) . ?
C22 C24 1.534(2) . ?
C22 P3 1.8461(17) . ?
Cl1 Ti 2.3119(5) . ?
Cl2 Ti 2.3384(5) . ?
N1 P1 1.6400(14) . ?
N1 Ti 2.0116(13) . ?
N2 P3 1.6374(14) . ?
N2 Ti 2.0501(14) . ?
P1 P2 2.1626(7) . ?
P1 Ti 2.9579(6) . ?
P2 P3 2.1424(6) . ?
P2 Ti 2.7832(6) . ?
P3 Ti 2.9545(6) . ?

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
C2 C1 C6 119.27(18) . . ?
C2 C1 N1 120.06(17) . . ?
C6 C1 N1 120.62(17) . . ?
C1 C2 C3 119.7(2) . . ?
C4 C3 C2 120.6(3) . . ?
C5 C4 C3 119.7(2) . . ?
C4 C5 C6 120.8(3) . . ?
C5 C6 C1 120.0(2) . . ?
C8 C7 C9 110.66(15) . . ?
C8 C7 P1 111.89(11) . . ?
C9 C7 P1 111.06(12) . . ?
C11 C10 C12 109.79(14) . . ?
C11 C10 P1 111.40(12) . . ?
C12 C10 P1 112.49(12) . . ?
C14 C13 C18 119.21(15) . . ?
C14 C13 N2 121.16(15) . . ?
C18 C13 N2 119.63(14) . . ?
C15 C14 C13 120.32(17) . . ?
C16 C15 C14 120.36(17) . . ?
C17 C16 C15 119.49(16) . . ?
C16 C17 C18 120.70(17) . . ?
C17 C18 C13 119.89(16) . . ?
C20 C19 P3 113.34(12) . . ?
C21 C19 C20 110.79(15) . . ?
C21 C19 P3 111.53(12) . . ?
C23 C22 P3 113.80(12) . . ?
C24 C22 C23 111.60(15) . . ?
C24 C22 P3 112.12(12) . . ?
C1 N1 P1 123.47(11) . . ?
C1 N1 Ti 128.72(10) . . ?
P1 N1 Ti 107.77(7) . . ?
C13 N2 P3 120.74(11) . . ?
C13 N2 Ti 133.15(10) . . ?
P3 N2 Ti 105.95(7) . . ?
C7 P1 C10 105.35(8) . . ?
C7 P1 P2 100.79(6) . . ?
C7 P1 Ti 124.23(6) . . ?
C10 P1 P2 121.89(6) . . ?
C10 P1 Ti 128.92(6) . . ?
N1 P1 C7 113.24(7) . . ?
N1 P1 C10 111.70(7) . . ?
N1 P1 P2 103.63(5) . . ?
N1 P1 Ti 40.36(5) . . ?
P2 P1 Ti 63.642(16) . . ?
P1 P2 Ti 72.231(17) . . ?
P3 P2 P1 108.45(2) . . ?
P3 P2 Ti 72.395(17) . . ?
C19 P3 P2 101.84(6) . . ?
C19 P3 Ti 111.53(6) . . ?
C22 P3 C19 107.48(8) . . ?
C22 P3 P2 119.17(6) . . ?
C22 P3 Ti 139.14(6) . . ?
N2 P3 C19 110.91(7) . . ?
N2 P3 C22 111.86(8) . . ?
N2 P3 P2 105.11(5) . . ?
N2 P3 Ti 41.85(5) . . ?
P2 P3 Ti 63.882(18) . . ?
Cl1 Ti Cl2 99.33(2) . . ?
Cl1 Ti P1 110.982(18) . . ?
Cl1 Ti P2 95.540(19) . . ?
Cl1 Ti P3 119.938(19) . . ?
Cl2 Ti P1 129.942(19) . . ?
Cl2 Ti P2 164.981(19) . . ?
Cl2 Ti P3 124.582(18) . . ?
N1 Ti Cl1 110.74(4) . . ?
N1 Ti Cl2 100.71(4) . . ?
N1 Ti N2 110.02(6) . . ?
N1 Ti P1 31.87(4) . . ?
N1 Ti P2 75.76(4) . . ?
N1 Ti P3 99.84(4) . . ?
N2 Ti Cl1 134.39(4) . . ?
N2 Ti Cl2 92.39(4) . . ?
N2 Ti P1 93.50(4) . . ?
N2 Ti P2 75.54(4) . . ?
N2 Ti P3 32.20(4) . . ?
P2 Ti P1 44.127(15) . . ?
P2 Ti P3 43.723(13) . . ?
P3 Ti P1 72.419(15) . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT213_3b                  
;
PROBLEM: Atom C4 has ADP max/min Ratio ..... 4.5 prolat
RESPONSE: C1-C6 atoms belong to a slightly disordered phenyl group.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_6a-Py
_database_code_depnum_ccdc_archive 'CCDC 1985137'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne Franche Comte
France
;
_audit_update_record             
;
2020-02-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_audit_creation_date             2020-02-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45 H44 Cl N4 P3 Ti'
_chemical_formula_sum            'C45 H44 Cl N4 P3 Ti'
_chemical_formula_weight         817.10
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.209(3)
_cell_length_b                   12.264(3)
_cell_length_c                   15.876(4)
_cell_angle_alpha                97.041(6)
_cell_angle_beta                 99.249(6)
_cell_angle_gamma                98.343(6)
_cell_volume                     2295.2(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2688
_cell_measurement_temperature    115
_cell_measurement_theta_max      24.799
_cell_measurement_theta_min      2.34
_shelx_estimated_absorpt_T_max   0.990
_shelx_estimated_absorpt_T_min   0.910
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_T_max  0.6461
_exptl_absorpt_correction_T_min  0.4785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0896 before and 0.0711 after correction. The Ratio of minimum to maximum transmission is 0.7406. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1718
_diffrn_reflns_av_unetI/netI     0.2524
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25340
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.055
_diffrn_reflns_theta_max         25.055
_diffrn_reflns_theta_min         2.909
_diffrn_ambient_temperature      115.0
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3472
_reflns_number_total             8072
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         8072
_refine_ls_number_restraints     421
_refine_ls_R_factor_all          0.1959
_refine_ls_R_factor_gt           0.0693
_refine_ls_restrained_S_all      0.898
_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)+(0.0751P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1892
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C45(H45)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.0539(5) 0.3367(6) 0.8771(4) 0.0361(17) Uani 1 1 d . U . . .
C2 C 0.0085(7) 0.2130(6) 0.8484(5) 0.068(3) Uani 1 1 d . U . . .
H2A H -0.035124 0.201850 0.789593 0.102 Uiso 1 1 calc GR . . . .
H2B H -0.040141 0.186125 0.887568 0.102 Uiso 1 1 calc GR . . . .
H2C H 0.071383 0.171563 0.849441 0.102 Uiso 1 1 calc GR . . . .
C3 C 0.1286(6) 0.3572(7) 0.9674(4) 0.058(2) Uani 1 1 d . U . . .
H3A H 0.193291 0.318566 0.965706 0.087 Uiso 1 1 calc GR . . . .
H3B H 0.084756 0.328611 1.008940 0.087 Uiso 1 1 calc GR . . . .
H3C H 0.155291 0.437298 0.984903 0.087 Uiso 1 1 calc GR . . . .
C4 C -0.0459(6) 0.3987(7) 0.8780(5) 0.053(2) Uani 1 1 d . U . . .
H4A H -0.018307 0.478003 0.899118 0.080 Uiso 1 1 calc GR . . . .
H4B H -0.094168 0.367805 0.915982 0.080 Uiso 1 1 calc GR . . . .
H4C H -0.089381 0.390093 0.819302 0.080 Uiso 1 1 calc GR . . . .
C5 C 0.2628(5) 0.1892(5) 0.7482(4) 0.0265(14) Uani 1 1 d . U . . .
C6 C 0.2022(6) 0.0857(6) 0.7152(4) 0.0400(18) Uani 1 1 d . U . . .
H6 H 0.159261 0.072700 0.658382 0.048 Uiso 1 1 calc R . . . .
C7 C 0.2032(7) 0.0001(6) 0.7643(5) 0.058(2) Uani 1 1 d . U . . .
H7 H 0.160913 -0.071514 0.740828 0.069 Uiso 1 1 calc R . . . .
C8 C 0.2642(6) 0.0172(6) 0.8461(5) 0.0483(19) Uani 1 1 d . U . . .
H8 H 0.264122 -0.041877 0.879615 0.058 Uiso 1 1 calc R . . . .
C9 C 0.3254(6) 0.1198(7) 0.8794(5) 0.0466(19) Uani 1 1 d . U . . .
H9 H 0.368104 0.132192 0.936292 0.056 Uiso 1 1 calc R . . . .
C10 C 0.3255(5) 0.2054(6) 0.8311(4) 0.0364(17) Uani 1 1 d . U . . .
H10 H 0.368889 0.276490 0.854771 0.044 Uiso 1 1 calc R . . . .
C11 C 0.2729(5) 0.1879(5) 0.5273(4) 0.0268(14) Uani 1 1 d . U . . .
C12 C 0.3430(6) 0.1455(5) 0.4747(4) 0.0364(17) Uani 1 1 d . U . . .
H12 H 0.420959 0.175698 0.485702 0.044 Uiso 1 1 calc R . . . .
C13 C 0.3004(6) 0.0605(6) 0.4069(5) 0.0456(19) Uani 1 1 d . U . . .
H13 H 0.349322 0.032870 0.371812 0.055 Uiso 1 1 calc R . . . .
C14 C 0.1872(6) 0.0152(6) 0.3896(4) 0.0436(18) Uani 1 1 d . U . . .
H14 H 0.158131 -0.045186 0.344340 0.052 Uiso 1 1 calc R . . . .
C15 C 0.1174(6) 0.0599(6) 0.4399(4) 0.0396(17) Uani 1 1 d . U . . .
H15 H 0.038933 0.031575 0.427310 0.048 Uiso 1 1 calc R . . . .
C16 C 0.1587(5) 0.1441(5) 0.5075(4) 0.0318(16) Uani 1 1 d . U . . .
H16 H 0.108760 0.172826 0.541153 0.038 Uiso 1 1 calc R . . . .
C17 C 0.4743(5) 0.2878(5) 0.6419(4) 0.0276(15) Uani 1 1 d . U . . .
C18 C 0.5483(5) 0.3498(5) 0.5997(4) 0.0319(16) Uani 1 1 d . U . . .
H18 H 0.521314 0.398948 0.562597 0.038 Uiso 1 1 calc R . . . .
C19 C 0.6616(5) 0.3391(6) 0.6122(4) 0.0372(17) Uani 1 1 d . U . . .
H19 H 0.711786 0.380768 0.583432 0.045 Uiso 1 1 calc R . . . .
C20 C 0.7005(6) 0.2687(6) 0.6660(5) 0.0396(18) Uani 1 1 d . U . . .
H20 H 0.777765 0.261329 0.673879 0.047 Uiso 1 1 calc R . . . .
C21 C 0.6300(6) 0.2090(6) 0.7083(5) 0.0416(18) Uani 1 1 d . U . . .
H21 H 0.658300 0.161657 0.746571 0.050 Uiso 1 1 calc R . . . .
C22 C 0.5159(5) 0.2177(6) 0.6954(4) 0.0374(17) Uani 1 1 d . U . . .
H22 H 0.466518 0.174603 0.723983 0.045 Uiso 1 1 calc R . . . .
C23 C 0.5136(5) 0.5763(5) 0.7103(4) 0.0229(14) Uani 1 1 d . U . . .
C24 C 0.5618(5) 0.5286(5) 0.7800(4) 0.0282(15) Uani 1 1 d . U . . .
H24 H 0.515463 0.493451 0.814918 0.034 Uiso 1 1 calc R . . . .
C25 C 0.6776(5) 0.5330(6) 0.7977(4) 0.0355(17) Uani 1 1 d . U . . .
H25 H 0.710194 0.502022 0.845829 0.043 Uiso 1 1 calc R . . . .
C26 C 0.7457(5) 0.5813(6) 0.7469(4) 0.0359(17) Uani 1 1 d . U . . .
H26 H 0.824826 0.583749 0.759724 0.043 Uiso 1 1 calc R . . . .
C27 C 0.6984(5) 0.6264(6) 0.6770(4) 0.0350(17) Uani 1 1 d . U . . .
H27 H 0.745372 0.660426 0.641981 0.042 Uiso 1 1 calc R . . . .
C28 C 0.5843(5) 0.6226(5) 0.6578(4) 0.0280(15) Uani 1 1 d . U . . .
H28 H 0.552652 0.651546 0.608296 0.034 Uiso 1 1 calc R . . . .
C29 C 0.3449(5) 0.6970(5) 0.6445(4) 0.0211(13) Uani 1 1 d . U . . .
C30 C 0.4206(5) 0.7944(5) 0.6790(4) 0.0326(16) Uani 1 1 d . U . . .
H30 H 0.483222 0.792524 0.722530 0.039 Uiso 1 1 calc R . . . .
C31 C 0.4051(6) 0.8931(6) 0.6505(5) 0.0408(18) Uani 1 1 d . U . . .
H31 H 0.458627 0.958623 0.673023 0.049 Uiso 1 1 calc R . . . .
C32 C 0.3119(6) 0.8981(6) 0.5889(4) 0.0389(17) Uani 1 1 d . U . . .
H32 H 0.300741 0.966800 0.569810 0.047 Uiso 1 1 calc R . . . .
C33 C 0.2356(5) 0.8016(5) 0.5559(4) 0.0322(16) Uani 1 1 d . U . . .
H33 H 0.171921 0.803843 0.513405 0.039 Uiso 1 1 calc R . . . .
C34 C 0.2514(5) 0.7027(5) 0.5842(4) 0.0282(15) Uani 1 1 d . U . . .
H34 H 0.197493 0.637330 0.562084 0.034 Uiso 1 1 calc R . . . .
C35 C 0.3385(5) 0.5953(5) 0.8471(4) 0.0250(14) Uani 1 1 d . U . . .
C36 C 0.3505(5) 0.7096(6) 0.8658(4) 0.0337(16) Uani 1 1 d . U . . .
H36 H 0.336791 0.750977 0.819528 0.040 Uiso 1 1 calc R . . . .
C37 C 0.3815(6) 0.7669(6) 0.9490(4) 0.0478(19) Uani 1 1 d . U . . .
H37 H 0.391099 0.845990 0.959081 0.057 Uiso 1 1 calc R . . . .
C38 C 0.3984(6) 0.7075(7) 1.0173(5) 0.0446(19) Uani 1 1 d . U . . .
H38 H 0.418389 0.745230 1.074919 0.054 Uiso 1 1 calc R . . . .
C39 C 0.3860(6) 0.5941(7) 1.0009(5) 0.0460(19) Uani 1 1 d . U . . .
H39 H 0.398405 0.553470 1.047771 0.055 Uiso 1 1 calc R . . . .
C40 C 0.3557(5) 0.5364(5) 0.9171(4) 0.0311(16) Uani 1 1 d . U . . .
H40 H 0.346640 0.457351 0.907390 0.037 Uiso 1 1 calc R . . . .
C41 C 0.0140(5) 0.5717(6) 0.6308(5) 0.0367(17) Uani 1 1 d . U . . .
H41 H 0.004216 0.517176 0.580989 0.044 Uiso 1 1 calc R . . . .
C42 C -0.0279(6) 0.6673(7) 0.6221(5) 0.0473(19) Uani 1 1 d . U . . .
H42 H -0.064307 0.679302 0.567269 0.057 Uiso 1 1 calc R . . . .
C43 C -0.0173(5) 0.7462(7) 0.6931(6) 0.0489(19) Uani 1 1 d . U . . .
H43 H -0.046277 0.813444 0.688406 0.059 Uiso 1 1 calc R . . . .
C44 C 0.0370(5) 0.7261(6) 0.7726(5) 0.0449(18) Uani 1 1 d . U . . .
H44 H 0.045186 0.778651 0.823339 0.054 Uiso 1 1 calc R . . . .
C45 C 0.0782(5) 0.6283(5) 0.7752(5) 0.0338(16) Uani 1 1 d . U . . .
H45 H 0.115799 0.615220 0.829327 0.041 Uiso 1 1 calc R . . . .
Cl Cl -0.00224(13) 0.30218(15) 0.62100(11) 0.0416(5) Uani 1 1 d . U . . .
N1 N 0.2609(4) 0.2807(4) 0.6998(3) 0.0222(12) Uani 1 1 d . U . . .
N2 N 0.3036(4) 0.5336(4) 0.7625(3) 0.0200(11) Uani 1 1 d . U . . .
N3 N 0.1192(4) 0.3764(4) 0.8141(3) 0.0240(12) Uani 1 1 d . U . . .
N4 N 0.0690(4) 0.5495(4) 0.7064(4) 0.0302(13) Uani 1 1 d . U . . .
P1 P 0.32497(13) 0.29582(13) 0.61949(10) 0.0230(4) Uani 1 1 d . U . . .
P2 P 0.28589(13) 0.44384(14) 0.57173(11) 0.0239(4) Uani 1 1 d . U . . .
P3 P 0.36323(13) 0.56464(13) 0.68240(10) 0.0211(4) Uani 1 1 d . U . . .
Ti Ti 0.16104(9) 0.40456(10) 0.72184(7) 0.0251(3) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
C1 C2 1.524(9) . ?
C1 C3 1.540(9) . ?
C1 C4 1.529(9) . ?
C1 N3 1.461(7) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.368(8) . ?
C5 C10 1.388(8) . ?
C5 N1 1.436(7) . ?
C6 H6 0.9500 . ?
C6 C7 1.383(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.365(10) . ?
C8 H8 0.9500 . ?
C8 C9 1.363(10) . ?
C9 H9 0.9500 . ?
C9 C10 1.374(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.397(8) . ?
C11 C16 1.390(8) . ?
C11 P1 1.811(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.379(9) . ?
C13 H13 0.9500 . ?
C13 C14 1.383(9) . ?
C14 H14 0.9500 . ?
C14 C15 1.383(9) . ?
C15 H15 0.9500 . ?
C15 C16 1.369(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.402(8) . ?
C17 C22 1.373(8) . ?
C17 P1 1.820(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.392(8) . ?
C19 H19 0.9500 . ?
C19 C20 1.367(9) . ?
C20 H20 0.9500 . ?
C20 C21 1.361(9) . ?
C21 H21 0.9500 . ?
C21 C22 1.396(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.400(8) . ?
C23 C28 1.403(8) . ?
C23 P3 1.798(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.388(8) . ?
C25 H25 0.9500 . ?
C25 C26 1.372(8) . ?
C26 H26 0.9500 . ?
C26 C27 1.382(8) . ?
C27 H27 0.9500 . ?
C27 C28 1.370(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.392(8) . ?
C29 C34 1.383(8) . ?
C29 P3 1.829(6) . ?
C30 H30 0.9500 . ?
C30 C31 1.370(9) . ?
C31 H31 0.9500 . ?
C31 C32 1.390(9) . ?
C32 H32 0.9500 . ?
C32 C33 1.383(9) . ?
C33 H33 0.9500 . ?
C33 C34 1.373(8) . ?
C34 H34 0.9500 . ?
C35 C36 1.378(8) . ?
C35 C40 1.402(8) . ?
C35 N2 1.425(7) . ?
C36 H36 0.9500 . ?
C36 C37 1.384(9) . ?
C37 H37 0.9500 . ?
C37 C38 1.383(9) . ?
C38 H38 0.9500 . ?
C38 C39 1.365(10) . ?
C39 H39 0.9500 . ?
C39 C40 1.394(9) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C41 C42 1.360(9) . ?
C41 N4 1.357(8) . ?
C42 H42 0.9500 . ?
C42 C43 1.368(10) . ?
C43 H43 0.9500 . ?
C43 C44 1.396(10) . ?
C44 H44 0.9500 . ?
C44 C45 1.368(9) . ?
C45 H45 0.9500 . ?
C45 N4 1.345(8) . ?
Cl Ti 2.422(2) . ?
N1 P1 1.615(5) . ?
N1 Ti 2.111(5) . ?
N2 P3 1.621(5) . ?
N2 Ti 2.130(5) . ?
N3 Ti 1.686(5) . ?
N4 Ti 2.254(5) . ?
P1 P2 2.138(2) . ?
P2 P3 2.144(2) . ?

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
C2 C1 C3 111.1(7) . . ?
C2 C1 C4 108.3(6) . . ?
C4 C1 C3 110.2(6) . . ?
N3 C1 C2 108.3(5) . . ?
N3 C1 C3 110.0(5) . . ?
N3 C1 C4 108.8(5) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C10 118.5(6) . . ?
C6 C5 N1 121.6(6) . . ?
C10 C5 N1 119.9(6) . . ?
C5 C6 H6 119.9 . . ?
C5 C6 C7 120.2(7) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.7(7) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 120.3 . . ?
C9 C8 C7 119.5(7) . . ?
C9 C8 H8 120.3 . . ?
C8 C9 H9 119.8 . . ?
C8 C9 C10 120.3(7) . . ?
C10 C9 H9 119.8 . . ?
C5 C10 H10 119.7 . . ?
C9 C10 C5 120.7(7) . . ?
C9 C10 H10 119.7 . . ?
C12 C11 P1 122.8(5) . . ?
C16 C11 C12 117.9(6) . . ?
C16 C11 P1 119.4(5) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.9(6) . . ?
C13 C12 H12 119.6 . . ?
C12 C13 H13 119.7 . . ?
C12 C13 C14 120.7(7) . . ?
C14 C13 H13 119.7 . . ?
C13 C14 H14 120.8 . . ?
C13 C14 C15 118.3(7) . . ?
C15 C14 H14 120.8 . . ?
C14 C15 H15 119.2 . . ?
C16 C15 C14 121.5(7) . . ?
C16 C15 H15 119.2 . . ?
C11 C16 H16 119.7 . . ?
C15 C16 C11 120.7(6) . . ?
C15 C16 H16 119.7 . . ?
C18 C17 P1 119.3(5) . . ?
C22 C17 C18 118.7(6) . . ?
C22 C17 P1 121.8(5) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 119.9(6) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 120.0(6) . . ?
C20 C19 H19 120.0 . . ?
C19 C20 H20 119.6 . . ?
C21 C20 C19 120.8(6) . . ?
C21 C20 H20 119.6 . . ?
C20 C21 H21 120.1 . . ?
C20 C21 C22 119.8(7) . . ?
C22 C21 H21 120.1 . . ?
C17 C22 C21 120.8(6) . . ?
C17 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C24 C23 C28 118.3(5) . . ?
C24 C23 P3 120.4(4) . . ?
C28 C23 P3 120.9(5) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 C23 119.7(6) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 H25 119.5 . . ?
C26 C25 C24 121.0(6) . . ?
C26 C25 H25 119.5 . . ?
C25 C26 H26 120.2 . . ?
C25 C26 C27 119.5(6) . . ?
C27 C26 H26 120.2 . . ?
C26 C27 H27 119.7 . . ?
C28 C27 C26 120.6(6) . . ?
C28 C27 H27 119.7 . . ?
C23 C28 H28 119.6 . . ?
C27 C28 C23 120.7(6) . . ?
C27 C28 H28 119.6 . . ?
C30 C29 P3 121.0(5) . . ?
C34 C29 C30 118.8(6) . . ?
C34 C29 P3 120.0(5) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 C29 120.4(6) . . ?
C31 C30 H30 119.8 . . ?
C30 C31 H31 119.7 . . ?
C30 C31 C32 120.6(7) . . ?
C32 C31 H31 119.7 . . ?
C31 C32 H32 120.5 . . ?
C33 C32 C31 119.0(7) . . ?
C33 C32 H32 120.5 . . ?
C32 C33 H33 119.8 . . ?
C34 C33 C32 120.4(6) . . ?
C34 C33 H33 119.8 . . ?
C29 C34 H34 119.6 . . ?
C33 C34 C29 120.8(6) . . ?
C33 C34 H34 119.6 . . ?
C36 C35 C40 117.0(6) . . ?
C36 C35 N2 124.4(6) . . ?
C40 C35 N2 118.4(6) . . ?
C35 C36 H36 118.5 . . ?
C35 C36 C37 123.1(7) . . ?
C37 C36 H36 118.5 . . ?
C36 C37 H37 120.5 . . ?
C38 C37 C36 119.1(7) . . ?
C38 C37 H37 120.5 . . ?
C37 C38 H38 120.4 . . ?
C39 C38 C37 119.2(7) . . ?
C39 C38 H38 120.4 . . ?
C38 C39 H39 119.2 . . ?
C38 C39 C40 121.7(7) . . ?
C40 C39 H39 119.2 . . ?
C35 C40 H40 120.1 . . ?
C39 C40 C35 119.8(6) . . ?
C39 C40 H40 120.1 . . ?
C42 C41 H41 118.1 . . ?
N4 C41 H41 118.1 . . ?
N4 C41 C42 123.8(7) . . ?
C41 C42 H42 120.3 . . ?
C41 C42 C43 119.4(8) . . ?
C43 C42 H42 120.3 . . ?
C42 C43 H43 120.6 . . ?
C42 C43 C44 118.8(7) . . ?
C44 C43 H43 120.6 . . ?
C43 C44 H44 121.0 . . ?
C45 C44 C43 118.0(8) . . ?
C45 C44 H44 121.0 . . ?
C44 C45 H45 117.8 . . ?
N4 C45 C44 124.4(7) . . ?
N4 C45 H45 117.8 . . ?
C5 N1 P1 124.8(4) . . ?
C5 N1 Ti 122.2(4) . . ?
P1 N1 Ti 112.8(3) . . ?
C35 N2 P3 122.1(4) . . ?
C35 N2 Ti 125.8(3) . . ?
P3 N2 Ti 111.8(2) . . ?
C1 N3 Ti 163.7(4) . . ?
C41 N4 Ti 125.5(5) . . ?
C45 N4 C41 115.6(6) . . ?
C45 N4 Ti 118.5(4) . . ?
C11 P1 C17 102.3(3) . . ?
C11 P1 P2 103.5(2) . . ?
C17 P1 P2 115.0(2) . . ?
N1 P1 C11 113.6(3) . . ?
N1 P1 C17 114.6(3) . . ?
N1 P1 P2 107.43(19) . . ?
P1 P2 P3 99.50(9) . . ?
C23 P3 C29 103.3(3) . . ?
C23 P3 P2 114.7(2) . . ?
C29 P3 P2 102.9(2) . . ?
N2 P3 C23 110.8(3) . . ?
N2 P3 C29 117.4(3) . . ?
N2 P3 P2 107.67(19) . . ?
N1 Ti Cl 93.70(14) . . ?
N1 Ti N2 93.12(18) . . ?
N1 Ti N4 162.16(18) . . ?
N2 Ti Cl 154.29(14) . . ?
N2 Ti N4 82.81(19) . . ?
N3 Ti Cl 98.33(17) . . ?
N3 Ti N1 101.7(2) . . ?
N3 Ti N2 104.5(2) . . ?
N3 Ti N4 96.1(2) . . ?
N4 Ti Cl 83.14(15) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.796 0.000 0.000 402.6 146.0 ?


_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT910_6a-Py               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         14 Note  
RESPONSE:  a set of poorly measured low-order reflections 
(too intense or affected by the beamstop) have 
been omitted from the final least-squares refinement
;
# end Validation Reply Form
####################################################################### 
# 
# 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_6a
_database_code_depnum_ccdc_archive 'CCDC 1985145'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne Franche Comte
France
;
_audit_update_record             
;
2020-02-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_audit_creation_date             2020-01-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H39 Cl N3 P3 Ti, C7 H8'
_chemical_formula_sum            'C47 H47 Cl N3 P3 Ti'
_chemical_formula_weight         830.13
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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                   12.4622(7)
_cell_length_b                   22.1019(12)
_cell_length_c                   15.1862(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.5670(10)
_cell_angle_gamma                90
_cell_volume                     4169.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8853
_cell_measurement_temperature    115
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.47
_shelx_estimated_absorpt_T_max   0.959
_shelx_estimated_absorpt_T_min   0.902
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.8118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0498 before and 0.0462 after correction. The Ratio of minimum to maximum transmission is 0.9417. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41349
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.747
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       "φ and ω scans'"
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7451
_reflns_number_total             9558
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.202
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         9558
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0458
_refine_ls_restrained_S_all      1.028
_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)+(0.0473P)²+5.6904P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1157
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1B)=Sof(C1C)=Sof(H1C)=Sof(C1D)=
 Sof(H1D)=Sof(C1E)=Sof(H1E)=Sof(C1F)=Sof(H1F)=Sof(C1G)=Sof(H1G)=1-FVAR(1)
 Sof(C1H)=Sof(H1HA)=Sof(H1HB)=Sof(H1HC)=Sof(C1I)=Sof(C1J)=Sof(H1J)=Sof(C1K)=
 Sof(H1K)=Sof(C1L)=Sof(H1L)=Sof(C1M)=Sof(H1M)=Sof(C1N)=Sof(H1N)=FVAR(1)
 Uiso(C1B)=Uiso(C1C)=Uiso(C1D)=Uiso(C1E)=Uiso(C1F)=Uiso(C1G)=Uiso(C1I)=
 Uiso(C1J)=Uiso(C1K)=Uiso(C1L)=Uiso(C1M)=Uiso(C1N)=FVAR(2)
 Uiso(C1A)=Uiso(C1H)=1.2*FVAR(3)
3.a Free rotating group:
 C1A(C1B,C1C,C1D,C1E,C1F,C1G), C1H(C1I,C1J,C1K,C1L,C1M,C1N)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C1C(H1C), C1D(H1D),
  C1E(H1E), C1F(H1F), C1G(H1G), C1J(H1J), C1K(H1K), C1L(H1L), C1M(H1M), C1N(H1N)
3.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C1A(H1AA,H1AB,
 H1AC), C1H(H1HA,H1HB,H1HC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Ti Ti 0.59624(3) 0.63358(2) 0.20945(3) 0.01112(10) Uani 1 1 d . . . . .
Cl Cl 0.61201(5) 0.72971(3) 0.27313(4) 0.02243(14) Uani 1 1 d . . . . .
P1 P 0.67982(5) 0.54202(2) 0.34453(4) 0.01097(12) Uani 1 1 d . . . . .
P2 P 0.54675(5) 0.59056(3) 0.39134(4) 0.01240(13) Uani 1 1 d . . . . .
P3 P 0.41621(5) 0.56961(3) 0.29620(4) 0.01145(12) Uani 1 1 d . . . . .
N1 N 0.71246(15) 0.56995(8) 0.24977(12) 0.0126(4) Uani 1 1 d . . . . .
N2 N 0.45166(15) 0.59120(8) 0.19950(12) 0.0133(4) Uani 1 1 d . . . . .
N3 N 0.60854(15) 0.65074(8) 0.10197(13) 0.0143(4) Uani 1 1 d . . . . .
C1 C 0.81131(18) 0.55321(10) 0.21390(15) 0.0139(4) Uani 1 1 d . . . . .
C2 C 0.8399(2) 0.58247(12) 0.13782(17) 0.0236(5) Uani 1 1 d . . . . .
H2 H 0.794186 0.613024 0.111605 0.028 Uiso 1 1 calc R . . . .
C3 C 0.9339(2) 0.56763(14) 0.09993(19) 0.0319(7) Uani 1 1 d . . . . .
H3 H 0.951065 0.587601 0.047467 0.038 Uiso 1 1 calc R . . . .
C4 C 1.0033(2) 0.52414(13) 0.13736(18) 0.0264(6) Uani 1 1 d . . . . .
H4 H 1.067955 0.514377 0.111385 0.032 Uiso 1 1 calc R . . . .
C5 C 0.9766(2) 0.49522(11) 0.21321(16) 0.0207(5) Uani 1 1 d . . . . .
H5 H 1.023626 0.465440 0.239838 0.025 Uiso 1 1 calc R . . . .
C6 C 0.88190(19) 0.50915(10) 0.25096(16) 0.0168(5) Uani 1 1 d . . . . .
H6 H 0.864657 0.488455 0.302813 0.020 Uiso 1 1 calc R . . . .
C7 C 0.65992(18) 0.46101(10) 0.33787(15) 0.0135(4) Uani 1 1 d . . . . .
C8 C 0.6435(2) 0.43454(11) 0.25471(16) 0.0182(5) Uani 1 1 d . . . . .
H8 H 0.649691 0.458304 0.203238 0.022 Uiso 1 1 calc R . . . .
C9 C 0.6180(2) 0.37358(12) 0.24676(18) 0.0260(6) Uani 1 1 d . . . . .
H9 H 0.605862 0.355800 0.189885 0.031 Uiso 1 1 calc R . . . .
C10 C 0.6103(2) 0.33849(12) 0.32197(19) 0.0292(6) Uani 1 1 d . . . . .
H10 H 0.593561 0.296661 0.316564 0.035 Uiso 1 1 calc R . . . .
C11 C 0.6272(2) 0.36466(11) 0.40482(18) 0.0236(5) Uani 1 1 d . . . . .
H11 H 0.622989 0.340491 0.456164 0.028 Uiso 1 1 calc R . . . .
C12 C 0.65007(19) 0.42587(10) 0.41336(16) 0.0173(5) Uani 1 1 d . . . . .
H12 H 0.659041 0.443856 0.470287 0.021 Uiso 1 1 calc R . . . .
C13 C 0.78342(18) 0.56132(10) 0.43109(14) 0.0133(4) Uani 1 1 d . . . . .
C14 C 0.80587(19) 0.62322(11) 0.44060(16) 0.0183(5) Uani 1 1 d . . . . .
H14 H 0.769311 0.651596 0.401972 0.022 Uiso 1 1 calc R . . . .
C15 C 0.8815(2) 0.64316(11) 0.50639(17) 0.0225(5) Uani 1 1 d . . . . .
H15 H 0.896923 0.685109 0.512439 0.027 Uiso 1 1 calc R . . . .
C16 C 0.9342(2) 0.60192(12) 0.56310(17) 0.0227(5) Uani 1 1 d . . . . .
H16 H 0.984719 0.615655 0.608931 0.027 Uiso 1 1 calc R . . . .
C17 C 0.91359(19) 0.54077(12) 0.55311(16) 0.0212(5) Uani 1 1 d . . . . .
H17 H 0.950919 0.512566 0.591540 0.025 Uiso 1 1 calc R . . . .
C18 C 0.83856(19) 0.52025(11) 0.48722(15) 0.0173(5) Uani 1 1 d . . . . .
H18 H 0.824997 0.478139 0.480582 0.021 Uiso 1 1 calc R . . . .
C19 C 0.36324(18) 0.49362(10) 0.29682(15) 0.0134(4) Uani 1 1 d . . . . .
C20 C 0.28726(19) 0.47362(11) 0.23010(16) 0.0181(5) Uani 1 1 d . . . . .
H20 H 0.264334 0.499773 0.182633 0.022 Uiso 1 1 calc R . . . .
C21 C 0.2456(2) 0.41546(11) 0.23363(16) 0.0207(5) Uani 1 1 d . . . . .
H21 H 0.194450 0.401854 0.188230 0.025 Uiso 1 1 calc R . . . .
C22 C 0.2782(2) 0.37709(11) 0.30291(17) 0.0212(5) Uani 1 1 d . . . . .
H22 H 0.250382 0.337113 0.304378 0.025 Uiso 1 1 calc R . . . .
C23 C 0.3513(2) 0.39723(11) 0.36994(17) 0.0209(5) Uani 1 1 d . . . . .
H23 H 0.372752 0.371179 0.417897 0.025 Uiso 1 1 calc R . . . .
C24 C 0.39338(19) 0.45534(10) 0.36741(16) 0.0169(5) Uani 1 1 d . . . . .
H24 H 0.442882 0.469032 0.413964 0.020 Uiso 1 1 calc R . . . .
C25 C 0.31004(18) 0.61692(10) 0.33409(14) 0.0150(5) Uani 1 1 d . . . . .
C26 C 0.3305(2) 0.67854(11) 0.34748(16) 0.0202(5) Uani 1 1 d . . . . .
H26 H 0.398426 0.694942 0.336022 0.024 Uiso 1 1 calc R . . . .
C27 C 0.2517(2) 0.71565(12) 0.37740(17) 0.0258(6) Uani 1 1 d . . . . .
H27 H 0.266038 0.757427 0.387285 0.031 Uiso 1 1 calc R . . . .
C28 C 0.1521(2) 0.69206(13) 0.39296(18) 0.0286(6) Uani 1 1 d . . . . .
H28 H 0.098342 0.717673 0.413701 0.034 Uiso 1 1 calc R . . . .
C29 C 0.1307(2) 0.63164(13) 0.3785(2) 0.0303(6) Uani 1 1 d . . . . .
H29 H 0.061923 0.615777 0.388653 0.036 Uiso 1 1 calc R . . . .
C30 C 0.2092(2) 0.59383(12) 0.34921(17) 0.0225(5) Uani 1 1 d . . . . .
H30 H 0.194119 0.552122 0.339423 0.027 Uiso 1 1 calc R . . . .
C31 C 0.38094(18) 0.58336(10) 0.12094(14) 0.0138(4) Uani 1 1 d . . . . .
C32 C 0.2938(2) 0.62162(12) 0.10209(16) 0.0213(5) Uani 1 1 d . . . . .
H32 H 0.280762 0.654091 0.140817 0.026 Uiso 1 1 calc R . . . .
C33 C 0.2255(2) 0.61221(13) 0.02609(17) 0.0283(6) Uani 1 1 d . . . . .
H33 H 0.166338 0.638688 0.012844 0.034 Uiso 1 1 calc R . . . .
C34 C 0.2431(2) 0.56452(13) -0.03033(17) 0.0271(6) Uani 1 1 d . . . . .
H34 H 0.195606 0.557852 -0.081511 0.033 Uiso 1 1 calc R . . . .
C35 C 0.3304(2) 0.52672(12) -0.01140(16) 0.0222(5) Uani 1 1 d . . . . .
H35 H 0.342997 0.494022 -0.049868 0.027 Uiso 1 1 calc R . . . .
C36 C 0.39980(19) 0.53628(11) 0.06338(16) 0.0178(5) Uani 1 1 d . . . . .
H36 H 0.460343 0.510596 0.075313 0.021 Uiso 1 1 calc R . . . .
C37 C 0.60885(19) 0.68140(10) 0.01735(15) 0.0158(5) Uani 1 1 d . . . . .
C38 C 0.5024(3) 0.71500(18) -0.0003(2) 0.0536(11) Uani 1 1 d . . . . .
H38A H 0.442747 0.686064 -0.001438 0.080 Uiso 1 1 calc GR . . . .
H38B H 0.501388 0.735771 -0.057360 0.080 Uiso 1 1 calc GR . . . .
H38C H 0.494737 0.744774 0.046627 0.080 Uiso 1 1 calc GR . . . .
C39 C 0.6210(3) 0.63574(13) -0.05568(18) 0.0415(8) Uani 1 1 d . . . . .
H39A H 0.687967 0.612959 -0.043161 0.062 Uiso 1 1 calc GR . . . .
H39B H 0.623203 0.656963 -0.112176 0.062 Uiso 1 1 calc GR . . . .
H39C H 0.559788 0.607799 -0.058924 0.062 Uiso 1 1 calc GR . . . .
C40 C 0.7013(3) 0.72630(15) 0.0211(2) 0.0452(9) Uani 1 1 d . . . . .
H40A H 0.695432 0.753991 0.070861 0.068 Uiso 1 1 calc GR . . . .
H40B H 0.698441 0.749471 -0.034089 0.068 Uiso 1 1 calc GR . . . .
H40C H 0.769847 0.704430 0.028853 0.068 Uiso 1 1 calc GR . . . .
C1A C -0.1293(5) 0.2288(3) 0.8666(4) 0.0424(5) Uiso 0.361(3) 1 d . . P A 1
H1AA H -0.205034 0.227207 0.843715 0.064 Uiso 0.361(3) 1 calc GR . P A 1
H1AB H -0.114140 0.268020 0.894914 0.064 Uiso 0.361(3) 1 calc GR . P A 1
H1AC H -0.114721 0.196350 0.909867 0.064 Uiso 0.361(3) 1 calc GR . P A 1
C1B C -0.0585(3) 0.22072(19) 0.7914(3) 0.0353(4) Uiso 0.361(3) 1 d G . P A 1
C1C C -0.0783(4) 0.1744(2) 0.7292(3) 0.0353(4) Uiso 0.361(3) 1 d G . P A 1
H1C H -0.138241 0.148331 0.733696 0.042 Uiso 0.361(3) 1 calc R . P A 1
C1D C -0.0115(5) 0.1659(2) 0.6607(3) 0.0353(4) Uiso 0.361(3) 1 d G . P A 1
H1D H -0.026096 0.134219 0.619155 0.042 Uiso 0.361(3) 1 calc R . P A 1
C1E C 0.0769(4) 0.2039(3) 0.6531(3) 0.0353(4) Uiso 0.361(3) 1 d G . P A 1
H1E H 0.122522 0.198213 0.606551 0.042 Uiso 0.361(3) 1 calc R . P A 1
C1F C 0.0974(4) 0.2504(2) 0.7144(4) 0.0353(4) Uiso 0.361(3) 1 d G . P A 1
H1F H 0.157282 0.276476 0.709577 0.042 Uiso 0.361(3) 1 calc R . P A 1
C1G C 0.0303(4) 0.2586(2) 0.7828(3) 0.0353(4) Uiso 0.361(3) 1 d G . P A 1
H1G H 0.044974 0.290396 0.824070 0.042 Uiso 0.361(3) 1 calc R . P A 1
C1H C -0.0425(3) 0.27907(17) 0.87781(19) 0.0424(5) Uiso 0.639(3) 1 d . . P A 2
H1HA H -0.076284 0.317740 0.860373 0.064 Uiso 0.639(3) 1 calc GR . P A 2
H1HB H 0.025074 0.286618 0.913675 0.064 Uiso 0.639(3) 1 calc GR . P A 2
H1HC H -0.091161 0.255699 0.912352 0.064 Uiso 0.639(3) 1 calc GR . P A 2
C1I C -0.0196(2) 0.24390(10) 0.79634(14) 0.0353(4) Uiso 0.639(3) 1 d G . P A 2
C1J C -0.08773(19) 0.19690(12) 0.76470(19) 0.0353(4) Uiso 0.639(3) 1 d G . P A
2
H1J H -0.150106 0.187749 0.794275 0.042 Uiso 0.639(3) 1 calc R . P A 2
C1K C -0.0654(2) 0.16332(12) 0.6904(2) 0.0353(4) Uiso 0.639(3) 1 d G . P A 2
H1K H -0.112463 0.131612 0.669942 0.042 Uiso 0.639(3) 1 calc R . P A 2
C1L C 0.0259(3) 0.17626(13) 0.64618(17) 0.0353(4) Uiso 0.639(3) 1 d G . P A 2
H1L H 0.041328 0.153423 0.595715 0.042 Uiso 0.639(3) 1 calc R . P A 2
C1M C 0.0944(2) 0.22308(14) 0.67676(19) 0.0353(4) Uiso 0.639(3) 1 d G . P A 2
H1M H 0.156574 0.232220 0.646940 0.042 Uiso 0.639(3) 1 calc R . P A 2
C1N C 0.0716(2) 0.25646(12) 0.75104(19) 0.0353(4) Uiso 0.639(3) 1 d G . P A 2
H1N H 0.118684 0.288223 0.771249 0.042 Uiso 0.639(3) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Ti Cl 2.3362(7) . ?
Ti P1 3.0079(7) . ?
Ti P2 3.0308(7) . ?
Ti P3 3.0395(7) . ?
Ti N1 2.0758(19) . ?
Ti N2 2.0256(19) . ?
Ti N3 1.6945(19) . ?
P1 P2 2.1434(8) . ?
P1 N1 1.6464(19) . ?
P1 C7 1.809(2) . ?
P1 C13 1.818(2) . ?
P2 P3 2.1388(8) . ?
P3 N2 1.6379(19) . ?
P3 C19 1.805(2) . ?
P3 C25 1.815(2) . ?
N1 C1 1.435(3) . ?
N2 C31 1.436(3) . ?
N3 C37 1.453(3) . ?
C1 C2 1.395(3) . ?
C1 C6 1.400(3) . ?
C2 C3 1.386(4) . ?
C3 C4 1.384(4) . ?
C4 C5 1.381(4) . ?
C5 C6 1.387(3) . ?
C7 C8 1.392(3) . ?
C7 C12 1.398(3) . ?
C8 C9 1.387(3) . ?
C9 C10 1.390(4) . ?
C10 C11 1.386(4) . ?
C11 C12 1.386(3) . ?
C13 C14 1.402(3) . ?
C13 C18 1.389(3) . ?
C14 C15 1.389(3) . ?
C15 C16 1.384(4) . ?
C16 C17 1.382(4) . ?
C17 C18 1.390(3) . ?
C19 C20 1.402(3) . ?
C19 C24 1.394(3) . ?
C20 C21 1.389(3) . ?
C21 C22 1.386(4) . ?
C22 C23 1.384(3) . ?
C23 C24 1.389(3) . ?
C25 C26 1.397(3) . ?
C25 C30 1.393(3) . ?
C26 C27 1.383(3) . ?
C27 C28 1.384(4) . ?
C28 C29 1.376(4) . ?
C29 C30 1.386(4) . ?
C31 C32 1.388(3) . ?
C31 C36 1.391(3) . ?
C32 C33 1.394(3) . ?
C33 C34 1.387(4) . ?
C34 C35 1.384(4) . ?
C35 C36 1.388(3) . ?
C37 C38 1.525(4) . ?
C37 C39 1.516(4) . ?
C37 C40 1.519(4) . ?
C1A C1B 1.5078 . ?
C1B C1C 1.4020 . ?
C1B C1G 1.4018 . ?
C1C C1D 1.3962 . ?
C1D C1E 1.3970 . ?
C1E C1F 1.3965 . ?
C1F C1G 1.3964 . ?
C1H C1I 1.5076 . ?
C1I C1J 1.4023 . ?
C1I C1N 1.4021 . ?
C1J C1K 1.3966 . ?
C1K C1L 1.3965 . ?
C1L C1M 1.3970 . ?
C1M C1N 1.3958 . ?

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
Cl Ti P1 108.45(2) . . ?
Cl Ti P2 85.68(2) . . ?
Cl Ti P3 106.52(2) . . ?
P1 Ti P2 41.577(16) . . ?
P1 Ti P3 67.604(17) . . ?
P2 Ti P3 41.260(16) . . ?
N1 Ti Cl 117.41(6) . . ?
N1 Ti P1 31.51(5) . . ?
N1 Ti P2 72.93(5) . . ?
N1 Ti P3 94.52(5) . . ?
N2 Ti Cl 119.76(6) . . ?
N2 Ti P1 89.86(5) . . ?
N2 Ti P2 71.25(5) . . ?
N2 Ti P3 30.05(5) . . ?
N2 Ti N1 107.72(7) . . ?
N3 Ti Cl 100.60(7) . . ?
N3 Ti P1 138.98(7) . . ?
N3 Ti P2 171.37(7) . . ?
N3 Ti P3 130.40(7) . . ?
N3 Ti N1 108.74(8) . . ?
N3 Ti N2 100.35(9) . . ?
P2 P1 Ti 69.78(2) . . ?
N1 P1 Ti 41.23(7) . . ?
N1 P1 P2 110.72(7) . . ?
N1 P1 C7 111.38(10) . . ?
N1 P1 C13 109.47(10) . . ?
C7 P1 Ti 126.10(8) . . ?
C7 P1 P2 114.06(8) . . ?
C7 P1 C13 111.03(10) . . ?
C13 P1 Ti 121.50(7) . . ?
C13 P1 P2 99.58(8) . . ?
P1 P2 Ti 68.64(2) . . ?
P3 P2 Ti 69.59(2) . . ?
P3 P2 P1 103.57(3) . . ?
P2 P3 Ti 69.15(2) . . ?
N2 P3 Ti 38.26(7) . . ?
N2 P3 P2 107.32(7) . . ?
N2 P3 C19 113.62(10) . . ?
N2 P3 C25 111.83(10) . . ?
C19 P3 Ti 135.89(8) . . ?
C19 P3 P2 117.17(8) . . ?
C19 P3 C25 104.96(11) . . ?
C25 P3 Ti 116.82(8) . . ?
C25 P3 P2 101.28(8) . . ?
P1 N1 Ti 107.26(10) . . ?
C1 N1 Ti 131.51(15) . . ?
C1 N1 P1 120.97(15) . . ?
P3 N2 Ti 111.69(10) . . ?
C31 N2 Ti 126.96(15) . . ?
C31 N2 P3 121.21(15) . . ?
C37 N3 Ti 164.38(16) . . ?
C2 C1 N1 118.6(2) . . ?
C2 C1 C6 117.5(2) . . ?
C6 C1 N1 123.9(2) . . ?
C3 C2 C1 120.9(2) . . ?
C4 C3 C2 121.0(3) . . ?
C5 C4 C3 118.7(2) . . ?
C4 C5 C6 120.8(2) . . ?
C5 C6 C1 121.1(2) . . ?
C8 C7 P1 118.44(17) . . ?
C8 C7 C12 119.6(2) . . ?
C12 C7 P1 121.64(18) . . ?
C9 C8 C7 120.2(2) . . ?
C8 C9 C10 120.0(2) . . ?
C11 C10 C9 119.9(2) . . ?
C10 C11 C12 120.5(2) . . ?
C11 C12 C7 119.7(2) . . ?
C14 C13 P1 115.33(17) . . ?
C18 C13 P1 125.34(18) . . ?
C18 C13 C14 119.3(2) . . ?
C15 C14 C13 120.1(2) . . ?
C16 C15 C14 120.0(2) . . ?
C17 C16 C15 120.0(2) . . ?
C16 C17 C18 120.5(2) . . ?
C13 C18 C17 120.0(2) . . ?
C20 C19 P3 121.05(17) . . ?
C24 C19 P3 119.52(17) . . ?
C24 C19 C20 119.3(2) . . ?
C21 C20 C19 119.8(2) . . ?
C22 C21 C20 120.5(2) . . ?
C23 C22 C21 119.8(2) . . ?
C22 C23 C24 120.3(2) . . ?
C23 C24 C19 120.2(2) . . ?
C26 C25 P3 118.59(18) . . ?
C30 C25 P3 122.10(18) . . ?
C30 C25 C26 119.3(2) . . ?
C27 C26 C25 120.0(2) . . ?
C26 C27 C28 120.1(2) . . ?
C29 C28 C27 120.2(2) . . ?
C28 C29 C30 120.2(3) . . ?
C29 C30 C25 120.1(2) . . ?
C32 C31 N2 121.1(2) . . ?
C32 C31 C36 119.7(2) . . ?
C36 C31 N2 119.3(2) . . ?
C31 C32 C33 119.7(2) . . ?
C34 C33 C32 120.6(2) . . ?
C35 C34 C33 119.4(2) . . ?
C34 C35 C36 120.4(2) . . ?
C35 C36 C31 120.2(2) . . ?
N3 C37 C38 108.6(2) . . ?
N3 C37 C39 110.13(19) . . ?
N3 C37 C40 109.1(2) . . ?
C39 C37 C38 109.4(3) . . ?
C39 C37 C40 110.0(3) . . ?
C40 C37 C38 109.6(3) . . ?
C1C C1B C1A 120.9 . . ?
C1G C1B C1A 120.9 . . ?
C1G C1B C1C 118.1 . . ?
C1D C1C C1B 121.1 . . ?
C1C C1D C1E 120.1 . . ?
C1F C1E C1D 119.4 . . ?
C1G C1F C1E 120.2 . . ?
C1F C1G C1B 121.1 . . ?
C1J C1I C1H 120.9 . . ?
C1N C1I C1H 121.0 . . ?
C1N C1I C1J 118.1 . . ?
C1K C1J C1I 121.1 . . ?
C1L C1K C1J 120.1 . . ?
C1K C1L C1M 119.4 . . ?
C1N C1M C1L 120.1 . . ?
C1M C1N C1I 121.1 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
